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Using the RamanFlex 400 Series . 57

Calibration and Performance Verification SOPs

Several different automated calibration tests are included in the software:

•

Wavelength (x-axis) calibration uses the position of precisely known lines in a neon

emission spectrum to calibrate the detector.

•

Intensity (y-axis) calibration is performed using coated glass with a well characterized

emission spectrum. This is used to correct for non-linearity in detector response.

•

Laser frequency calibration determines the exact laser wavelength.

An additional wavelength calibration verification routine has been included in the software,

which compares a series of peaks for polystyrene (ASTM E 1840) with values collected using

a polystyrene sample. These calibration/verification tests allow for in-house instrument

performance verification.

Intensity calibration is only performed if the instrument has been moved, or as part of an

annual service, or if there have been appreciable temperature variations in the local

environment.

Backgrounds are always collected during a calibration procedure. The background measures

the bias and dark signal over the selected area of the CCD. This is a necessary part of the

calibration routines, so it is always performed.

The spectrometer has no moving parts in its detection system; therefore frequent calibration

is not necessary.

We recommend that you calibrate the instrument in accordance with the following SOP.

SOP-6: 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 laboratory environment.

When carrying out the calibration/verification procedures, the instrument laser power should

be set to 100% and the Data Interval to 2 cm

−1

or smaller.

On completion of the wavelength calibration verification, the result of the verification

procedure is displayed. A spectrum detailing the outcome of the verification (or calibration)

procedure is saved to the folder …\pel_data\config\Raman\Calibration Files\Logs with the

filename Calibration Report [Name of calibration][Date].sp

IMPORTANT: If the instrument passes the wavelength calibration verification procedure,

the instrument is optimized for performance and does not require wavelength calibration.

Содержание Raman Flex 400 Series

Страница 1: ...RamanFlex 400 Series Getting Started Guide MOLECULAR SPECTROSCOPY ...

Страница 2: ...antability 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 whatsoe...

Страница 3: ...ies 29 Spectrograph Detector Systems 30 Preparing your Facility 33 Specifications 34 Finding a Suitable Location for the Instrument 35 Instrument Dimensions 36 Installing your RamanFlex 400 Series 37 Unpacking the Instrument 38 Lifting the Instrument 39 Attaching the External Interlock Override 40 Installing the Instrument in Spectrum Software 41 Switching on the Instrument 42 Moving the Instrumen...

Страница 4: ...alibration 61 Summary 63 Additional Parts and Upgrades 64 Safety and Calibration 64 Fiber Optic Probes 64 SERS Consumables 65 Maintenance and Troubleshooting 67 Maintenance 68 Cleaning the Spectrometer and Power Supply Units 68 Cleaning the Air Filters 69 Servicing the Spectrometer 70 Service of the Fiber Optic Probe 70 Troubleshooting 71 Hardware 71 Software 71 Decontamination 72 WEEE Instruction...

Страница 5: ...Introduction ...

Страница 6: ...paring your Facility This chapter shows you how to position your RamanFlex 400 Series instrument and what utilities are required for example electricity and temperature control Installing your RamanFlex 400 Series This chapter contains step by step instructions about how to unpack and assemble your RamanFlex 400 Series instrument and information on installing your instrument in the software Using ...

Страница 7: ... have to press two keys at the same time for example ALT F All eight digit numbers are PerkinElmer part numbers unless stated otherwise The term RamanFlex 400 Series means the RamanFlex 400 and the RamanFlex 400F Raman Spectrometers Notes Cautions and Warnings Three terms in the following standard formats are also used to highlight special circumstances and warnings NOTE A note indicates additiona...

Страница 8: ...tros 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 ATTENZION...

Страница 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...

Страница 10: ...10 RamanFlex 400 Series Getting Started Guide ...

Страница 11: ...Safety Practices ...

Страница 12: ...lieved 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 p...

Страница 13: ...rature 15 C to 30 C Relative Humidity 80 maximum non condensing Avoid any adjustment maintenance or repair of the opened operating instrument If any adjustment maintenance or repair of the opened instrument is necessary this must be done by a skilled person who is aware of the hazards involved The instrument has been designed to be safe under the following conditions Indoor use Altitude up to 2000...

Страница 14: ...00 Series Getting Started Guide Fire Safety Ensure that there is at least 15 cm 6 between any cooling vents and adjacent equipment or walls Ensure that the power supply unit PSU vents or fan do not become obstructed ...

Страница 15: ...ourself and damage to the instrument switch OFF all components in the system and disconnect them from the line power supply before you alter or make any new electrical connections Electrical Protection Insulation Class I rating for external circuits Only connect equipment that meets the requirements of IEC 61010 1 IEC 60950 or equivalent standards Power Supplies The RamanFlex 400 and RamanFlex 400...

Страница 16: ...llation of the instrument and at any time the instrument is plugged into a different power point socket Power Cords Between PSU and Power Outlet Socket The power cord supplied to connect the instrument PSU to the power point socket should be appropriate for the country listed as the shipping destination WARNING If the power cord is not appropriate for your country it must be removed from use immed...

Страница 17: ...ith the EMC 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...

Страница 18: ...moval of the protective housing or external panels is dangerous If the 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 RamanFlex 400 Series are classified as Class 3B The Fiber Optic Probe provides a focused beam of laser radiation...

Страница 19: ... hazard to the eye if the direct beam or spectral 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 position The key should be removed from the laser when it is not in use and kept in a safe place in...

Страница 20: ...ver possible using a beam attenuator or cover The laser should also be turned off and the probe covered when the system is not in use AVOID DIRECT EXPOSURE TO THE BEAM Figure 1 Schematic of the fiber optic probe not to scale When using the fiber optic probe the following precautions must always be observed Use an interlock switch on the door to the laboratory and or the reaction vessel being used ...

Страница 21: ...hen the probe is in use always ensure that no stray laser radiation is directed at people in the vicinity Use protective laser safety goggles with an optical density OD of at least 3 at 785 nm as a precaution against accidental exposure to the direct or reflected laser light Suitable goggles are available from PerkinElmer part number L1323518 Do not use the TFOP if it shows any sign of damage If r...

Страница 22: ...ard distance for 785 nm Raman systems Table 3 Nominal Ocular Hazard Distance NOHD for 785 nm Probe focal length mm NOHD for 100 mW exiting fiber optic probe cm 7 5 10 27 3 NOTE Other focal lengths are available contact PerkinElmer for details In particular the use of an ultra long working distance lens adaptor part number L1320071 provides a working distance of 25 mm Where different focal lengths ...

Страница 23: ... modified power voltage and current values 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...

Страница 24: ...24 RamanFlex 400 Series Getting Started Guide ...

Страница 25: ...Raman History Theory and Instrumentation ...

Страница 26: ... 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 f...

Страница 27: ...scattered and will be detected at either longer wavelengths lower frequencies ν Stokes 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 5 Figure 5 Rayleigh Stokes and Anti Stokes Scat...

Страница 28: ...olecule 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 6 Raman spectrum of cyclohexane showing Stokes anti Stokes and Rayleigh scattering Anti Stokes x12 Rayleigh Stokes Raman Shift cm 1 ...

Страница 29: ...irrors fiber optics filters lenses spectrograph and a CCD detector The laser supplies light through an objective lens onto the sample through the fiber optic probe The scattered light from the sample is collected with the same objective lens and transmitted back to the spectrometer A schematic of the system configuration is provided in Figure 8 Figure 8 Schematic of the RamanFlex 400 Series Optica...

Страница 30: ...dispersing the light in two dimensions by using two gratings Figure 9 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 10 Str...

Страница 31: ...on spectrum with a full spectral range There are no moving parts which improves instrument reliability ruggedness and the quality of calibration The lack 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 al...

Страница 32: ...32 RamanFlex 400 Series Getting Started Guide ...

Страница 33: ...Preparing your Facility ...

Страница 34: ...e 15 C 59 F 30 C 86 F Recommended Temperature 20 C 68 F 22 C 72 F Power Supply 100 230 V AC 10 50 60 Hz 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 Incorrect shutdown power fluctuations or brown outs may damage the spectrometer ...

Страница 35: ...e workbench where the spectrometer and PC are to be located should be at a suitable height to allow the user to work comfortably Use conducting floor coverings to minimize static discharge Floor vibrations or noise from heavy manufacturing equipment can affect the performance of the instrument Locate the spectrometer at least 5 5 meters 18 feet away from any intense magnetic fields Never place the...

Страница 36: ...meter weighs approximately 20 kg Laboratory benching must be strong enough to support the combined weight of the instrument and any ancillary equipment without warping or wobbling The bench must be at least 650 mm 26 in depth Figure 11 Dimensions of the RamanFlex 400 Series 530 mm 600 mm 161 mm ...

Страница 37: ...Installing your RamanFlex 400 Series ...

Страница 38: ... PerkinElmer Service Representative immediately Part Number Description RamanFlex 400 Series 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 LX108872 L1323503 Laser key x2 L1321802 Mains PSU L1320821 USB Cable...

Страница 39: ...ies 39 Lifting the Instrument The RamanFlex 400 Series spectrometer module weighs 20 kg To avoid injury or damage to the instrument please use proper lifting techniques WARNING Always hold the instrument under the base when you lift it ...

Страница 40: ...e satisfied You must connect an external door interlock to the 7 way DIN connector labeled INTERLOCK on the rear panel of the spectrometer or attach the External Interlock Override part number L1320264 supplied with the instrument If your Laser Safety Officer determines that an interlock is required on the door to the room you will need to purchase the Raman Laser Safety Kit part number L1320262 F...

Страница 41: ...Raman Manuals CD part number L1050002 After the software is installed you should switch on your instrument See Switching on the Instrument on page 42 Wait a few moments for your instrument to initialize and then connect the instrument USB cable and if applicable the triggered fiber optic probe USB cable to the PC The instrument then needs to be added to the software See Installing a Raman Instrume...

Страница 42: ...our instrument is fitted with a deep depletion CCD connect the 7 5 V PSU part number L1323525 from the DD POWER socket on the rear panel to a mains power socket 3 If your instrument is fitted with a deep depletion CCD connect the Tygon tubing between the water recirculator part number L1323010 and the WATER IN OUT sockets on the rear panel fill the storage tank of the cooler with water and then pl...

Страница 43: ... must use the original supplied packing materials to prevent damage to the system When the instrument has reached its destination and has been reassembled you should perform the appropriate calibration verification procedures as described in the Calibration and Performance Verification SOPs on page 57 ...

Страница 44: ...44 RamanFlex 400 Series Getting Started Guide ...

Страница 45: ...Using the RamanFlex 400 Series ...

Страница 46: ...s the power status of the laser If the LED is illuminated then the laser is receiving power This does not mean that laser radiation is present throughout the optical path of the instrument only that the laser power is on Active This LED indicates the status of the laser shutters If the LED is illuminated then the shutters are activated open and laser radiation present throughout the optical path o...

Страница 47: ...hat the optical window is not soiled or damaged NOTE If you use the probe body in any chemical or aggressive environment you must use an immersion sleeve to protect the probe body DO NOT ATTEMPT TO USE THE PROBE BODY IN SUCH AN ENVIRONMENT WITHOUT THE USE OF AN IMMERSION SLEEVE part number L1320003 If required contact PerkinElmer for further details Attaching Removing the Fiber Optic Probe The sta...

Страница 48: ...he polarizing ridge on the FOP cable is aligned with the slot in the coupler casing before carefully pushing the cable into the coupler 7 If you have a standard probe connect the DIN connector to the nearby socket marked LED FIBER 1 OR If you have a RamanFlex 400F and are connecting a second fiber optic probe connect the DIN connector to the socket marked LED FIBER 2 OR If you have a triggered pro...

Страница 49: ...in films of materials should be folded so that the sample covers the entire depth of field Solids can be analyzed in glass and plastic containers similar to liquid samples NOTE Raman spectra are measured in the visible and near infrared region Room lights and sunlight will contaminate your spectra Take care not to misinterpret room lights or sunlight as sample features Sampling Liquids Liquid samp...

Страница 50: ... is not possible to use quartz containers then it is possible to acquire a spectrum of the container and then spectrally subtract this from any spectra containing this fluorescent signature When working through containers it is best to try different probe positions If the liquid of interest is not absorbing it may be best to focus through the container by placing the FOP in contact with the contai...

Страница 51: ...For step by step instructions for calibrating the spectrometer see Calibration and Performance Verification SOPs starting on page 57 SOP 1 Turning the Instrument On 1 Switch on the PC and monitor 2 Login to Windows 3 Ensure the laser power key on the front panel of the instrument is in the ARM position 4 Ensure the power supply is connected to a mains outlet and that the outlet is switched on 5 To...

Страница 52: ...1 Shut down Spectrum software by selecting Exit from the File menu to return to the Windows operating environment 2 Switch off the spectrometer by pressing the power switch on the PSU to OFF ON Ο OFF After Spectrum closes if you do not switch off the instrument it will remain active for 5 minutes This is so that you do not have to wait for the CCD detector to cool and the laser to stabilize should...

Страница 53: ...End points of the scan range in Raman Shift for example 3600 cm 1 to 100 cm 1 and enter a unique Sample ID and Description 6 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 Time and Accumulations are 5 seconds and 5 exposures respectively Spectra may be optimized by increasi...

Страница 54: ...ory a background will be acquired at this point You will see a progress bar for the background collection on the Live tab When the collection of backgrounds is complete the software will automatically begin collecting spectra The upper progress bar shows the progress of the current scan while the lower progress bar shows the overall progress of the measurement for example 1 of 2 scans if for examp...

Страница 55: ...tarted Guide supplied with your accessory SOP 4 Selecting the Fiber Optic Probe 1 Ensure the RamanFlex 400 is switched on If not follow SOP 1 2 If you did not connect to your instrument on starting Spectrum software select Instruments from the Setup menu and then Select Instrument from the sub menu The Instrument Connection dialog is displayed 3 Select your Raman instrument and then click Connect ...

Страница 56: ...g cannot be saved NOTE To see the Live display the Show live display option must be selected on the Setup Instrument Data Collection tab 1 Ensure that the RamanFlex 400 is switched on If not follow SOP 1 2 Click The Live tab will be displayed and real time spectral acquisition will commence 3 Adjust the Laser power on the Live tab to an appropriate value for your sample 4 Adjust the Exposure time ...

Страница 57: ...measures the bias and dark signal over the selected area of the CCD This is a necessary part of the calibration routines so it is always performed The spectrometer has no moving parts in its detection system therefore frequent calibration is not necessary We recommend that you calibrate the instrument in accordance with the following SOP SOP 6 Calibration Performance Verification We recommend that...

Страница 58: ...w When you have addressed these issues repeat the wavelength calibration verification to ensure that the instrument has been brought back within specification If the instrument fails the wavelength calibration verification again please contact PerkinElmer SOP 7 Wavelength Calibration Verification 1 Ensure the RamanFlex 400 is switched on If not follow SOP 1 NOTE If you have a RamanFlex 400F with t...

Страница 59: ...tion should fail follow Figure 16 SOP 8 Wavelength Calibration Wavelength calibration should only be performed if the instrument has failed a wavelength calibration verification 1 Ensure the RamanFlex 400 is switched on If not follow SOP 1 2 If you have a fiber optic probe connected to the LED FIBER 1 connector disconnect the probe as described in Removing the FOP on page 48 3 If you have a RamanF...

Страница 60: ...ration Laser frequency calibration should only be performed if the instrument has failed a wavelength calibration verification 1 Ensure the RamanFlex 400 is switched on If not follow SOP 1 NOTE If you have a RamanFlex 400F with two fiber optic probes ensure that the probe not in use is covered 2 Select Raman Instrument from the Setup menu The Setup Instrument tabs are displayed 3 Select the Setup ...

Страница 61: ...mperature at which data is to be acquired Otherwise any data should be used for qualitative analyses only The NIST intensity correction is valid in the recommended operating temperature range 20 C 25 C If you move the instrument to an environment outside this temperature range that is 15 C 20 C or 25 C 30 C we recommend that you perform a NIST intensity correction at this new temperature Contact y...

Страница 62: ... the Setup Instrument Advanced tab and click Toolbox The Adjustments Toolbox dialog is displayed 7 Select The Intensity Calibration dialog is displayed 8 Ensure that you have followed the instructions on the dialog and then click Next The instrument will now perform the intensity calibration routine At the end of the calibration the result is displayed Any data acquired will now be intensity corre...

Страница 63: ...on procedure The wavelength and laser frequency calibrations should only be performed if the instrument fails the wavelength calibration verification procedure The intensity calibration should only be performed on a yearly basis or if the environment temperature and or humidity changes significantly or if the instrument is moved or following a service repair ...

Страница 64: ...Number Description L1320002 Raman fiber optic probe 7 5 mm working distance maximum working temperature 80 C 5 m cabling L1320003 Liquid immersion sleeve for Raman fiber optic probe L1320011 Raman probe long 350 mm long suitable for non contact and liquid immersion Maximum working temperature 200 C maximum working pressure 1500 psi 5 m cabling L1320012 Raman probe max suitable for non contact and ...

Страница 65: ...omized working distance or cable length fiber optic probes contact your PerkinElmer Sales Representative SERS Consumables Part Number Description L1329300 SERS gold colloid 50 nm particles 20 ml L1329307 SERS gold colloid 100 nm particles 20 ml L1329308 SERS gold colloid 200 nm particles 20 ml L1329301 Aggregating agent MgSO4 0 16 M in milli Q water 20 ml L1329303 Standard crystal violet pigment 0...

Страница 66: ...66 RamanFlex 400 Series Getting Started Guide ...

Страница 67: ...Maintenance and Troubleshooting ...

Страница 68: ... not use abrasive or solvent based cleaning materials Always perform a patch test on an inconspicuous 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 c...

Страница 69: ...ct the line power cord If you have an optional deep depletion CCD disconnect the additional line power cord 3 Remove the 4 screws holding the top cover in position and then lift off the cover Figure 17 Removing the top cover of the spectrometer module 4 Unclip the filter covers remove the filters and wash in a mild detergent 5 Dry the filters thoroughly 6 Fit the air filters back into the spectrom...

Страница 70: ... maintenance or servicing of the FOP The immersion sleeve if purchased is manufactured with 316 stainless steel or Hastelloy C and contains either a quartz or sapphire optical window that is sealed The quartz window can be removed for cleaning by unscrewing the end of the immersion tube The sapphire window cannot be removed as it is welded into place If removing the quartz window do not lose the P...

Страница 71: ...ivers Description This may happen if you disconnect the instrument control USB cable and reattach it to a different USB port or if you switch the instrument off and then switch it on again Solution Refer to the Spectrum Administrator s Guide part number L1050095 for details of how to reinstall the drivers Software Problem Spectrum software stops responding Description When you are using the softwa...

Страница 72: ...rom contamination 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...

Страница 73: ...e 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 informat...

Страница 74: ...74 RamanFlex 400 Series Getting Started Guide ...

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