Laser-Induced Breakdown Spectroscopy LIBS2500plus Installation
Contents
1. 12 Other Software Installation 15 Imaging Module Camera 15 Crossfire Camera Driver ia sio eee dise eere eles cet eoe et breed dae da Fede dd deu o na an 15 System Sta Pe nt 15 Assigning Spectrometers neiere neiaa ar Ranie Le ee in 15 Loading the Element OBa rs a iaaa on cud ieee AA ARRA 18 166 00000 000 02 0108 Table of Contents Chapter 3 COO inm 19 OVENI W sass 19 Scip mc TU 19 Set SWIECI Delay sm 19 RISO 21 Set up Radiometric Information 22 Initial TEStNg 23 Using OOILIBSplus Software Modes 24 Pixel Correlation Mode nien Mte t e E ee Ea Ele daba teca d Hed eta Rn 24 Pixel Correlation Procedure creen tid ettet dide De ed td qe dk eed 25 luam 27 Elemental ID Procedure iier eme oeste eim used eae EL dab d 27 Peak Analysis E e ba Y eee edic e e ode a ra oe 28 Liries to Analyze Options Pel it Pet Ended eet d ETAR 28 Lines Informations e eoe een enden nione nenne ERE e pte eA a ee 29 Peak Analysis Procedure phe ie He EE ucl bd eee uid dips 29 Performing2. Network adapters Ocean Optics Devices 8100 Ocean Optics HR2000 Eprom Load E8 Ocean Optics HR2000 Eprom Load 880 Ocean Optics HR2000 Eprom Load E8 Ocean Optics HR2000 Eprom Load 88 Ocean Optics HR2000 Eprom Load 88 Ocean Optics HR2000 Eprom Load 8 Ocean Optics HR2000 Eprom Load a Ports COM amp LPT q Sound video and game controllers Storage volumes System devices 8 5 1 9 9 b Click on Ocean Optics Devices node If this node is absent expand USB Devices node Up to seven HR2000 Spectrometer entries should be visible depending on how many channels are in your LIBS system This indicates that the LIBS2500plus spectrometers have been properly installed Note If there are any yellow or red symbols next to each spectrometer entry then you must reinstall OOILIBSplus reboot the system and then reconnect the spectrometer 3 Inthe OOILIBSplus program select Tools Select Spectrometer Modules The HR2000 Configuration screen appears There are 8 possible spectrometer assignments However only the number of spectrometer channels that you have in your LIBS system are active 16 166 00000 000 02 0108 ptics mc it in Photonics 4 First 2 Installing the LIBS System HR2000 Configuration Unit Serial Number Unit Range Unit 7 ud E Unit C Unit D
3. 3 Unit E 71 Unit F ex Unit G xj Click on the arrow for the first box Unit A to see selection of up to 7 serial numbers corresponding to the number of spectrometer channels in your LIBS system Double click on the lowest number and assign it to the first space This is important in that it tells the software which serial number correlates to the lowest wavelength spectrometer The range box should display the range of the spectrometer this feature is not fully implemented Note If you mistakenly assign an incorrect serial number click on the text in the Unit Serial Number column for that serial number Highlight the text and delete it Then reassign the correct serial number Proceed to assign serial numbers in order of ascending serial numbers to Units B G depending on the number of spectrometer channels in your LIBS system Click the OK button when you have assigned all serial numbers You have now configured the Select Spectrometer Modules screen Exit OOILIBSplus software Restart OOILIBSplus software The range at the bottom of the screen should be about 200 980 nm If this is not the case or if you receive another error message refer to Chapter 4 Troubleshooting Otherwise you are ready to collect data 166 00000 000 02 0108 17 2 Installing the LIBS System Loading the Element Library IPtics inc First in Photonics The element library enable
4. em ennemis 47 TOONS 47 LAGS MEM EAA 48 Eorum Emm 48 Dialog Ball m 48 SOLEUS BAD 49 IC HB fno a 20 M 50 I d M 51 166 00000 000 02 0108 q ptics mc Table of Contents First in Photonics vi 166 00000 000 02 0108 About This Manual Document Purpose and Intended Audience This document provides the user of the LIBS2500plus for setting up calibrating and performing experiments with their system Document Summary Chapter Description Chapter 1 ntroduction Contains descriptive information about the LIBS2500plus system It also provides laser requirements and shipment components Chapter 2 Installing the LIBS System Provides installation and configuration instructions Chapter 3 Operation Contains instructions for operating the LIBS2500plus System Chapter 4 Troubleshooting Contains recommended steps to isolate and correct common problems Appendix A Specifications Provides product specification data Appendix B User Interface Contains a quick reference guide to the OOILIBSplus user interface features Product Related Documentation You can access documentation for Ocean Optics products by visiting o
5. Caution You MUST install the OOILIBSplus software application prior to connecting the LIBS System hardware to the PC The OOILIBSplus software installation installs the drivers required for HR2000 spectrometer installation If you do not install OOILIBSplus first the system will not properly recognize the spectrometers If you have already connected the spectrometers to the PC prior to installing OOILIBSplus software consult Chapter 4 Troubleshooting for information on correcting a corrupt HR2000 Spectrometer installation Procedure 1 Insert the OOILIBSplus CD that you received with your LIBS2500plus System and install the OOILIBSplus software The password for this software is on the back of the CD Jacket 2 Follow the prompts in the Installation Wizard to install the software Hardware Cabling Procedure 1 Plug the external 5 VDC power supply into the USB hub of the LIBS2500plus 12 166 00000 000 02 0108 ptics one 2 Installing the LIBS System EXT Q SWITCH EXT TRIGGER LAMP SYNC RECEPTACLE Rear Panel of 7 Channel Spectrometer Rack 2 Plug the USB cable into the USB port on the rear of the spectrometer rack then into the PC s USB port The computer s operating system will recognize the new hardware and load the appropriate drivers for each of the spectrometers in the LIBS system 3 Connect the fiber from the rear of the Sample Chamber or Crossfire system to each spectromet
6. Procedure 1 Check that the switches on the rear of the laser power supply are set for external triggering 2 Turn the laser power supply on making sure that the prf laser repetition rate is set to 0 the Q Switch is on and the power bar is adjusted to 5 bars 3 Push the Run button on the laser power supply The flash lamp capacitor should charge and remain idle while waiting for an external trigger 4 Open the door of the Sample Chamber and make sure that the laser power supply automatically shuts down 5 Close the Sample Chamber door and push the Run button again to recharge the flash lamp capacitors Insert a standard LIBS sample into the Sample Chamber In OOILIBSplus select Scan Type Single Shot from the menu bar In OOILIBSplus click the Scan button The laser should fire in the Sample Chamber ND In the Sample Chamber align the fiber optic assembly relative to the sample plasma to optimize sensitivity of the LIBS measurement 10 In OOILIBSplus select Tools Set Q Switch Delay from the menu bar This opens the Adjust Q Switch window displaying the signal based on the Q switch delay You can be sure that this is functioning properly by observing the change in continuum and emission strength as a function of delay settings both positive and negative 166 00000 000 02 0108 23 ptics mc it tonics 3 Operation 3 First in Photonics Adjust Q Switch Switch Delay us 80 000000
7. Dtics m First in Photonics Laser Induced Breakdown Spectroscopy LIBS2500plus Installation and Operation Manual Document Number 166 00000 000 02 0108 Offices Ocean Optics Inc World Headquarters 830 Douglas Ave Dunedin FL USA 34698 Phone 727 733 2447 Fax 727 733 3962 8 a m 8 p m Mon Thu 8 a m 6 p m Fri EST E mail Info OceanOptics com General sales inquiries Orders OceanOptics com Questions about orders TechSupport OceanOptics com Technical support HALMA GROUP COMPANY Additional Offices 137 Xianxia Road Suite 1802 Changning District Shanghai PRC 200051 Phone 86 21 5206 8686 Fax 86 21 5206 8686 E Mail Sun Ling OceanOptics com Geograaf 24 6921 EW DUIVEN The Netherlands Phone 31 0 26 3190500 Fax 31 0 26 3190505 E Mail Info OceanOpticsBV com Copyright O 2001 2008 Ocean Optics Inc All rights reserved No part of this publication may be reproduced stored in a retrieval system or transmitted by any means electronic mechanical photocopying recording or otherwise without written permission from Ocean Optics Inc This manual is sold as part of an order and subject to the condition that it shall not by way of trade or otherwise be lent re sold hired out or otherwise circulated without the prior consent of Ocean Optics Inc in any form of binding or cover other than that in which it is published Trademarks All products and services he
8. Wavelength nm These spectra are courtesy of the U S Army Research Laboratory and the U S Army Soldier and Biological Chemical Command LIBS2500plus Spectra of Anthrax SurrogatesBC Bacillus Cereus BG Bacillus Globigii BT Bacillus Thuringiensis Applications The LIBS technique is useful in areas such as e Environmental monitoring soil contamination particulates sediments e Materials analysis metals plastics slag glass e Forensics and biomedical studies teeth bones e Military and safety applications explosive particles chemical and biological warfare agents e Art restoration conservation pigments precious ancient metals e Metrology silicone wafers semiconductor materials e Bioresearch plants grains LIBS Components Ocean Optics LIBS functionality can be purchased as a complete system including the spectrometers and related fibers laser LIBS Imaging Module and OOILIBSplus software The system is also completely customizable The modular nature of the LIBS2500plus system allows you to purchase just the spectrometer Users can then provide their own fixtures and or Q switched laser You can specify the number of spectrometers 1 7 as well as their gratings lenses slits and filters Contact an Ocean Optics Application Scientist for more information on customizing your LIBS System 166 00000 000 02 0108 IPtics inc 1 Introduction First in Photonics LIBS Spe
9. 47 Library Options Element ID menu 46 Library Options menu 46 LIBS2500plus Controller 4 Lines Information 29 Lines to Analyze options 28 menu Background 45 Background Mode 46 File 41 Library Options 46 Library Options Correlation 47 Library Options Element ID 46 Mode 45 Overlay 44 ScanType 44 Stage 48 Tools 47 View 43 Mode menu 45 OOILIBS 1 2 6 freeze 38 installation 12 lock up 38 operation 1 19 options Lines to Analyze 28 Overlay sub menu 44 p Peak Analysis 28 procedure 29 Pixel Correlation 24 product related documentation vii Q Q Switch delay 19 52 ptics mc it in Photonics First radiometric setup 22 remove improperly installed files 35 unknown device 34 S safety glasses 7 sample chamber 6 setup 10 samples add to library 31 save library 33 ScanType menu 44 setup hardware 9 setup options 21 software 6 Crossfire camera driver 15 imaging module camera driver 15 installation 12 software modes 24 Element ID 27 Peak Analysis 28 Pixel Correlation 24 software troubleshooting 38 specifications 39 spectrometer cabling 13 channels 5 configuration 16 troubleshooting 36 spectrometers 4 Stage menu 48 Status bar 49 system start up 15 T testing 23 Tool bar 48 Tools menu 47 troubleshooting 34 166 00000 000 02 0108 ptics mc First in Photonics Index laser 36 remov
10. Left 0 Cursor Right 0 Cursor Update Wavelength nm Switch Delay 20 0 2 Verify that data from the Element ID Library appears in the Element Line List 18 166 00000 000 02 0108 Chapter 3 Operation Overview Laser Induced Breakdown Spectroscopy LIBS is based on the interaction of a laser with a sample to produce an optical emission spectrum specific to that sample A pulsed laser focused onto a solid liquid or gas sample vaporizes a small portion of that sample for analysis The super heated ablated material is transformed into plasma Plasma is a form of matter in which the original chemical bonds of the substance are broken apart and the resulting atoms are converted into a mixture of neutral atoms ions and electrons The atoms and ions within the expanding plasma release some of their energy by emitting light which produces a characteristic emission spectrum in the UV VIS and NIR spectral range Configuration Set Q Switch Delay The Q Switch enables you to control laser firing from an external device and is the means by which the OOILIBSplus application controls timing of the ablation process To facilitate this timing you must configure the Q Switch delay setting to insure that the spectrometers begin acquiring spectral data at the optimal time within the lifespan of the plasma Theoretically this delay is the period of time after the laser vaporizes the material and the spectrometer begins acquiring data
11. New Library Creates a new correlation library Save Library Saves the correlation library Load Library Loads a correlation library Tools Menu Tools Help Set Q Switch Delay Select Spectrometer Modules Setup Options Menu Option Description Set Q Switch Delay Opens the Adjust Q Switch window Select Spectrometer Modules Selects the serial numbers of the spectrometers to be used Setup Options Sets up general options for OOILIBSplus software Setup Radiometric Calibration Sets up the radiometric calibration options 166 00000 000 02 0108 47 ptics mc t tonics First in Phot B User Interface Stage Menu Control Move Stage Menu Option Description Control Opens the Sample Chamber stage control window Move Stage Automatically moves the stage during sampling Only available on the closed loop sample chamber Tool Bar The OOILIBSplus tool bar located at the top of the screen features the following options Icon Description amp Prints the contents of the graph window Saves the contents of the graph window Scale the contents of the graph window according to the highest and lowest readings i Auto scales the contents of the graph window fi Scales the contents of the graph window according to the highest readings Dialog Bar Int Time
12. Pixel Correlation Correlation Results View Sample Correlate Linear Rank From this point you can add a sample to the correlation library Adding Samples to the Correlation Library Procedure 1 Click the More button to expand the Pixel Correlation window Notice that the library is currently empty indicated by the empty correlation results list 166 00000 000 02 0108 31 ptics mc First in Photonics 3 Operation Pixel Correlation Correlation Results Same View Samp Correlate Linear Rank Add Sample Delete Sample ____SaveResuts You can now add samples to the library 2 Click the Add Sample button The Scan button changes to a Save Samp button aAA 3 Set the number of scans to average and click the Save Samp button A dialog box opens 4 Enter the name of the sample in the dialog box and click the OK button You are then prompted to enter a name for the sample Enter a name for this Sample Libray Sample Creation Assign a name that is indicative of the sample it will be representing If you do not want to name the sample click the Cancel button to abort the sampling process 32 166 00000 000 02 0108 ptics mc it in Photonics First 3 Operation The new sample then appears in the list in the Correlation Results window Click the Scan button to update the list with the results of the scan of your sample You sh
13. Previous Switch Delay 80 000000 5 11 In OOILIBSplus select Scan Type Continuous from the menu bar 12 Change the power settings on the laser power supply and verify that the power adjusts accordingly You should hear a pop of the laser in the Sample Chamber indicating a change in power Cane 13 Click the button in OOILIBSplus to test the LED targeting sources Using OOILIBSplus Software Modes The mode windows Mode menu selection or analysis windows provide multiple ways of analyzing LIBS data When you select a mode from the Mode menu the control window for that mode opens You can then analyze your data You can have multiple windows open at once but only the current mode will automatically update after each scan You will need to manually configure the other windows to update with each new scan Pixel Correlation Mode Option Description Correlation Displays the library entries and their correlation coefficient comparing each to the Results current sample in memory View Sample Displays the selected library entry in the graph window Correlate Correlates the sample in memory against the current library Linear Rank Two different methods of correlation 24 166 00000 000 02 0108 ptics mc First in Photonics 3 Operation Option Description More Less Changes the size of the window Allows you to shrink the window to allow better viewing
14. RR EH REP vii Document Purpose and Intended vii Docurnent SUrmaly d eL rete ide e e ne er ere pfe din vii Product Related Documentation vii SS viii Chapter 1 Introductioh 1 Prod ct OVerview ian a a i aa i e e E CU anes 1 How the LIBS2500plus 1 Advantages of Broadband LIBS Techniques 1 LIBS Emission ID t Leti Mae ae ee 2 Applications HERR 3 EIBS Gomporientss ederet ites teste fedet Feu be ha ade 3 ABS Spectromelters 4 Laser Requirements for LIBS2500plus sss emen 5 LIBS Sample Chamber rtt REP Hia et bie rie ade 6 LIBS Imaging Modula 4 iioii iuter Hte uH perm HERR bitu e fedet ide 6 OOIEIBSpluS SOftWAare 3 ent eoi abest t ree ead geek rite ted ce res bebe ede 6 Other Required 7 Additional Recommended 7 Chapter 2 Installing the LIBS System 9 OVSTVIOW M e reci ebbe Pub e vire desc e Poetae 9 Hardware Set Up aote reote be t o 9 Software Installation 12 iue rumor
15. Remove the USB devices from the PC 2 Remove all installed Ocean Optics USB drivers 3 Restart the system 4 Ensure that OOILIBSplus is installed then reconnect the LIBS2500plus spectrometers to the PC 36 166 00000 000 02 0108 ptics mc t in Photonics First 4 Troubleshooting System Prompts for ezusb sys or an inf File Problem During installation the system is requesting a file named ezusb sys or an INF file Probable Cause The system cannot locate the USB drivers or INF files Solution Navigate to the appropriate directory for each file For the ezusb sys file e Windows 98 ME C windows system32 drivers Windows 2 Directory may be winnt instead of windows other information the same For the INF file e Windows 98 ME C windows inf or C windows inf other Windows 2 Directory may be winnt instead of windows other information the same Verifying Device Setup Problem How do I verify that the devices have been setup correctly Solution Procedure Follow the steps below to verify device installation 1 Navigate to Start Settings Control Panel 2 Double click on the System icon 3 Select the Device Manager tab Windows 98 ME or click the Device Manager button Windows 2K XP A list of installed devices appears 4 Expand the USB Devices tree The Ocean Optics HR2000 should be listed several times depending on the number of spe
16. optimal setting Dual Pulse Indicates whether or not a secondary pulse laser will be implemented in the scan Laser 2 Delay The amount of time in microseconds allotted to the secondary pulse laser before it fires This number is plotted from the same zero point as the Laser 1 Delay allowing this laser to be fired before or after Laser 1 Set button Calculates the Q Switch Zero point from the Laser 1 and Laser 2 Delay settings The spectrometer s internal clock operates on 41667 ys pulses and all time based events occur at a multiple of that value For this reason the values entered for Laser 1 and Laser 2 Delay will be reformatted to display the actual time interpreted by the spectrometer Orig Integration Start Delay 20 Displays the last saved value of the Integration Start Delay in microseconds 166 00000 000 02 0108 ptics mc First in Photonics 3 Operation Option Description Integration Start Delay Displays the current position of the Integration Start Delay slider bar Cumulative Q Switch Displays the entire delay time representing the Q Switch Delay Delay Slider Bar Increases or decreases the Integration Start Delay in 41667 us intervals Procedure 1 Enter a Laser 1 Delay setting taking into consideration Big Sky Laser s recommended setting 2 Enter a Laser 2 Delay setting taking into account the desired delta between the two pul
17. pop 37 ME 37 iv 166 00000 000 02 0108 ptics mc it in Photonics First Table of Contents OOILIBSplus Software Troubleshooting eeeeceeeeeee 38 Program Keeps Freezing or Locking Up 38 ie 38 Probable Causo osso nia A 38 e 38 Appendix A 39 Appendix B User 41 41 File 41 Save MER 42 EXpOrt SUB MENU mE 43 VSW cian 43 Overlay SUB MENU coh decking i ette ede er iba p irae ERE C 44 Scan Type ette dte ea edet aen ases e 44 Mi IM 45 Background Men er ihre a RO EE eu n PSOE ed RN 45 Background Mode nenne enne eren nemen nnne en neret nis 46 Library Options 46 Library Options Element ID eren 46 Library Options Correlation
18. when not adding new samples Add Sample Adds a new sample to the current library Click the Scan button to take a scan After the scan is complete you will be asked to enter a name for the sample Once you enter a name the sample is added to the library Remember to save the library Library Options Correlation Linear Correlation Save Library Delete Sample Deletes the selected sample from the library After deleting a sample the changes to the library are not saved Save the changes Library Options Correlation Linear Correlation Save Library Start Range Specifies the beginning boundary used in the correlation End Range Specifies the end boundary used in the correlation Pixel Correlation Procedure Procedure Follow the steps below to use the Pixel Correlation Mode 1 Select Mode Pix Correlation from the menu Pixel Correlation Correlation Results Sample Coef View Sample Correlate Linear Rank 2 Click the More button 166 00000 000 02 0108 25 ptics mc 3 Operation First in Photonics Pixel Correlation Correlation Results Same View Samp Correlate Linear Rank Add Sample Delete Sample Save Results 3 Click the Add Sample button The Scan button now changes to a Sample button 4 Set the number of averages you want to use then click the Save Sample button 5 Enter a library name f
19. Averages Shot Count 2 fi fi Clean 48 166 00000 000 02 0108 Fist in Photonics B User Interface Icon Description Int Time Displays the integration time in Spectrometer Mode Averages Displays the averages of the specified number of scans all modes Shot Count Displays the number of shots to take and the average Single and Continuous Shot Modes Allows you to manually take a scan Single Shot Mode Resets the spectrometer in the event that a trigger is missed Not used Clean Takes the specified number of cleaning shots This option is configured in the Setup Options window Turns the alignment light on or off Status Bar Wavelength 474 973 Counts 70 5333 Pixel 5215 Q Switch Delay 0 0 The OOILIBSplus Status Bar located at the bottom of the screen features the following options Option Description Wavelength 474 973 Counts 70 5333 Pixel 5215 Displays the wavelength counts _ and pixel number of the current cursor location O Switch Delay 0 0 Displays the current Q Switch delay Displays the current Continuous Save File name when in use 166 00000 000 02 0108 49 IPtics inc it in Photonics B User Interface Firs Graph Window Counts 4000 Wavelength nm The OOILIBSplus Grap
20. Correlation in 5 30 Accessing the Correlation eee nnne 30 Adding Samples to the Correlation 31 Saving the Correlation 33 Correlation 33 Chapter 4 Troubleshooting nennen 34 UENIT EEEEMTMMTMMSM 34 HR2000 Connected to PC Prior to OOILIBSplus Installation 34 Remove the Unknown Device from Windows Device 34 Remove Improperly Installed 35 Laser 36 Problemi 36 Probable Or UR 36 36 Spectrometer Troubleshooting 36 Continuous Beeping from eene eene 36 Problemi HET 36 Probable Cause LR 36 SOLUTION 36 System Prompts for ezusb sys or an 37 37 Probable Cau Se ee eae 37 P 37 Verifying Device 1 37 Proble ued
21. First in Photonics B User Interface Background Mode Menu Background Library Options Tools Help Sampled Background Dark Load Sampled Background Add Sampled Background Mix Sample Background Menu Option Description None No background subtraction Sampled Sampled background subtraction loaded using Background Menu options Background Dark Dark subtraction uses the masked pixels of each detector as the background Note If hot pixels spikes on the graph are observed use dark subtraction Background Mode Dark to remove them Library Options Menu Library Options Element ID gt Correlation gt Menu Option Description Element ID Brings up the Element ID library menu see Library Options Element ID Menu Correlation Brings up the Correlation library menu see Library Options Correlation Menu Library Options Element ID Menu Library Options dese Tools Help Element ID gt Load Library Correlation 46 166 00000 000 02 0108 ptics mc First in Photonics B User Interface Menu Option Description Load Library Loads an Element ID library Analyze For future use Library Options Correlation Menu Library Options isa Tools Help Element ID gt Linear Correlation gt New Library Save Library Load Library Menu Option Description
22. a line from the left and right points then subtracts that value from the peak Mean average intensity of all count scans taken Std Dev Standard deviation of all count scans taken Residual standard deviation of all count scans taken Integrated values calculated by adding the intensities from the L Wave to the R Wave All Intg calculations are based on this value 28 166 00000 000 02 0108 ptics mc First in Photonics 4 3 Operation Count Number of scans taken for each line This value is used in the calculations described above Lines Information Wavelength Wavelength assigned to the currently selected line You can change this value and set the custom value for a custom line Place the graph cursor at the desired position and click the cursor button to set this value Left wavelength or L Wave Place the graph cursor at the desired position and click the cursor button to set this value Right wavelength or R Wave Place the graph cursor at the desired position and click the cursor button to set this value Save the information to the currently selected line No changes will be made until you Click the update button Peak Analysis Procedure Procedure Follow the instruction below to use the Peak Analysis Mode 1 Select Mode Peak Analysis from the menu The Peak Analysis screen appears 166 00000 000 02 0108 29 ptics mc First in Photoni
23. a BNC tee Ext Q Sw EXT Q SWITCH This cable connects to the external Q switch of the laser It fires the Q switch under software control Most lasers have a switch that must be set to allow this to happen If only an external trigger input is available you do not need to use this line but you will have no control over the Q Switch event 7 Connect one end of the BNC cable to the LIBS Sample Chamber Remove the cap from the Remote Interlock Remote Intlk connector on the back of the laser power supply and attach the other end of the BNC cable Remote e 31 e S 4 A q a b ya 5 4D 9 7 o 26 1 y U a0 I LIBS Sample Chamber Connecting LIBS Sample Chamber to the Laser Power Supply and Inert Gas 8 Install the fiber optic assembly in the Sample Chamber and roughly align 9 Ensure that the switches on the rear of the laser power supply are set for external triggering 10 If you intend to use inert gas in your set up connect the gas tank to the LIBS Sample Chamber 14 166 00000 000 02 0108 ptics mc Z t in Photonics First 2 Installing the LIBS System Other Software Installation Imaging Module Camera Driver If you are using the imaging module install the driver for the imaging module camera Crossfire Camera Driver If you are using the Crossfire system you must install its camera driv
24. allowing the plasma sufficient cooling time In practice there are a number of factors that constitute this delay Upon receiving the signal to fire the laser requires a period of time on the magnitude of microseconds to reach maximum power and fire With a dual pulsed system there is also the delay time between the firing of the first and second laser pulse to be considered Determining the amount of time needed to reach that precise point of time when the laser has fired and produced the beginnings of plasma is known as Q Switch Zeroing The amount of time from Q Switch Zero until the spectrometer begins acquiring data is the Integration Start Delay The Q Switch window allows you to set the position of the firing of the laser with respect to the opening of the electronic aperture If you do not hear the laser firing it is most likely due to an improper setting of the Q Switch 166 00000 000 02 0108 19 3 Operation Adjust Q Switch ptics mc First in Photonics Switch Zero Orig Integration Start Delay us 340 Laser 1 Delay us 13458 Integration Start Delay 2 99 Dual Pulse Laser 2 Delay 135 83 Cumulative Q Switch Del umulative Q Switch Delay Set Cancel Option Description Laser 1 Delay The amount of time in microseconds allotted to the primary pulse laser to charge its flash lamps before firing Refer to Big Sky Laser s specification for the
25. can replace this file with custom code Saturation Detect Displays a message if the spectrum is saturated Continuous Laser Mode Instructs the software to use the Continuous Laser mode Only use this mode with laser systems that must continuously fire the flash lamp Time Between Samples Continuous Mode Delay that occurs after a scan in Continuous mode and prior to the next Scan Delay Between Scans Averaging Delay between scans on any type of scan averaging shot count etc Use Radiometric Calibration Enables the radiometric calibration files Set up Radiometric Information Use this screen to assign calibration files to each channel Radiometric Calibration Radiometric Calibration File 2000 qUVcd o o HR2000 2VlScal 0 Radiometric Adj Cancel To use the Radiometric Calibration screen select the calibration files for each channel using the browse button located between the two columns 22 166 00000 000 02 0108 ptics mc it in Photonics First 3 Operation The first radiometric calibration file is for Spectrometer Unit A the second file is for Spectrometer Unit B etc You can also apply a channel specific Radiometric Adjustment to scale the calibrated data Initial Testing Once you have set up your LIBS2500plus system and configured it you are ready to perform initial testing with a sample
26. cs 3 Operation Element Line List Scans for Selected Line Element Wavelength Pixel Counts Intg Counts Add Clear Calculations AddCustom Custom Save Calculations Delete Load List Ae Save List Lines To Analyze Element Wave LWave A Wave StdDev RSD_ Intg Mean Intg Std Dev Intg RSD Count Line Information Wavelength 0 Cursor Left 0 Cursor Right 0 Cursor Update 2 Select a line from the element list then click the Add button Repeat this step until you have loaded all the desired lines 3 Modify any properties the L Wave the R Wave or set the Wavelength value for custom waves 4 Click the Update button to save the changes 5 Click the Scan button repeatedly You should begin to see data appear in the Lines to Analyze section Performing Correlation in OOILIBSplus Follow the instructions in the sections below to perform a correlation in OOILIBSplus e Accessing the Correlation Window e Adding Samples to the Correlation Library e Saving the Correlation Library Accessing the Correlation Window Procedure 1 Start the OOILIBSplus software 2 Obtain a few samples to make sure that the system is working correctly 30 166 00000 000 02 0108 ptics mc it Photonics First 3 Operation 3 Then select Pix Correlation from the Mode menu available from the OOILIBSplus menu bar The main Pixel Correlation window appears
27. ction but it cannot be loaded for overlays or display Continuous Save Starts Continuous Save When activated each scan is saved with a file appended with an incremental file number 166 00000 000 02 0108 41 B User Interface ptics mc First in Photonics Menu Option Description Save Graph Tags Load Graph Tags Export Save Grams Print Spectrum Prints the spectrum displayed in the graph window Exit Exits the program Save Sub Menu Ell OOI LIBS LIBS 2000 V4 5 0 7 Open Spectrum Save Graph Tags Load Graph Tags Export Print Spectrum Exit i View ScanType Mode Background Libr Save Spectrum Save Background Continuous Save Menu Option Description Save Spectrum Saves a spectrum file ols You can load this file into overlays or opened it directly Save Background Saves a background spectrum You can use this for background subtraction but it cannot be loaded for overlays or display Continuous Save Starts Continuous Save When activated each scan is saved with a file appended with an incremental file number 42 166 00000 000 02 0108 ptics mc First in Photonics B User Interface Export Sub Menu 00I LIBS LIBS 2000 V4 5 0 7 I View ScanType Mode Background Open Spectrum Save gt Shot Count 1 Save Graph Tags L
28. ctrometers As lower cost options LIBS2500plus Systems are available with fewer than seven channels see table below with a narrower wavelength range for element specific analyses Depending on the range of your analyses you may require a system LIBS2500plus 1 at a significantly lower cost You can turn your HR2000 Spectrometer into a 1 channel LIBS System LIBS2500 1PLUS with the LIB2500plus Controller and the following equipment e LIBS Sample Chamber LIBS SC e LIBS Laser 200mJ or 50 mJ e LIBS Imaging Module LIBS IM USB LIBS Controller Cables Contact Ocean Optics to return your HR2000 to the factory for a firmware upgrade and the required LIBS equipment to upgrade your HR2000 Spectrometer to a LIBS2500 1PLUS Fiber Bundles LIBS Fiber Bundles Item LIBS System Description Optical Fiber Bundle LIBS2500 7PLUS 7 channel LIBS System includes all channels A G LIBS BUN 7 LIBS2500 6PLUS 6 channel LIBS System choose 6 channels from A G LIBS BUN 6 LIBS2500 5PLUS 5 channel LIBS System choose 5 channels from LIBS BUN 5 LIBS2500 4PLUS 4 channel LIBS System choose 4 channels from A G LIBS BUN 4 LIBS2500 3PLUS 3 channel LIBS System choose 3 channels from A G LIBS BUN 3 LIBS2500 2PLUS 2 channel LIBS System choose 2 channels from BIF600 2 UV VIS LIBS2500 1PLUS 1 channel LIBS System choose 1 channel from A G P600 2 UV VIS LIBS2500plus 1 channel co
29. ctrometers in your system 5 Verify that there are no entries with yellow or red warning symbols next to them If this is the case the devices are correctly installed If this is not the case follow the instructions in Remove Improperly Installed Files You have now verified device setup 166 00000 000 02 0108 37 ptics mc t tonics First in Phot 4 Troubleshooting OOILIBSplus Software Troubleshooting Program Keeps Freezing or Locking Up Problem The OOILIBSplus software keeps freezing or locking up Probable Cause Multiple causes Solution Procedure 1 Click on the Reset button If the system unfreezes the problem is solved 2 Reboot the computer You must also reset the spectrometer system by disconnecting the USB cable and power from the PC 3 Verify that the Lamp Sync trigger is being transmitted to the spectrometer 4 Ensure that the same serial numbers are not assigned twice in the Select Spectrometer Modules window 38 166 00000 000 02 0108 Specification Appendix A Specifications Value Dimensions for 7 channel version LxWxH 33 4 cm x 15 x 14 13 2 x 5 9 5 5 in Weight for 7 channel version 6 36 kg 14 1 Ibs Spectrometer range 200 980 nm Resolution 0 1 nm FWHM Detection CCDs with a combined 14 336 pixels Frame rate 10 Hz capability computer controlled Integration time 2 1 ms variable in the fr
30. e Element Counts Wavelength Element Lines Start nm 0 Cursor End nm 0 Cursor Update Analyze i ao Search Width 13 pixels Peak Height Q counts 2 Click the Scan button You should now have a list of lines detected in the left window of the Element Identification window If you do not obtain this data increase the search width or decrease the peak height 166 00000 000 02 0108 27 ptics mc 3 Operation First in Photonics Peak Analysis Mode Elements List Displays a list of all elements in the Elemental Library Scans for Selected Displays the individual scan data for the selected lines in the Lines to Analyze Line window Adds the selected elements from the Elements List to the Lines to Analyze list Add Custom Adds a blank element to the Lines to Analyze list You must set the wavelength after adding a custom type Removes the selected line from the Lines to Analyze list Saves the list of lines to an ASCII file allowing you to load it later Load List Loads the saved list of lines Lines to Analyze Displays the list of lines for analysis including the Element Name Wavelength and several other values see table below Clear Calculations Clear the calculations Save Calculation Save the calculations to an ASCII file Lines to Analyze Options L Wave R Wave Left and right side of the peak used to subtract background The system draws
31. e 34 OOILIBS 38 upgrades viii spectrometer 36 user interface 41 unknown device View menu 43 166 00000 000 02 0108 53 lt ptics mc Index First in Photonics 54 166 00000 000 02 0108
32. e Hide System Files and Folders and Hide File Extensions for Known File Types options in Windows Folder Options Access Windows Folder Options from Windows Explorer under the Tools Folder Options menu selection 4 5 6 7 Delete the OOL_USB INF in the INF directory If your computer is running either the Windows 2000 or XP operating system you must also delete the USB PNF file in the INF directory Navigate to the Windows System32 Drivers directory Delete the EZUSB SYS file Reinstall your Ocean Optics application and reboot the system when prompted Plug in the USB device The system is now able to locate and install the correct drivers for the USB device 166 00000 000 02 0108 35 ptics mc t tonics First in Phot 4 Troubleshooting Laser Troubleshooting Problem The laser will not start Probable Cause On water cooled lasers bubbles may have developed in the cooling system This will prevent water from traveling to the laser head and result in a nonfunctional laser Solution Procedure 1 Tilt the power supply of the laser 30 degrees right or left 2 Allow the power supply to remain in that position until the bubbles clear 3 Try to start the laser again Spectrometer Troubleshooting Continuous Beeping from System Problem The system is continuously beeping Probable Cause The PC cannot communicate with the USB devices Solution Procedure 1
33. e top of the sample chamber with three bolts The replace the imaging module cover 4 Install the LIBS laser as follows Big Sky Laser Mount the laser head on top of the LIBS Imaging Module if purchased or directly on top of the sample chamber if you do not have an imaging module If you are using a 50 mJ laser a mounting bracket is attached to the laser head with steel rods to facilitate mounting and laser alignment into the sample chamber If you are using a 200 mJ laser fasten the laser s mounting plate to the top of the imaging module or the sample chamber if you do not have an imaging module then attach the laser to the mounting plate Crossfire Laser Place it on a stable flat surface separately from the sample chamber and imaging module Mounting Rods ar M Laser LIBS Imaging _ Module LIBS Sample Chamber Example of a 50 mJ Laser Installation Rear View 5 Fill the laser power supply with distilled coolant water See the manual that accompanied your laser for more information 6 Go on to Software Installation 166 00000 000 02 0108 11 ptics mc tonics 2 Installing the LIBS System First in Pho Software Installation OOILIBSplus Software was designed specifically for the LIBS2500plus System It records and stores data for export to Microsoft Excel and similar programs using the standard Microsoft commands such as File Save File Print etc
34. ee run mode Trigger delay 121 us to 135 us in 500 ns steps computer controlled Trigger jitter 250 ns Trigger level TTL not to exceed 5 5 V Computer connection USB 1 1 in all computers Software OOILIBSplus Power requirement 5 volts at lt 1 amp power supply included Input optical fiber 2 meter multimode sampling probe with SMA connector and collimating lens Size for 7 Channels 84HP x 3U Rack Housing with handles 130 mm x 483 mm x 350 mm Certification CE 166 00000 000 02 0108 39 B User Interface 40 ptics mc First in Photonics 166 00000 000 02 0108 Appendix B User Interface Menu Bar The OOILIBSplus Menu Bar is located at the top of the OOILIBSplus screen and features the following options Fie View ScanType Mode Background Library Options Tools Help File Menu E OO LIBS LIBS 2000 4 5 0 7 gi View ScanType Mode Background Open Spectrum Save gt Shot Count 1 Save Graph Tags Load Graph Tags Export gt Print Spectrum Exit Menu Option Description Open Spectrum Opens a Saved Spectrum file and displays it in the graph You can analyze this data Save Allows you to save data on your graph Save Spectrum Saves a spectrum file ols You can load this file into overlays or opened it directly Save Background Saves a background spectrum You can use this for background subtra
35. elengths back to 0 e There are two methods of correlation Linear and Rank Rank is more powerful but you should experiment with Linear to see how your results differ Switch between modes by toggling the button between Linear and Rank e You may receive better results by taking multiple single shots then loading the shots into their library rather than averaging a single sample into the library For instance if you are sampling stone you would add a sample called Stone 1 Then you would move the stone to a different spot and take another sample saving it as Stone 2 etc This way you have several samples of the same material A scan that identifies any of these materials will return a match for stone 166 00000 000 02 0108 33 Chapter 4 Troubleshooting Overview The following sections contain information on troubleshooting issues you may encounter when using the LIBS2500plus system If the suggested solutions do not correct the situation contact Ocean Optics Technical Support HR2000 Connected to PC Prior to OOILIBSplus Installation If you connected your Ocean Optics USB device s to the computer prior to installing your Ocean Optics software application you may encounter installation issues that you must correct before your Ocean Optics device will operate properly Follow the applicable steps below to remove the incorrectly installed device device driver and installation files Note If these procedures do not co
36. er channel s SMA connector on the front of the spectrometer rack 4 Start the OOILIBSplus software and configure your spectrometers see System Start up 5 Attach the laser cables from the laser to the laser power supply See your laser s documentation for specific instructions 6 Using the supplied BNC cables attach them to the connectors on the back of the laser power supply then connect them to the rear panel of the spectrometer rack as described in the following table Caution Beware of lasers that use negative logic and or high voltage outputs Lamp Sync signals as high as 33 volts have been observed in testing and the electronics in the LIBS2500plus may not survive pulse voltages of this intensity The spectrometer electronics are designed to drive the 50ohm loads normally associated with BNC connectors and all signals are 5V TTL Laser Connection Spectrometer Function Connection Ext Trig EXT TRIG This cable is connected to the external trigger connection of the laser It initiates a laser fire 166 00000 000 02 0108 13 ptics mc First in Photonics 2 Installing the LIBS System Laser Connection Spectrometer Function Connection Lamp Sync LAMP SYNC This cable is connected to the laser s strobe synchronization output It tells the spectrometer the exact time the strobe is firing If such a line is not available connect this to the Laser Trigger OUT cable using
37. er and software Procedure 1 Install the Crossfire camera driver CameraDriver Windows warns you that this is a nonapproved device Choose Continue Anyway 2 Install Microsoft NET framework dotnetfx 3 Install Crossfire s oView software oViewSetup Do not run oView software at this time System Start up When you first use the HR2000 Spectrometer s for the LIBS2500plus on this computer you must assign each spectrometer to specific channels and load the element library Assigning Spectrometers Procedure 1 Start the OOILIBSplus program You may receive an error message the first time you start the software This is normal Continue to Step 2 2 Confirm that the spectrometers have installed properly To do this a Navigate to Control Panel System or right click on My Computer and select Properties For Windows 2000 XP Click the Hardware tab then click the Device Manager button For Other Windows Versions Click the Device Manager tab The System Properties screen appears 166 00000 000 02 0108 15 ptics mc 2 Installing the LIBS System Lon Device Manager Of x Action View i JEREMY Computer Disk drives 5 Display adapters aay 23 DVD CD ROM drives Floppy disk controllers Floppy disk drives 52 IDE ATA ATAPI controllers Keyboards 9 Mice and other pointing devices Monitors
38. h Window located in the center of the screen features the following options e In the main display window the X axis represents Wavelength and the Y axis represents Counts or arbitrary intensity if Use Radiometric Calibration is checked e Click directly on the graph window to place the cursor at a specific point e Double click on the graph window to reset the zoom ranges e Hold the both the SHIFT and left mouse buttons down then drag and outline a region to zoom in on that region 50 166 00000 000 02 0108 applications 3 B Background Mode menu 46 Background menu 45 beep 36 broadband 1 C cabling 12 components 3 configuration 19 controller 4 correlation library 31 33 performing in OOILIBS 30 tips 33 window 30 D Device Manager 15 34 Dialog bar 48 document audience vii purpose vii summary vii Element ID 27 element library 18 emission ID 2 equipment other required 7 recommended 7 ezusb sys file 37 166 00000 000 02 0108 Index fiber bundles 4 File menu 41 graph window 50 hardware cabling 12 setup 9 hardware setup 10 HR2000 4 34 configuration 16 imaging module 1 6 setup 11 inert gas 7 inf file 37 installation 9 hardware 12 software 11 12 laser 1 Big Sky 5 cabling 13 Crossfire 5 mounting 11 requirements 5 setup 11 troubleshooting 36 library add samples 31 saving 33 51 Index Library Options Correlation menu
39. he continuum will not mask the line structure During this time the higher order transitions decay away leaving mostly I and II atomic emissions These are the ones that are identified Also entering into the emissions from the elements in the interrogated plasma are the collision dynamics of the plasma Rate equations can be used to analyze the target but emission signatures sample standards and correlation techniques are preferred to identify materials with the OOILIBSplus Software Elemental analysis and identification are very important in understanding content and in some cases are used for quantitative analysis To perform analysis and identification you must use an element catalog to help determine when a particular element is present We use a catalog that was derived from the NIST and other wavelength tables It consists of the persistent lines of the elements from spark spectra and is the closest to a complete catalog of the brightest lines around the temperature of the decayed plasma How can we be sure that the identified elements are actually present OOILIBSplus software contains two rating mechanisms e first rating mechanism indicates how many lines of those in our persistent line set are present Thus if 5 of 7 possible have been identified you can be fairly certain that this particular element is present If one of 7 is present could it be something else Perhaps a line that is not in our catalog from another specie
40. in Photonics First 1 Introduction e Additional Features Control of when to sample the plasma during its decay radiometric calibration of the spectrometers and method saving features to set and perform procedures for an entire sample test NOTE At the present time there are only qualitative methods for obtaining percentage composition of the elements Other Required Equipment Q Personal computer With Windows 98 Me 2000 XP operating system Additional Recommended Equipment Q Inert Gas Tank and Cable Supplies inert gas to the LIBS Sample Chamber for ablation area purge Q Laser Safety Glasses Although the LIBS Sample Chamber is constructed of special safety glass to protect you from the laser it is recommended that you purchase laser safety glasses rated for Nd YAG laser applications OD6 1064 to use whenever you are working with a Class 3 or above laser 166 00000 000 02 0108 7 q ptics mc 1 Introduction First in Photonics 8 166 00000 000 02 0108 Chapter 2 Installing the LIBS System Overview In general installing the LIBS2500plus involves the following steps Procedure l 2 Unpack and set up the LIBS2500plus components See Hardware Set up Install the OOILIBSplus software on the PC you intend to use with your LIBS2500plus System and then restart the PC See Software Installation Connect the cables to the appropriate connectors on the LIBS2500plu
41. ines of spark spectra We are investigating other spectral library packages e Reference Correlation by Full Pixel The Reference Correlation feature allows for real time matching of a complete spectrum with spectra in a user generated library You can compare the full spectrum produced by your sample to those in the library and the software instantly provides the match with the closest composition the correlation coefficient and a list of all other close matches The reference full pixel library is limited to a specific LIBS2500plus spectrometer channel e Reference Correlation by Spectral Line This version of the Reference Correlation feature is wavelength based not pixel based You can set various parameters to identify the presence of a specific line or lines for wavelength matching The spectral library can be shared among many spectrometers even those with different ranges e Line Tracking Over Multiple Samples This feature allows you to track the height from one to thousands of chosen lines over many spectra and perform statistical analysis for identifying and tracking various elements in samples e Time Dependent Analysis This feature performs analysis of the time decay of the plasma The spectrometer takes a set of data while delaying the point in which the spectrometer looks at the plasma after the laser fires You can then plot progressive decay or differential decay 6 166 00000 000 02 0108 ptics mc it
42. is broadband high resolution instrument allows for spectral analysis from 200 980 nm with resolution of 0 1 nm FWHM Sensitivity has been reported to parts per billion and picogram levels The LIBS 2500plus consists of 1 to 7 spectrometer channels and operates with any 32 bit USB compatible Windows PC We provide OOILIBSplus Application Software with spectral saving and data logging capabilities for operating the LIBS2500plus and for firing the laser Correlation Software provides instant material identification when using the LIBS2500plus and a spectral library consisting of 2500 atomic emission lines from the NIST National Institute of Standards and Technology tables for elemental identification The LIBS Imaging Module is available for use with the LIBS system to enable you to precisely adjust the laser to focus on the exact spot on the sample that you wish to analyze The LIBS Imaging Module also comes with special software for the camera to capture high quality images on your PC How the LIBS2500plus Works A high intensity 10 nanosecond wide laser pulse beam is focused on the sample area When the laser is fired the high temperature of the laser ablates the surface of the sample and creates a plasma As the plasma decays or cools excited atoms in the plasma emit light of characteristic wavelengths distinct to the elements present All elements have emission spectra in the 200 980 nm region The detection system uses up to seven of ou
43. ntroller assembly for HR2000 P600 2 UV VIS CNTRL Spectrometer LIBS System Software OOILIBSplus T N A includes elemental emission lines library 4 166 00000 000 02 0108 ptics mc it in Photonics First 1 Introduction LIBS Spectrometer Channels A G Channel Description LIBS CH A Spectrometer channel with 200 305 nm wavelength range LIBS CH B Spectrometer channel with 295 400 nm wavelength range LIBS CH C Spectrometer channel with 390 525 nm wavelength range LIBS CH D Spectrometer channel with 520 635 nm wavelength range LIBS CH E Spectrometer channel with 625 735 nm wavelength range LIBS CH F Spectrometer channel with 725 820 nm wavelength range LIBS CH G Spectrometer channel with 800 980 nm wavelength range Note Channels do NOT have to be consecutive Laser Requirements for LIBS2500plus You can supply your own Q switched laser from our certified list or you can purchase one through Ocean Optics Laser requirements include a low divergence laser beam a tight focus is required to achieve a spark an active electro optic Q switch and external triggering and synchronization capability for the laser flashlamp and Q switch We recommend the ULTRA CFR Nd YAG laser from Big Sky Laser Technologies www bigskylaser com compactseries html The ULTRA CFR was used when testing prototypes of the LIBS2500plus The rugged and field portable ULTRA CFR delive
44. oad Graph Tags Save Grams Print Spectrum Exit Menu Option Description Save Grams 2 View Menu ScanType Mode Spectrum Int Y Background c A Overlays Menu Option Description Cursor Info Displays the Cursor info dialog box This dialog box lets you customize and record information about the cursor Spectrum Display the Spectrum in the graph window Background Display the background data in the graph window Overlays Brings up the Overlay sub menu which displays and loads an overlay 166 00000 000 02 0108 43 ptics mc B User Interface ye First in Photonics Overlay Sub Menu ScanType Mode Background Libr amp wv Spectrum Int Background a a Overlay 2 Select Overlay 1 Select Overlay2 Menu Option Description Overlay 1 Display overlay 1 Overlay 2 Display overlay 2 Select Overlay 1 Load an ols file into Overlay 1 Select Overlay 2 Load an ols file into Overlay 2 ScanType Menu 001 LIBS LIBS 2000 V4 5 File View Mode Back E Spectrometer Single Shot Continuous Shot Int Time E Menu Option Description Spectrometer Selects Spectrometer mode You can set the integration time in this mode but laser control is not enabled Single Shot Selects Single Shot mode This mode controls the laser and allows you to manually fire it Continu
45. or the saved sample Enter a name for this Sample Libray Sample Creation 6 Click the Correlate button You should get a 1 7 Click the Scan button You should get a number very close to 1 8 Savethe new library using the Correlation menu 26 166 00000 000 02 0108 ptics mc First in Photonics 3 Operation Element ID Mode ___ Lines Detected Displays the number of Elemental Lines detected and lists them in a table below You can click on any column header to sort the data by that column Double click on any line to zoom in on that line Analyzes the current sample in memory and displays the results Save Results Writes an ASCII file containing a list of the lines and elements Element List Displays the number of elements detected and displays a table of them below The element name number of lines found and the element probability are listed Search Width Specifies the range of pixels surrounding the wavelength to examine when detecting a peak Peak Height Specifies the minimum height of a peak to qualify for inclusion on the list Range Sets the elemental analysis range You can click the cursor buttons to use current cursor positions Elemental ID Procedure Procedure Follow the instruction below to use the Elemental ID Mode 1 Select Mode Element ID from the menu to open the Element Identification window Element Identification Lines Detected 0 Element List 0 fa
46. ould now have a correlation coefficient very close to 1 depending on the properties of the material 5 Repeat this process for as many samples as you would like to compare against 6 Click the Less button to minimize the extra information You only need to expand this option when you are adding new samples Saving the Correlation Library Procedure 1 Open the Library Options Menu 2 Select Correlation Linear Correlation Save Library 3 Enter the name of the library to save and click the Save button Upon startup the software automatically loads the last library in use If you now load the saved library then exit and restart the program your saved library will automatically load upon startup In Pixel Correlation mode each time you take a scan the system will automatically correlate it If you are in a different mode you must manually click the Correlate button The system then correlates the library against the current spectrum in memory Correlation Tips The following tips will help you perform a correlation with OOILIBSplus e On occasion you may only want to look at a specific range You can do this by manually defining a Correlation Range Place the cursor at the starting wavelength and click the Cursor button This populates the starting wavelength Then repeat for the ending wavelength After you enter the range click the Update button to save them To use the full range set both the starting and ending wav
47. ous Shot Selects Continuous mode This mode fires the laser on a interval set in the Setup Options and the software acquires and analyzes data 44 166 00000 000 02 0108 ptics mc First in Photonics Mode Menu B User Interface E 00I LIBS LIBS 2000 V4 5 0 0f Fie view ScanType BA Background L amp p v Normal Average Pix Correlation HESSE n _ Element ID Peak Analysis Menu Option Description Normal Data collection only No analysis is performed Pix Correlation Allows you to correlate against a library and determine the closest match based on pixel information Element ID Attempts to pick out the lines of elements contained in the spectrum Peak Analysis Allows you to get some statistical information on user definable peaks Background Menu Background Library Options Toc Mode b Load Sampled Background Add Sampled Background Mix Sample Background Menu Option Description Mode Allows you to select the type of background subtraction Load Sampled Loads a background file to be subtracted off in Sampled Background mode Background Add Sampled Adds together a sampled background doing a per point add on to the Background background files Mix Sample Mixes two background files retaining the higher counts per point Background 166 00000 000 02 0108 45 ptics mc
48. r HR2000 High resolution Miniature Fiber Optic Spectrometers each with a 2048 element linear CCD array All spectrometers are triggered to acquire and read out data simultaneously The detectors in the broadband 200 980 nm LIBS2500plus collect the signal software included with the system displays and identifies the emission spectrum Advantages of Broadband LIBS Techniques Many LIBS systems have a small spectral range The LIBS2500plus is the first to provide broadband spectral analysis Because the system is noninvasive you can perform real time measurements in situ in hostile industrial chemical and biochemical environments with little or no sample preparation 166 00000 000 02 0108 1 ptics mc 1 Introduction First in Photonics LIBS Emission ID The reason we at Ocean Optics have designed a broadband high resolution spectrometer is to be able to both see and resolve all the lines from all the elements The spectral resolution is 0 1 nm less than this in the UV blue and a bit higher in the red IR Because the LIBS generated lines are stark broadened to about 0 2 nm or so in the UV and about 0 3 nm in the IR the system can resolve everything that is possible to measure The laser induced plasma begins life as very hot 15 000 degree K plasma emitting a large bremsstrahlung continuum Depending on the sample matrix most emission analysis is performed for a few microseconds after the initial plasma generation so t
49. rein are the trademarks service marks registered trademarks or registered service marks of their respective owners Limit of Liability Every effort has been made to make this manual as complete and as accurate as possible but no warranty or fitness is implied The information provided is on an as is basis Ocean Optics Inc shall have neither liability nor responsibility to any person or entity with respect to any loss or damages arising from the information contained in this manual Important Safety Notices WARNING The Ocean Optics LIBS System uses a Class 4 laser When operated as designed and with the sample chamber closed this system meets Class 1 laser safety requirements and so requires no special precautions Exposure to a Class 4 laser can cause eye and skin damage Although the LIBS System incorporates numerous safety features due care is required when using a laser to prevent injury Never operate this system without all safety covers in place and sample interlock chamber functioning 1 Use laser safety glasses rated for Nd YAG laser applications OD6 1064 at all times when operating the laser 2 Only permit properly trained and certified personnel to operate the laser 3 Readall the instructions that accompanied your laser 166 00000 000 02 0108 q ptics mc Important Safety Notices First in Photonics ii 166 00000 000 02 0108 Table of Contents About This Manual coeds M
50. rrect your device driver problem you must obtain the Correcting Device Driver Issues document from the Ocean Optics website http www oceanoptics com technical engineering correctingdevicedriverissues pdf Remove the Unknown Device from Windows Device Manager Procedure 1 Open Windows Device Manager Consult the Windows operating instructions for your computer for directions if needed 2 Locate the Other Devices option and expand the Other Devices selection by clicking on the sign to the immediate left 166 00000 000 02 0108 34 ptics inc it Photonics First 4 Troubleshooting Note Improperly installed USB devices can also appear under the Universal Serial Bus Controller option Be sure to check this location if you cannot locate the unknown device Rem l 2 Locate the unknown device marked with a large question mark Right click on the Unknown Device listing and select the Uninstall or Remove option Click the OK button to continue A warning box appears confirming the removal of the Unknown Device Click the OK button to confirm the device removal Disconnect the HR2000 Spectrometer s from your computer Perform the steps in the following Remove Improperly Installed Files section ove Improperly Installed Files Procedure Open Windows Explorer Navigate to the Windows INF directory Note If the INF directory is not visible you must disable th
51. rs Q switched pulses at 1 06 with variable repetition rates from 1 to 20 Hz At 1 06 um the laser has a pulse stability of 3 We also offer the Crossfire double pulsed laser system in which two laser pulses are used with very short 0 1 5 us inter pulse spacing The Crossfire is the backbone of a flexible LIBS system that can be configured for single or dual pulse operation quickly and with high repeatability This enables users to apply and compare both analytical methods and to reproduce many set ups referenced in existing publications Timing between laser pulses is controlled via Crossfire software or through the spectrometer s Imaging and targeting of samples is supported by means of the on board video microscope and electronics controlled via the Crossfire software See http www photon machines com for more information 166 00000 000 02 0108 5 ptics mc 5 it in Photonics First in Photonics 1 Introduction LIBS Sample Chamber The LIBS SC Sample Chamber is a key component of the Ocean Optics LIBS system and is designed to perform various functions safely and in clear view The chamber houses a manually controlled x y stage The chamber is made of an eye protective polymer that provides a clear view of a sample The laser focus lens and spectrometer probe mounting hardware is easily adjustable to accommodate samples varying in height The sample chamber also includes an exhaust system to evacua
52. s e For the second analysis technique the emission lines have an appearance value based on experimental observation It could be that this single line is the brightest of those from this element and the others are weak So we rate the element using a formula based on these appearance levels If only the weakest line of the 7 appears it is ranked very low and indicates that this is from one of the unknowns If it is the strongest line it will be rated high allowing you to be certain that it was present If you have the highest 5 of the 7 in the table the rating will be extremely high OOILIBSplus software allows you to call any number of spectral libraries you wish to use The present library has greater than 2000 lines available There are no overlaps but as we advance to more sophisticated libraries there certainly will be The full NIST catalog has so many lines 7100 000 that everything would be identified many times over even though the probability of appearance may be small to zero That is why we have not included it Refer to http physics nist gov PhysRefData contents atomic html to print lists and observe the latest work For a list of the persistent lines of spark spectra consult one of the CRC manuals Handbook of Chemistry and Physics Even the old publications are quite accurate 2 166 00000 000 02 0108 ptics mc it in Photonics First 1 Introduction Counts 200 300 400 500 600 700 900 900
53. s equipment see Hardware Cabling Test that the LIBS2500plus System is operational see System Start up Note Consult the instructions provided with the LIBS Imaging Module and the laser being used for complete installation and operation instructions for those products General guidelines are provided in this manual but may not cover all the information that you need to install and operate these components of your LIBS System Hardware Set up Set up your LIBS2500plus System in the configuration shown in the following figure Do NOT connect any of the cables until you have installed the OOILIBSplus Software 166 00000 000 02 0108 IPtics inc S First in Photonics 2 Installing the LIBS System Laser Inert Gas Tank bete optional eM LIBS Imaging Module LIBS Sample Chamber Spectrometer Rack LIBS2500plus Hardware Set up Using Single Laser Spectrometer Rack Inert Gas Tank optional LIBS2500plus Hardware Set up Using Dual Laser Procedure 1 Remove the LIBS2500plus components and laser from their packaging 2 Place the sample chamber or Crossfire system and the rack of spectrometers on a clean flat surface 10 166 00000 000 02 0108 ptics mc First in Photonics 2 Installing the LIBS System 3 Ifyou have purchased the LIBS Imaging Module attach it to the sample chamber To do this you must take the cover off the imaging module and attach the base plate to th
54. s you to identify the elements present in a sample by comparing the emission lines detected in the sample to elements in a standard catalog Procedure To load the Element ID Library 1 Select Library Options Element ID Load Library from the OOILIBSplus software menu 2 Browse to the element catalog that you want to load By default the OOILIBSplus installation places the catalog in Program Files Ocean Optics OOILIBSplus unless you changed its location 3 Select the file spe and click Open to load the file It is recommended that you select the OOlISpeciesB spe file since it contains more element lines than the OOISpecies spe file You can check that the library has loaded successfully on the Peak Analysis screen Procedure To check that the Element ID Library has loaded successfully 1 Select Mode Peak Analysis from the menu The Peak Analysis screen appears Element Lines Wil OO LIBS LIBS 2000 V4 5 0 0f File View ScanType Mode Background Library Options Tools Help 40 0 0 Int Time Averages Shot Count Scans for Selected Line Counts Intg Counts a 388 556 Add Clear Calculations 417 998 Add Custom Save Calculations 418 312 419 44 Delete 438 453 Analyze 439 571 Load List 446 273 Save List 461 393 471 658 Lines To Analyze Element Wave LWave RWave Mean StdDev RSD IntgMean Intg Std Dev Intg RSD Count Line Information Wavelength 0 Cursor
55. ses and that this laser also requires time to build power 3 Click the Set button Note Since these values are initialized to the last saved settings you will only need to perform the following steps if the requirements of the experiment require a change of these settings 4 Move the slider bar to desired Integration Start Delay value Refer to the displayed spectrum to determine if any further modification is needed 5 Click OK to accept these settings or Cancel to return to the main screen Setup Options Use this screen to configure the setup options for your LIBS system Setup Options Laser Intervals Time Between Samples Continuous Mode 500 ms Delay Between Scans Averaging Shot Count 10 Use pp ms Use Extemal Triggering DLL Saturation Detect Continuous Laser Mode Radiometric Calibration 166 00000 000 02 0108 21 ptics mc 3 Operation First in Photonics Option Description Percent Adjust Multiplier for the Real Time Background options OOILIBSplus calculates the background and multiplies it by this variable before subtracting Clean Shots e Number of clean shots to take when you click the Clean button or e Number of clean shots to take before each scan if you enable the Use button Use External Triggering DLL Uses the External Triggering DLL OOILIBSplus makes calls before and after scans to this DLL file You
56. te any particulates created by the ablation process and an inert gas induction port for ablation area purge The chamber door is magnetically latched and interacts with the safety interlock that prevents the laser from firing when the door is open A 12 Volt DC power supply is included for chamber lighting and exhaust fan power LIBS Imaging Module The LIBS IM USB Imaging Module directly attaches to the LIBS SC Sample Chamber which enables users to magnify a sample image and to establish a laser ablation target on the sample The camera 15 also useful for adjusting the laser focus above or below the sample surface The LIBS IM USB is in the same focal plane as the sample surface when the image is in focus the laser is focused to the surface of the sample enabling precise rapid and convenient laser focus The USB enabled color camera captures pre and post ablation images of the sample and provides up to 1280 x 1024 pixel resolution OOILIBSplus Software The Windows based OOILIBSplus Analysis Software operates the LIBS2500plus spectrometer system fires the laser and identifies the element being analyzed There are five main features in the software e Element Identification The Element Identification feature compares the sample spectrum against a spectral library to find possible matches The software will provide a rating of any matches found based on the number of identical lines Currently OOILIBSplus comes with a library of persistent l
57. ur website at http www oceanoptics com Select Technical Operating Instructions then choose the appropriate document from the available drop down lists Or use the Search by Model Number field at the bottom of the web page You can also access operating instructions for Ocean Optics products from the Software and Technical Resources CD that ships with the product Engineering level documentation is located on our website at Technical Engineering Docs Other Ocean Optics documentation related to your LIBS system includes the following e LIBS Imaging Module Installation and Operation Instructions located at http www oceanoptics com technical LIBS Install pdf e Correcting Device Driver Issues located at http www oceanoptics com technical engineering correctingdevicedriverissues pdf 166 00000 000 02 0108 vii ptics mc About This Manual First in Photonics Upgrades Occasionally you may find that you need Ocean Optics to make a change or an upgrade to your system To facilitate these changes you must first contact Customer Support and obtain a Return Merchandise Authorization RMA number Please contact Ocean Optics for specific instructions when returning a product viii 166 00000 000 02 0108 Chapter 1 Introduction Product Overview The Ocean Optics LIBS2500plus Laser induced Breakdown Spectrometer is a detection system that permits real time qualitative measurements of trace elements Th
Download Pdf Manuals
Related Search