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30 . Raman IdentiCheck Getting Started Guide

The change between the incident radiation and the Stokes/Anti-Stokes radiation represents a

change in the vibrational and/or rotational energy of the molecule. The frequency shifts from

the frequency of the incident beam are displayed on the x-axis of a Raman spectrum,

generally in relative wavenumbers (otherwise known as Raman Shift) and the intensity of the

bands are displayed in arbitrary units on the y-axis.

Figure 5 Raman spectrum of cyclohexane, showing Stokes, anti-Stokes and

Rayleigh scattering

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Summary of Contents for Raman IdentiCheck

Page 1: ...Raman IdentiCheck Getting Started Guide MOLECULAR SPECTROSCOPY ...

Page 2: ...bility and fitness for a particular purpose PerkinElmer shall not be liable for errors contained herein for incidental consequential damages in connection with furnishing performance or use of this material Copyright Information This document contains proprietary information that is protected by copyright All rights are reserved No part of this publication may be reproduced in any form whatsoever ...

Page 3: ...n IdentiCheck Specifications 37 Unpacking the Instrument 38 Spectrometer Parts 38 Optional Tablet PC 39 Triggered Fiber Optic Probe Parts 39 Spectrometer Module 40 Right hand Panel 40 Left hand Panel 41 Triggered Fiber Optic Probe TFOP 43 Analyzing Samples with the Probe 44 Power Supply Unit 46 Raman IdentiCheck PC 47 Commissioning your Instrument 48 Using the Raman IdentiCheck 51 Introduction 52 ...

Page 4: ...the Spectrometer 67 Cleaning the Air Filters 67 Maintaining the Triggered Fiber Optic Probe 67 Cleaning the Triggered Fiber Optic Probe 67 Replacing the Triggered Fiber Optic Probe 68 Troubleshooting 70 Hardware 70 Software 70 Decontamination 71 WEEE Instructions for PerkinElmer Products 72 Appendix A Using your own PC 73 Introduction 74 Configuring the PC 75 Installing Spectrum Software 76 Config...

Page 5: ...Introduction ...

Page 6: ...er Raman History Theory and Instrumentation This chapter contains a brief overview of the history and theory of Raman spectroscopy Introduction to the Raman IdentiCheck This chapter gives an overview of the instrument and contains an introduction to the spectrometer and the triggered fiber optic probe Using the Raman IdentiCheck This chapter contains a number of Standard Operating Procedures SOPs ...

Page 7: ... keys on the PC keyboard is used to show that you have to press two keys at the same time for example ALT F All eight digit numbers are PerkinElmer part numbers unless stated otherwise Notes Cautions and Warnings Three terms in the following standard formats are also used to highlight special circumstances and warnings NOTE A note indicates additional significant information that is provided with ...

Page 8: ...ros En los recuadros como éste se proporciona información sobre este tipo de circunstancias Caution Attention Nous utilisons le terme CAUTION ATTENTION pour signaler les situations susceptibles de provoquer de graves détériorations de l instrument ou d autre matériel Les détails sur ces circonstances figurent dans un encadré semblable à celui ci Caution Attenzione Con il termine CAUTION ATTENZIONE...

Page 9: ...recuadros como éste se proporciona información sobre este tipo de circunstancias Warning Danger Nous utilisons la formule WARNING DANGER pour avertir des situations pouvant occasionner des dommages corporels à l utilisateur ou à d autres personnes Les détails sur ces circonstances sont données dans un encadré semblable à celui ci Warning Pericolo Con il termine WARNING PERICOLO vengono segnalate s...

Page 10: ...10 Raman IdentiCheck Getting Started Guide ...

Page 11: ...Safety Practices ...

Page 12: ...ved to be correct and complete PerkinElmer shall not be liable for errors contained herein nor damages concerned with the use of this document PerkinElmer does not accept liability for the interpretation of information resulting either directly or indirectly from our spectrometers or associated software interfaces All results supplied by PerkinElmer s spectrometers or software are intended to prov...

Page 13: ...ent temperatures of 5 C to 35 C The temperature range for optimal performance is 15 C to 30 C this range being defined by the requirements of NIST calibration A maximum ambient relative humidity of 80 non condensing for temperatures up to 35 C NOTE The performance of the instrument will be affected by the ambient temperature and humidity At elevated temperatures the internal camera may shut down i...

Page 14: ... to prolonged storage in unfavorable conditions Has been subjected to severe transport stresses Storage When not in use the IdentiCheck should be stored packed in its case indoors at a temperature between 20 C to 60 C CAUTION Do NOT store your IdentiCheck in a location that receives direct sunlight as elevated temperatures generated inside the case may damage the electronics CAUTION Do NOT store o...

Page 15: ...equipment that meets the requirements of IEC 61010 1 IEC 60950 or equivalent standards Power Supplies The Raman IdentiCheck is powered by one external power supply unit The power supply unit can adjust automatically to a variety of AC power sources as outlined in Table 1 Table 1 Power supply unit input voltages and mains fluctuations information Input Voltage Mains Fluctuations 100 230 V AC 10 of ...

Page 16: ...nation WARNING If the power cord is not appropriate for your country it must be removed from use immediately and replaced If the power cord has any physical damage it must be removed from use immediately and replaced To avoid electrical hazards the ground pin on the power cord should not be interfered with in any way Fuses The only fuses that you may have to replace are those in the mains power co...

Page 17: ...C standard EN61326 EMC standard for electrical equipment for measurement control and laboratory use and EN55011 ISM class A RF emissions FCC rules and regulations This product is classified as a digital device used exclusively as industrial commercial or medical test equipment It is exempt from the technical standards specified in Part 15 of the FCC Rules and Regulations based on Section 15 103 c ...

Page 18: ... protective covers or service panels on the instrument appear to be damaged turn the instrument off secure it against any unauthorized operation and contact PerkinElmer for advice before using the instrument again The triggered fiber optic probe TFOP provides a focused beam of laser radiation 100 mW at 785 nm During normal operation laser radiation is accessible from the end of the probe The outpu...

Page 19: ...sible radiation up to a maximum of 0 5 W continuous wave CW is longer than 0 25 s They present a hazard to the eye if the direct beam or specular reflections are viewed without appropriate protection You must only operate Class 3B lasers in a designated area 2 You must fit each Class 3B device with a captive key control switch such that the key cannot be removed from the lock except in the OFF pos...

Page 20: ...TFOP with a plastic spacer always rotate the spacer so that the screw is beneath the probe barrel when not in use when in this position the spacer acts as a lens cap Never look directly into the laser beam or at the laser light scattered from a reflective surface or sample Permanent eye injury may result Do NOT attempt to examine the probe tip when the Path Active light on the probe is lit Post wa...

Page 21: ...xposure J cm 2 For the TFOP bo is 0 254 cm therefore the above equation can be simplified to give 2 1 Φ 442 4 MPE f NOHD o For the wavelength range 700 1050 nm the MPE for a 10 second exposure can be calculated from 4 7 0 2 10 10 1 10 λ MPE J cm 2 Where λ is the laser wavelength in micrometers µm For example a laser wavelength of 785 nm 0 785 µm will have an MPE value of 1 49 x 10 2 J cm 2 or 1 49...

Page 22: ...aser systems have the potential to cause harm or injury to those using them or others in the vicinity of the instrument For more information refer to Attaching the External Interlock Override on page 41 The Raman IdentiCheck has been designed for use outside of a laboratory with the external interlock overridden WARNING The Raman IdentiCheck should not be left unattended when the laser safety key ...

Page 23: ... MAXIMUM OUTPUT 250mW PULSE DURATION CONTINUOUS WAVE EMITTED WAVELENGHS 785nm THIS LASER PRODUCT CONFORMS TO IEC 60825 1 1993 21 CFR 1040 10 1040 11 LASER RADIATION AVOID EXPOSURE TO BEAM CLASS 3B LASER PRODUCT MAXIMUM OUTPUT 250mW PULSE DURATION CONTINUOUS WAVE EMITTED WAVELENGHS 785nm THIS LASER PRODUCT CONFORMS TO IEC 60825 1 1993 21 CFR 1040 10 1040 11 LASER RADIATION AVOID EXPOSURE TO BEAM CL...

Page 24: ... clipped shut Transporting the instrument without the use of the shipping carton may affect the performance of the instrument We recommend using the shipping carton when moving the instrument over long distances The Raman IdentiCheck weighs approximately 30 kg including the optional tablet PC and the power supply unit To avoid injury or damage to the instrument please use proper lifting techniques...

Page 25: ...ight of the instrument and any ancillary equipment without warping or wobbling There must be two power points available one for the instrument power supply unit and one for the PC Floor vibrations or noise from heavy manufacturing equipment can affect the performance of the instrument Avoid proximity to intense magnetic fields Never place the instrument near a window that receives direct sunlight ...

Page 26: ...26 Raman IdentiCheck Getting Started Guide ...

Page 27: ...Raman History Theory and Instrumentation ...

Page 28: ...observed the scattering from water and alcohol visually In addition to the blue incident light a faint green light also scattered later named Stokes scattering By the 1930s much of the theory underlying Raman scattering was understood but due to the complexity of the instrumentation the initial interest in Raman spectroscopy was not maintained Improvements in charge coupled device CCD detectors fi...

Page 29: ...okes scattering or shorter wavelengths higher frequencies ν Anti Stokes scattering With Stokes scattering some of the incident photons give up a portion of energy to the molecules and are detected at a lower frequency longer wavelength than the Rayleigh radiation Figure 4 Figure 4 Rayleigh Stokes and Anti Stokes Scattering Virtual Energy State Rayleigh Anti Stokes Stokes Excited Energy ν 0 ν 0 ν 0...

Page 30: ...ational energy of the molecule The frequency shifts from the frequency of the incident beam are displayed on the x axis of a Raman spectrum generally in relative wavenumbers otherwise known as Raman Shift and the intensity of the bands are displayed in arbitrary units on the y axis Figure 5 Raman spectrum of cyclohexane showing Stokes anti Stokes and Rayleigh scattering ...

Page 31: ...a laser mirrors fiber optics filters lenses spectrograph and a CCD detector The laser supplies light through an optical pathway onto the sample through the fiber optic probe The scattered light from the sample is collected and transmitted back to the spectrometer Figure 6 Schematic of the Raman IdentiCheck Laser Spectrograph Optical Head Objective Lens High Performance TE cooled CCD ...

Page 32: ... two dimensions by using two gratings Figure 7 The first grating disperses the light horizontally onto the second grating where the light is further dispersed vertically onto the CCD detector The light is spread over a number of strips on the CCD that are read simultaneously therefore a full spectral range at high resolution can be achieved with one acquisition Figure 8 Strips of light on the CCD ...

Page 33: ...ing parts in the spectrograph which improves instrument reliability ruggedness and the quality of calibration The absence of moving parts also means that as you acquire the spectrum there is no change in the spectrograph s stray light performance meaning that there are no stitch marks in the final spectrum No light is lost all the light goes onto the detector and all the strips are read out simult...

Page 34: ...34 Raman IdentiCheck Getting Started Guide ...

Page 35: ...Introduction to the Raman IdentiCheck ...

Page 36: ...transport case with wheels and a carrying handle A power supply unit A 5 meter triggered fiber optic probe a 20 meter option is available as are other types of probe A tablet or laptop PC This chapter provides an introduction to these components and also describes how to unpack and prepare your IdentiCheck for use Figure 9 Raman IdentiCheck ...

Page 37: ... 5 C 41 F 35 C 95 F Optimal Temperature 15 C 59 F 30 C 86 F Humidity Max 80 non condensing Power Supply 100 230 V 10 50 60 Hz Power Consumption 50 W max If the electricity supply does not conform to these specifications please consult PerkinElmer prior to installation If the supply of power is erratic please use an uninterruptible power supply UPS Power fluctuations or brown outs may damage the sp...

Page 38: ...nue with the installation Contact your PerkinElmer Customer Care Representative immediately Spectrometer Parts Part Number Description L1320090 Raman IdentiCheck Spectrometer Module LX108870 Spectrum Std for Raman Software Kit Contains the Spectrum Std Software CD LX100877 the Raman Instrument Configuration Disk LX108869 the Raman Spectral Libraries CD L1321877 and the Spectrum Insight Software CD...

Page 39: ...Italy OR L9003646 US OR L9003695 UK Dell XT 2 Tablet PC Various Country specific power cable L9003770 External Media Bay DVD RW Drive Triggered Fiber Optic Probe Parts Part Number Description L1320030 OR L1320031 OR L1320058 Triggered Fiber Optic Probe 5 m cable Triggered Fiber Optic Probe 20 m cable Triggered Fiber Optic Probe 5 m cable 120 cm 1 cut off L1320324 Raman probe fixed spacer kit 7 5 m...

Page 40: ...ht hand panel of the Raman IdentiCheck Figure 10 contains 3 LED indicators see table below for details Laser key switch Air filters for the cooling fans External interlock override Figure 10 Spectrometer module right hand panel Laser key switch External interlock override Air filters LEDs ...

Page 41: ...safety interlock when the Active LED is illuminated the shutters will close Attaching the External Interlock Override The Raman IdentiCheck has an external interlock connection located on the right hand side of the top panel Figure 10 To operate the instrument the external interlock must be satisfied This can be achieved in one of two ways Either by attaching the External Interlock Override part n...

Page 42: ...aman IdentiCheck Getting Started Guide Figure 11 Spectrometer module left hand panel WARNING The Aux power connector is covered and should not be used USB port Probe connectors Main power Aux power covered ...

Page 43: ... remote measurement of samples Figure 12 Side view of probe with plastic spacer fitted ready for use The probe body contains the filtering optics and electronics and is interfaced with two fiber optic cables an excitation fiber and collection fiber Care should be taken when handling the probe body so that the optical window is not soiled or damaged Trigger Plastic spacer ...

Page 44: ...Samples with the Probe NOTE A set of sampling accessories is available for use with a TFOP See Additional Parts and Upgrades on page 64 for details Analyzing free solids The standard TFOP has a tight focus spot that is approximately 7 5 mm away from the lens other customized distances are available The focused spot enables you to pinpoint the measurement area on the sample A plastic spacer 7 5 mm ...

Page 45: ...ry different probe positions If the liquid of interest is not absorbing it may be best to focus through the container by placing the TFOP in direct contact with the container When using 785 nm lasers many types of glass exhibit bands between 1400 1600 cm 1 Spectra of the container should be obtained before analyzing the sample to ensure that glass derived bands do not pose a problem With 785 nm ex...

Page 46: ...is designed to operate in situ strapped within the lid of the IdentiCheck transport case although it can be removed if required NOTE For information on running the Raman IdentiCheck from a battery supplied powerpack contact your PerkinElmer Business Unit CAUTION You must ensure that the power supply unit is secured within the lid of the case using the straps provided during transport ...

Page 47: ... be used in situ within the lid of the IdentiCheck transport case although it can be removed if required Figure 15 Tablet PC NOTE If you choose to provide your own laptop or tablet PC for use with your Raman IdentiCheck you must ensure that it meets the appropriate hardware and software specifications that it is configured correctly and that the appropriate software is installed See Appendix A Usi...

Page 48: ... of the instrument to the PC Connect the USB extender cable from the triggered fiber optic probe to the PC OR If you are using your own laptop you should follow the procedures described in Appendix A Using your own PC starting on page 73 before continuing at step 8 of this procedure 5 Switch on the laptop or tablet PC and start up the Windows operating system 6 Connect the instrument power supply ...

Page 49: ... Instrument Basic tab 11 Ensure that the Triggered Fiber Optic Probe you wish to use is selected as the Accessory When you make the selection the Probe Path LED on the probe will light up blue This indicates that the probe is ready for use NOTE For safety reasons when the TFOP is selected as the Accessory all Scan buttons in the software are disabled Scanning using a TFOP can only be started using...

Page 50: ...50 Raman IdentiCheck Getting Started Guide ...

Page 51: ...Using the Raman IdentiCheck ...

Page 52: ...orward or simple for the task you wish to perform so treat these Standard Operating Procedures SOPs as a starting point and with time you may wish to develop your own SOPs which better suit your specific mode of use This chapter also acts as a learn by doing section allowing you to explore the functionality of the software and spectrometer NOTE If you are in any doubt about any aspect of using you...

Page 53: ...emains to carry out the experiments you want to perform 5 Connect the USB extender cable from the probe to your PC 6 Connect the USB cable from the spectrometer to your PC 7 Ensure that the interlock is satisfied or the interlock override is fitted 8 Insert the laser power key into the instrument and turn it to the ARM position 9 From the Windows Start menu select All Programs the PerkinElmer Appl...

Page 54: ...e by selecting Exit from the File menu to return to the Windows operating environment 2 Remove the laser power key and if appropriate the interlock override 3 Switch off the power supply and then unplug the power supply unit 4 Shut down your PC and then disconnect the triggered fiber optic probe USB extender cable 5 Disconnect the USB cable that connects the PC to your IdentiCheck 6 If appropriate...

Page 55: ... Using the Instrument Settings toolbar check and set the instrument parameters such as the Start and End points of the scan range in Raman Shift for example 3200 cm 1 to 100 cm 1 and enter a unique Sample ID and Description 3 Set the Exposure Time and number of Accumulations You can define the Accumulations as a number of Exposures or as a number of minutes or seconds Typical values for Exposure T...

Page 56: ... of the trigger may result in a failure to start data collection Once the Path Active LED is illuminated you can release the trigger The indicator will remain lit during data collection indicating that laser light is being emitted from the TFOP When the acquisition is complete the Path Active LED will extinguish or will start to blink if you are still depressing the trigger The blue Probe Path LED...

Page 57: ...mmend that you calibrate the instrument in accordance with the following SOP SOP 5 Calibration Performance Verification We recommend that wavelength calibration verification is performed on a regular basis to ensure that the instrument is performing within specification This can be once a day or once a week depending on your requirements and the environment in which the instrument is used IMPORTAN...

Page 58: ...ecause the spectral intensity is low then this may also be due to the calibration sample not being correctly positioned optimally focused or because the laser key is not switched on or the laser power is too low Then repeat the wavelength calibration verification to ensure that the instrument has been brought back within specification If the instrument fails the wavelength calibration verification...

Page 59: ...isable to collect some spectra from the polystyrene sample to ensure that the Raman signal is optimized and that there is no contribution to the spectra from the sample holder Refer to SOP 4 Collecting a Spectrum with a Triggered Fiber Optic Probe on page 56 5 Cover the probe and sample with a thick black cloth to avoid any stray light reaching the detector 6 Select Toolbox on the Setup Instrument...

Page 60: ... the probe 2 Ensure the IdentiCheck is switched on and is stable by following SOP 1 3 Ensure that the Triggered Fiber Optic Probe is selected as the Accessory see Commissioning your Instrument on page 48 The Probe Path LED on the probe will be illuminated 4 Select the Setup Instrument Advanced tab and click Toolbox The Adjustments Toolbox dialog is displayed 5 Select The Wavelength Calibration dia...

Page 61: ...isable to collect some spectra from the polystyrene sample to ensure that the Raman signal is optimized and that there is no contribution to the spectra from the sample holder Refer to SOP 4 Collecting a Spectrum with a Triggered Fiber Optic Probe on page 56 5 Cover the probe and sample with a thick black cloth to avoid any stray light reaching the detector 6 Select Toolbox on the Setup Instrument...

Page 62: ...ioning your Instrument on page 48 The Probe Path LED on the probe will be illuminated 3 On the Setup Instrument Advanced tab ensure that the laser power is set to 100 4 Optimize the Raman signal from the NIST standard part number L1321831 with the dull surface pointing upwards and then clamp the probe in place using a clamp stand It is advisable to collect some spectra from the sample to ensure th...

Page 63: ... the intensity calibration routine should fail please ensure that the laser key switch is set to ARM the laser power is set to 100 the NIST sample is correctly positioned dull side facing up and sample is optimally focused confirmed by collecting a few scans ...

Page 64: ...ive Intensity Correction Triggered Fiber Optic Probe Part Number Description L1320031 Triggered Fiber Optic Probe 20 m cable NOTE A 20 m triggered fiber optic probe cannot be transported within the Raman IdentiCheck case L1320070 Short immersion sleeve for TFOP L1320071 Ultra long working distance lens adaptor for Raman fiber optic probes L1320095 Raman probe sampling accessory kit Other Probes an...

Page 65: ...Maintenance and Troubleshooting ...

Page 66: ...use abrasive or solvent based cleaning materials Always perform a patch test on a small area before you clean the entire instrument Avoid spilling liquid into the instrument Clean all external spills immediately If anything that is spilled enters the main body of the spectrometer make the instrument inoperative and then contact a PerkinElmer Service Engineer WARNING Do not directly clean electrica...

Page 67: ...ck into the spectrometer module Maintaining the Triggered Fiber Optic Probe The TFOP is designed to be maintenance free under normal operating conditions and should not be opened or adjusted by anyone other than a PerkinElmer Service Engineer Contact PerkinElmer if you have any questions regarding maintenance or servicing of the TFOP Damage to the TFOP as a result of accident neglect misuse or as ...

Page 68: ...d a collection cable The excitation fiber transmits the laser energy whereas the collection cable is a conduit for the Raman energy Both fibers terminate in FC style connectors Removing a probe 1 Ensure the attenuator cap is attached to the probe 2 Disconnect the instrument from the power supply 3 Unscrew and remove the probe cable retaining bar Figure 17 Figure 17 Probe connectors CAUTION Do not ...

Page 69: ...the USB cable from the probe to the PC 4 Remove the retained screw in caps from the two couplers on the left hand panel 5 Remove the protective caps from the ends of the probe fibers and keep them for future use 6 Connect the excitation and collection cables of the probe to the appropriately labeled couplers Make sure that the polarizing ridge on the probe cables are aligned with the slot in the c...

Page 70: ...IdentiCheck Solution 2 Ensure your external interlock is wired up correctly and that any interlocked room entrances or sampling enclosures are closed Software Problem Spectrum software stops responding Description When you are using the Software for some reason it stops working that is mouse clicks have no effect Solution Hold down the CTRL ALT DELETE keyboard buttons to display the Windows Securi...

Page 71: ...ntamination The customer s responsible body is required to follow the Equipment Decontamination Procedure and complete the Certificate of Decontamination These documents are available on the PerkinElmer public website http las perkinelmer com OneSource decontamination htm Alternatively if you do not have access to the internet contact Customer Care Customer Care USA 1 800 762 4000 inside the USA 8...

Page 72: ...s the most effective means of protecting the customer s environment The requirements for waste collection reuse recycling and recovery programs are set by the regulatory authority in your location Contact your local responsible person such as your laboratory manager or authorized representative for information regarding applicable disposal regulations See the PerkinElmer web address below for info...

Page 73: ...Appendix A Using your own PC ...

Page 74: ...t number L1050095 Switch on the IdentiCheck refer to SOP 1 Switching the IdentiCheck on page 53 Add a Raman Instrument to the Spectrum software refer to the Spectrum Administrator s Guide L1050095 Configure the Spectrum software to use a triggered fiber optic probe as described on page 77 NOTE If you choose to provide your own laptop or tablet PC these steps will be carried out by a PerkinElmer Se...

Page 75: ...You can now start using the PC 5 It is important that the PC used with Raman IdentiCheck does not switch into Standby mode Select the Display option on the Control Panel On the Screen Saver page of the Display Properties dialog click Power and then set the System standby and Turn off hard disks values to Never for both Plugged in and Running on batteries NOTE To help ensure PC security we recommen...

Page 76: ...ment See SOP 1 Switching the IdentiCheck on on page 53 Wait a few moments for your instrument to initialize and then connect the instrument USB cable and the triggered fiber optic probe USB cable to the PC The instrument then needs to be added to the software See Installing a Raman Instrument in the Spectrum Administrator s Guide part number L1050095 You can add multiple FT IR spectrometers to Spe...

Page 77: ...ue If you have any doubts about the required safety precautions click Cancel When you make the selection the Probe Path LED on the probe will light up blue This indicates that the probe is ready for use When the laser is on and the shutter is open the Laser Status icon on the Measurement bar will be updated to Class 3B Laser Status Laser light will be emitted from the probe during data collection ...

Page 78: ...78 Raman IdentiCheck Getting Started Guide ...

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