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Index

120

User Manual

Product versions ......................................... 28

Pure element spectra .................................. 55

Radiation protection .................................... 13

Reference

Points ...................................................... 71

Spectra .................................................... 54

Report ....................................................... 105

Report template ........................................ 105

Resolution, Spectrometer ........................... 22

Result calculation ........................................ 27

Room planning ............................................ 33

Safety

Considerations ........................................ 13

Equipment ............................................... 15

Instructions .............................................. 12

Requirements .......................................... 12

Rules ....................................................... 14

Switches .................................................. 16

Sample

Measurement .......................................... 59

Positioning ............................................... 50

Shutdown .................................................. 110

Smoking, eating and drinking ..................... 12

Spectra

Correction ................................................ 25

Primary .................................................... 56

Pure element ........................................... 55

Reference ................................................ 54

Standard .................................................. 57

System ............................................ 54, 103

Spectrometer, Weight of ............................. 13

Spectrum

Composition of ........................................ 24

Display .................................................... 66

Manipulation ............................................ 66

Staff requirements ...................................... 15

Stage control ............................................... 50

Stage program

Create ............................................... 70, 72

Edit .......................................................... 72

Load ........................................................ 70

Workspace .............................................. 69

Stage program workspace .......................... 69

Standard delivery contents ....................... 115

Standard spectra ........................................ 57

Standards ................................................... 77

Load ........................................................ 78

New ......................................................... 79

Save ........................................................ 78

Standby mode .......................................... 110

Statistical error Sigma ................................ 26

Switching off the instrument ..................... 110

System settings ........................................ 105

System spectra ................................... 54, 103

Technical parameters ................................. 31

Touch screen user interface ....................... 67

Transportation .......................................... 113

Video settings ............................................. 52

Warning labels ............................................ 17

Warranty ..................................................... 11

Workspace

Data ....................................................... 105

Measurement .......................................... 59

Methods .................................................. 80

Spectra .................................................. 103

Stage program ........................................ 69

Standards ................................................ 77

System .................................................. 105

XData

Control elements ..................................... 75

Display elements ..................................... 75

Installation ............................................... 35

Start-up ................................................... 75

Using the program .................................. 75

X-ray

Fluorescence spectra, Evaluation of ....... 25

Fluorescence spectrum ........................... 24

Generation .............................................. 18

X-ray quanta, Detection of .......................... 20

X-ray radiation

Biological effects ................................... 117

XSpect Pro

Содержание M1 MISTRAL

Страница 1: ...M1 ORA M1 MISTRAL Micro XRF Benchtop Spectrometer User Manual...

Страница 2: ...ecked the contents of this manual for agreement with the hardware and software described Since deviations cannot be precluded entirely we cannot guarantee full agreement However the data in this manua...

Страница 3: ...6 Evaluation of X ray Fluorescence Spectra 25 4 The M1 ORA MISTRAL System 28 4 1 Product Description 28 4 2 Product Versions 28 4 2 1 M1 ORA 28 4 2 2 M1 MISTRAL 29 4 3 Hardware System Components 30 4...

Страница 4: ...XData Program Start up 75 6 2 Display and Control Elements 75 6 3 Managing Standards 77 6 3 1 Saving a List of Standards 78 6 3 2 Loading a List of Standards 78 6 3 3 Editing Basic Data 78 6 3 4 Crea...

Страница 5: ...river path manually for the unknown devices 42 Fig 25 Windows security warning during driver installation 42 Fig 26 Finishing the successful instrument driver installation 42 Fig 27 Status display dur...

Страница 6: ...or Calibration tab without added standards 93 Fig 75 The available samples dialog 93 Fig 76 Method editor Calibration tab with added standards before FP calculation 94 Fig 77 Method editor Calibration...

Страница 7: ...Functions in the XSpect Pro navigation bar 48 Table 11 Functions for the stage movement 51 Table 12 Functions in the main panel for measurements with XSpect Pro 59 Table 13 Keyboard shortcuts 62 Table...

Страница 8: ......

Страница 9: ...Nano GmbH Please familiarize yourself with the contents and follow the safety instructions particularly those regarding the handling of the product This way you can be sure of taking full advantage of...

Страница 10: ...g applications are explicitly excluded from the definition of intended usage Any sort of medical and biological application Radiographic applications Online process control for industrial or research...

Страница 11: ...humidity vibrations aggressive chemical substances etc Structural modifications to the M1 ORA MISTRAL Operation of the M1 ORA MISTRAL while the protective housing is not completely closed or damaged O...

Страница 12: ...ives and regulations are defined for safety and radiation protection These must strictly be adhered to by both manufacturer and users 2 1 Basic Safety Requirements The following basic safety requireme...

Страница 13: ...anufacturer s radiation protection measures the X ray source used in this instrument constitutes a health risk A direct exposure to the excitation beam for several seconds could cause a deep damage of...

Страница 14: ...event bodily injuries of the operator due to the measures taken and the technical installations provided by the manufacturer The same basic safety rules refer to section 2 1 are valid both for the pre...

Страница 15: ...ring the operation of the instrument Behavior and actions to be taken in hazardous situations 2 6 Safety Equipment Danger The M1 ORA MISTRAL must only be operated with functional safety equipment In t...

Страница 16: ...he time period of emitting X rays 8 Internal safety switches Interlock circuit connected with the housing parts inside the instrument Opening the instrument for service purposes will lead to an interr...

Страница 17: ...ng Labels Table 2 Name plates and warning labels on the M1 ORA MISTRAL instrument Element Location Function Front panel Company logo Front panel Product name Rear panel Name plate of the instrument Re...

Страница 18: ...ng rise to the characteristic X ray line spectrum The second leads to a continuous spectrum the so called bremsstrahlung radiation 3 1 1 X ray Fluorescence In atomic physics fluorescence generally is...

Страница 19: ...le emits electromagnetic radiation This physical principle is valid for acceleration deceleration and also for any change of direction of the movement of the particle The blue color of the sky as well...

Страница 20: ...al counter detector is a cylindrical capacitor filled with gas usually Argon and with an entrance window which is transparent for X rays The incident photon ionizes multiple Ar atoms on its way throug...

Страница 21: ...h incoming pulses height and increments the counter of the channel attributed to this specific height by 1 The resulting spectrum shows how many pulses were counted into individual channels Since howe...

Страница 22: ...rocess Usual integration times are between 10 s and 180 s per spectrum 3 4 Spectrometer Resolution The emitted X ray spectrum is not composed of sharp lines Quantum mechanics dictates that each fluore...

Страница 23: ...s the capability of a spectrometer to clearly discriminate adjacent peaks is its resolution There are different possible definitions for a spectral separation of two lines but in XRF analysis it is co...

Страница 24: ...half maximum FWHM 3 5 Composition of a Spectrum Typical XRF spectra of different sample types are shown in Fig 7 The inset depicts the same spectra but with a square root y scale to emphasize the bac...

Страница 25: ...ound 3 6 Evaluation of X ray Fluorescence Spectra X ray fluorescence analysis yields two central results Which elements are present in a sample and what is their share in the total sample composition...

Страница 26: ...on 4 Deconvolution Some combinations of elements within a sample can lead to a strong overlap of fluorescence lines In order to determine the actual intensity of each individual element peak profiles...

Страница 27: ...values are an indicator for misidentified or non identified elements or for an inaccurate gain correction 2 1 2 2 1 2 2 1 1 n n i i i fit y y n n 7 Result calculation The net peak areas are transferr...

Страница 28: ...e types and applications Low operating costs Application fields of the M1 ORA MISTRAL Quality control Materials sciences Analysis of alloys precious metal alloys and jewelry Layer thickness analysis 4...

Страница 29: ...ue to the significantly better signal to background ratio SDDs achieve a higher sensitivity and element specific detection limits in the range down to 100 parts per million ppm ideally even below that...

Страница 30: ...of the M1 ORA MISTRAL The connections of the M1 ORA MISTRAL system are listed in Table 4 Table 4 Connections of the M1 ORA MISTRAL system components Pos Component Connection Function 1 Spectrometer Li...

Страница 31: ...380 mm x 420 mm x 350 mm 27 kg without computer 550 mm x 680 mm x 430 mm 50 kg without computer Connection values Voltage Frequency Power Connections 110 230 V AC 50 60 Hz max 150 W 3 prong grounded...

Страница 32: ...etector control and PC connection type Bruker Nano GmbH XGS XCU Sample stage Sample positioning Stage Traversing range Optional stage Traversing range manual Z stage 105 mm motorized Z stage 75 mm man...

Страница 33: ...ulation Operational elements on the front touch panel of the instrument must be easily accessible for the operator Fig 11 Room planning for the installation of the M1 ORA MISTRAL 4 5 2 Electrical Conn...

Страница 34: ...ges XSpect Pro and XData XSpect Pro is the control software for operating the instrument and monitoring its functionalities It gives access to all measurement and quantification procedures and is used...

Страница 35: ...lication data Setup and edit of measurement methods A detailed description of the XData program can be found in chapter 6 4 6 2 Program Installation The installation and setup of the software programs...

Страница 36: ...s to be selected Fig 14 As indicated in the corresponding dialog the update option keeps all previous user data accessible while Remove and install will erase all previously recorded data from the com...

Страница 37: ...libration spectra database entries log files or methods Fig 16 It is recommended to use the default settings Fig 16 Select data folder Choose whether the full software package with the instrument cont...

Страница 38: ...irst time install of the software For updates the installation can be skipped choosing the Exit option After the installation or to skip the installation the Exit button has to be clicked by the user...

Страница 39: ...In case of a software update XSpect Pro and or XData are now ready for use If the software is installed for the first time or an older version was de installed completely prior to the installation th...

Страница 40: ...he instrument can be used This initial setup should be performed by the Bruker service personnel 4 6 3 Installation of Drivers The M1 ORA MISTRAL is connected to the instrument control computer via US...

Страница 41: ...s entry and choose Properties In the next dialog go to the Driver tab and choose Update Driver Fig 23 Fig 23 Properties dialog for the M1 ORA MISTRAL before installing the correct driver In the next d...

Страница 42: ...Install this driver software anyway option Fig 25 Fig 25 Windows security warning during driver installation The installation process commences After installation the M1 ORA MISTRAL is shown in the d...

Страница 43: ...port or storage in cold environments the instrument must be warmed up at room temperature before switching it on For the start of operation the operator must be familiar with the measurement and evalu...

Страница 44: ...measuring software can be authorized by a user and password query 5 Switch on the high voltage on the keypad after the respective request from the program 6 Performing a reference measurement After th...

Страница 45: ...king the corresponding button During the measurement the accumulation of the spectrum can be monitored in the spectrum tab of the measurement section If a method was chosen the expected elements will...

Страница 46: ...the user will be asked to switch on the high voltage HV of the X ray tube as shown in Fig 28 Fig 28 Switching on the high voltage As soon as the HV button is pressed the HV generator is activated and...

Страница 47: ...which largely depend on the currently active workspace Fig 29 Main screen of the XSpect Pro program After the start of the software the instrument should be given a 20 min warm up phase to reach therm...

Страница 48: ...ay the operation of the sample chamber door must be done manually HV off HV on The high voltage is switched on at the start of the XSpect Pro program and switched off when exiting the program refer to...

Страница 49: ...report and report template section please refer to section 6 7 1 Close the XSpect Pro program 5 2 3 Print Report Additional Information Clicking the button opens a dialog which allows entering additio...

Страница 50: ...en the sample image in the optical microscope shows the best contrast Display of the sample image in the optical microscope Fig 31 Stage control for the manual Z stage 5 3 2 Motorized Z Stage The moto...

Страница 51: ...on Auto focus sample is positioned in the focal plane automatically Z joystick Click and move option click into the video image and the excitation spot will be positioned on that point Useful for exac...

Страница 52: ...tically moves towards the door to facilitate sample changing and positioning Once the door is closed again the stage moves back into the sample chamber 5 3 5 Video Settings Three buttons can be found...

Страница 53: ...Note The video settings may negatively affect auto focus capabilities High contrast and sharpness settings are suggested Clicking the icon opens the SAVE dialog where the folder and the name of the i...

Страница 54: ...ts Standards on the right side of the main working area has to be selected The Spectrum tab displays the currently or the last measured spectrum 5 4 1 Measuring Reference Spectra Reference spectra are...

Страница 55: ...rection during measurement relative to the first reference measurement here 0 9097 The values should be close to 1 gain int corr and 0 offset res MnK AgK Energy resolution for the given elements The v...

Страница 56: ...all collimators automatically or only for the currently set one 4 Click on the icon and select an element Elements already measured for the preset conditions are highlighted 5 Put in and align the re...

Страница 57: ...o box will pop up 5 Put in and align a scattering sample 6 Start the measurement with Fig 40 Recording primary spectra Note If the measurement conditions HV change the primary spectrum must be measure...

Страница 58: ...Choose a standard which is to be measured from the list the standard has to be defined in the XData program prior to the measurement under the preset measurement conditions and marked with a green Y...

Страница 59: ...ays the recorded spectra Independent of the selected tab the user has access to the main working area of the measurement workspace It is located below the instrument status bar The buttons available i...

Страница 60: ...the base material The measurement has to be done on the uncoated base The layer thickness values of the method will be set to 0 and the concentration of the base elements will be a fitting parameter T...

Страница 61: ...ect Method tab Fig 43 and the pre examination option Pre examination tab Fig 44 Fig 43 Selection of an existing measurement method 1 Measurement methods have to be defined in the XData program From th...

Страница 62: ...sed method The pre examination serves as a method independent measurement mode It allows for a quick qualitative and quantitative FP Fundamental Parameter model analysis of samples The measurement par...

Страница 63: ...space Results tab 5 5 4 Table Tab Quantitative results of any repeated measurement or analyses of multiple positions with identical specifications are best viewed in the Table tab Here an easy compari...

Страница 64: ...y are the only element present Density column shows an additional column per layer which displays the preset density of every layer Error columns displays the uncertainty of the results Comment column...

Страница 65: ...ll recorded spectra are accessible Fig 48 Measurement workspace Spectrum tab The spectrum list is located below the spectrum display The most recent spectrum will always be named Measure If a new meas...

Страница 66: ...ing the x axis to the right or to the left Change the intensity scale by holding the left mouse button down and moving the y axis down or upwards Alternatively use the cursor keys and or PgUp and PgDo...

Страница 67: ...on an element to open the ELEMENT PROPERTIES EDITOR dialog The ELEMENT PROPERTIES EDITOR dialog for a selected element allows to select the color for displaying the element lines the element lines sho...

Страница 68: ...the result display on the right side Results are presented either as table with statistics or as a trend line The bottom line features the following control elements Table 16 Control elements in the...

Страница 69: ...e the X ray beam shutter between each measurement and the use of a z base When z base is activated the stage will move to the z position defined next to the according check box before driving to the n...

Страница 70: ...ccessively Additional actions z base or autofocus will be performed as during the actual measurement No spectra are recorded This option only serves as a check for the sample positioning 5 6 1 Load Cr...

Страница 71: ...longer used stage programs can be deleted by clicking the button after being highlighted in the list 5 6 2 Graphic Display of Measurement Points In the upper half of the middle panel a graphic visuali...

Страница 72: ...re Points Table The lower of the two visible tables is the Measure points table The coordinates of all defined measurement positions as well as additional information like measurement time or number o...

Страница 73: ...gram Clicking on one measure point entry highlights this single entry and unlocks the options on the right side of the main panel These options are compiled in Table 18 Table 18 Options for selected s...

Страница 74: ...es unlocks the options listed in Table 19 Table 19 Options for selected multiple entries in the measure points table Button Description The marked measurement point s will be deleted Measurement time...

Страница 75: ...e XSpect Pro program During the start up of the XData program the following dialog is displayed Fig 55 Status display during initialization of the XData program 6 2 Display and Control Elements The Gr...

Страница 76: ...additional information on the structure of the selected sample Method management Method editor Lists all available methods and allows for adding editing and deleting methods Access to templates Filter...

Страница 77: ...andards Standards are used to increase the precision of a quantification method A defined and measured standard can be used to calibrate a measurement method as described in section 6 4 1 The standard...

Страница 78: ...erred to another computer all four files have to be saved Fig 58 List of files needed to save a list of standards 6 3 2 Loading a List of Standards It is possible to include a list of standards to the...

Страница 79: ...tion bulk in the main type list Then type a new name in the sub type field and choose the elements which will be present by clicking them on the periodic table Save the sub type by clicking 6 3 4 Crea...

Страница 80: ...ing below the sample structure and fill the layers with elements Change the thickness of a layer by highlighting it and typing in a value in the thickness field Change the concentration of an element...

Страница 81: ...ectra for the pre set measurement conditions Alternatively these system spectra can be loaded 6 4 1 1 Standard based Bulk Methods LT The Lucas Tooth LT method is a calculation procedure that works bas...

Страница 82: ...e the layout of the samples here a bulk sample containing Au Ag and Cu 6 If the samples have roughly known concentration the start concentration values can be chosen accordingly 7 Tick the Normalize s...

Страница 83: ...trations might speed up the quantification algorithm In some rare cases it can prevent the software from fitting wrong results Unit If one element is expected to have a very low concentration the numb...

Страница 84: ...elements are also abundant in the layer Use tolerances If selected additional fields appear where the target value and low and high concentration values can be entered These tolerances are for elemen...

Страница 85: ...pure element spectrum found in database red No pure element spectrum found in database for preset measurement conditions 11 Link elements to respective pure element spectra Either automatically only f...

Страница 86: ...e button opens the AVAILABLE SAMPLES dialog Fig 65 Out of all entries in the database only those standards are shown which based on their structure and element selection can be used for calibrating th...

Страница 87: ...87 14 Save and exit the AVAILABLE SAMPLES dialog Fig 67 Method editor Calibration tab with added standards before calibration 15 Start the calibration process by clicking the button Fig 68 Method edi...

Страница 88: ...mit for the active calibration range Note After adding or deleting a calibration range click on the Start calibration button In the example in Fig 69 three calibration ranges have been set red frame T...

Страница 89: ...alibration with a right click on the highlighted value c If most values for a certain standard deviate significantly check for inconsistencies in the respective standard s spectrum The spectrum can be...

Страница 90: ...nd support the calculation method with an empirical approach It is possible to complete the creation of an FP method after the normation process This is the quickest way to get a measurement method re...

Страница 91: ...ons the start concentration values can be predefined accordingly 7 Tick the Normalize sample standard Target value checkbox 8 If the sample is known to have a Density different from the bulk density e...

Страница 92: ...s b or manually by assigning spectra using the spectrum working area on the right side c At this point the method should be saved by clicking the button so it can be used as a non calibrated method Al...

Страница 93: ...ABLE SAMPLES dialog Fig 75 Out of all entries in the database only those standards are shown which based on their structure and element selection can be used for calibrating the method 13 Select the s...

Страница 94: ...ick the button to perform a FP calculation for all selected standards The calculated FP values will be plotted against the given values of the selected standards The displayed data can be selected by...

Страница 95: ...ntally until they appear Fig 78 Method editor Calibration tab after first calibration 17 If individual values are far off the red 1 1 line the following options are available a In order to check if it...

Страница 96: ...uses the FP calculation algorithm and its setup is therefore very much similar to the one of a standard supported bulk FP method Again calibration is optional Start the process by changing to the Meth...

Страница 97: ...light elements In cases where the layer is too thick to be measured in emission mode it might be possible to use the absorption mode If you use this mode double click on the first element in the base...

Страница 98: ...all element lines b or manually by assigning spectra using the spectrum working area on the right side c At this point the method should be saved by clicking the button and it can be used as a non cal...

Страница 99: ...button opens the AVAILABLE SAMPLES dialog Fig 83 Out of all entries in the database only those standards are shown which based on their structure and element selection can be used for calibrating the...

Страница 100: ...Calibration tab with added standards before FP calculation 17 Click the button to perform FP calculation for all selected standards The calculated FP values will be plotted against the given values o...

Страница 101: ...processed the chart will be updated with the calibrated results The calibration coefficients are displayed in the bottom left corner The results should be much closer to the blue line than before the...

Страница 102: ...mple values and start the calibration process again b After careful evaluation the point can be excluded from the calibration with a right click on the highlighted value c If most values for a certain...

Страница 103: ...a serve as basic data for the calculation routines and should therefore be treated with great care Fig 87 Spectra workspace On the left hand side three tabs navigate you through the branches of Pure e...

Страница 104: ...below the spectrum chart it will be highlighted in gray The measurement conditions of the selected spectrum are displayed in the table on the left hand side 3 Select the respective pure element standa...

Страница 105: ...ditional tools for database management and reporting and provides access to archived measurement data The main working area is divided into the tabs Report templates Integrity Backup Restore Data proc...

Страница 106: ...roperties section A fixed object cannot be moved until unfixed When a fixed object is highlighted an anchor is shown Check the Pass on option in the Properties section to show an object on every page...

Страница 107: ...t by clicking the icon or the icon respectively Pages added at the end of the report will inherit all objects with property Pass on from the previous page To delete the current page click the icon If...

Страница 108: ...with archived data are displayed in the table Fig 91 To display the results select one job by clicking and highlighting the respective row in the Selection of results table Then change to the Results...

Страница 109: ...Using the XData Program M1 ORA MISTRAL 109 Fig 92 Data processing Results tab...

Страница 110: ...STRAL instruments can operate several hours without reducing the service life A standby mode is recommended only for waiting times 5 h but not absolutely necessary The instruments have no automatic st...

Страница 111: ...the rear panel of the instrument Malfunctions in the instrument or voltage fluctuations can cause a blow of this fuse This fuse could be the reason why the green power lamp on the front panel is not...

Страница 112: ...ntamination The stage should be cleaned only with non aggressive cleansing agents Caution The detector is located close above the measurement position It has a beryllium window which should never be t...

Страница 113: ...lifted and carried with the help of two people Caution Danger of instrument damage due to impacts coldness and moisture The transportation must be performed carefully The instrument must not be expose...

Страница 114: ...eryllium The disposal of these components must be executed by the manufacturer All components of the M1 ORA MISTRAL excepting the X ray tube and the detector are disposed as hazardous waste The compon...

Страница 115: ...ent Parts 1 M1 ORA M1 MISTRAL 1 Control computer Windows 7 control software programs XSpect Pro and XData 1 Mouse 1 Serial connection cable 1 Power connection cable 1 Instrument adjustment sample pure...

Страница 116: ...a year It is highly unlikely that the radiation worker dose limits will be exceeded when trained and qualified personnel use such devices Read the section Safety Instructions of this manual chapter 2...

Страница 117: ...tremely high doses cells cannot be replaced quickly enough and tissues fail to function Tissue sensitivity In general the radiation sensitivity of a tissue is proportional to the rate of proliferation...

Страница 118: ...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 expo...

Страница 119: ...al safety precautions 116 Hardware components 30 Installation Driver 40 Place of 13 33 Program 35 Requirements 33 XData 35 XSpect Pro 35 Instrument status bar 48 Integrity 107 Intended usage 10 Key sw...

Страница 120: ...tage control 50 Stage program Create 70 72 Edit 72 Load 70 Workspace 69 Stage program workspace 69 Standard delivery contents 115 Standard spectra 57 Standards 77 Load 78 New 79 Save 78 Standby mode 1...

Страница 121: ...Index M1 ORA MISTRAL 121 Control elements 48 Display elements 48 Installation 35 Start up 46 Using the program 46 X Y Z stage 51 Z stage Manual 50 Motorized 50...

Страница 122: ......

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