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Using the RamanMicro 200 Series . 83

11.

Focus on the sample of polystyrene.
If you have a motorized stage you can use the joystick or Stage Position controls on the
SetupMicroscope XYZ Stage tab. Alternatively, click

Raman AutoFocus

to focus

using the strongest Raman signal.
If you do not have a motorized stage, you may find it useful to Monitor your sample to

view the Raman signal while manually adjusting the focus.

12.

When the polystyrene sample is optimally focused for Raman signal, select the Setup

Instrument Advanced tab and click

Toolbox

The Adjustments Toolbox dialog is displayed.

13.

Select

The Frequency Calibration dialog is displayed.

14.

Ensure that you have followed the instructions on the dialog, and then click

Next

The instrument will now perform the laser frequency calibration routine. This will take a

few minutes. When the calibration is complete, the result is displayed.

The instrument in now laser frequency calibrated.

In the unlikely event that the laser frequency calibration routine should fail, please perform a

wavelength calibration and repeat the laser frequency calibration.

NOTE: If the calibration fails again, please contact your PerkinElmer Service Representative.

SOP-13: Intensity Calibration

The intensity calibration must be performed using the National Institute of Standards and

Technology (NIST) Standard Reference Material. NIST SRM 2241 is the relative intensity

correction standard for Raman spectroscopy when using 785 nm excitation.

NOTE: NIST calibration is temperature dependent. If you intend to perform quantitative

analyses, you should ensure that your instrument is NIST calibrated at the

temperature at which data is to be acquired. Otherwise, any data should be used for

qualitative purposes 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 strongly recommend

that you perform a NIST intensity correction at this new temperature. Contact your

PerkinElmer Raman Business Unit.

Содержание RamanMicro 200 Series

Страница 1: ...RamanMicro 200 Series Getting Started Guide MOLECULAR SPECTROSCOPY...

Страница 2: ...tability 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...

Страница 3: ...Specifications 34 Finding a Suitable Location for the Instrument 35 Instrument Dimensions 36 Installing Your RamanMicro 200 Series 37 Unpacking the Instrument 38 Lifting the Instrument 39 Attaching th...

Страница 4: ...SOP 10 Wavelength Calibration Verification 79 SOP 11 Wavelength Calibration 81 SOP 12 Laser Frequency Calibration 82 SOP 13 Intensity Calibration 83 Summary 85 Additional Parts and Upgrades 86 Micros...

Страница 5: ...Introduction...

Страница 6: ...pectroscopy Preparing your Facility This chapter shows you how to position your RamanMicro 200 Series instrument and what utilities are required for example electricity and temperature control Install...

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 RamanMicro 200 Series means the RamanMicro 200 and the R...

Страница 8: ...otros En los recuadros como ste se proporciona informaci n sobre este tipo de circunstancias Caution Attention Nous utilisons le terme CAUTION ATTENTION pour signaler les situations susceptibles de p...

Страница 9: ...os recuadros como ste se proporciona informaci n sobre este tipo de circunstancias Warning Danger Nous utilisons la formule WARNING DANGER pour avertir des situations pouvant occasionner des dommages...

Страница 10: ...10 RamanMicro 200 Series Getting Started Guide...

Страница 11: ...Safety Practices...

Страница 12: ...ed 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 interpretati...

Страница 13: ...ature 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 instr...

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 be...

Страница 15: ...ds Power Supplies The RamanMicro 200 is powered by one external PSU The PSU used with the spectrometer module can adjust automatically to a variety of AC power sources as outlined in Table 1 Table 1 P...

Страница 16: ...G 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 repla...

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...

Страница 18: ...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 RamanMicro 200 emits a fo...

Страница 19: ...ided as a general overview only This information is rudimentary and is supplied to assist in the interpretation of this manual Under no circumstances use this information as the basis of a laser safet...

Страница 20: ...ned off when the system is not in use AVOID DIRECT EXPOSURE TO THE BEAM Figure 1 Schematic of the microscope When using the microscope the following precautions must always be observed Never look dire...

Страница 21: ...tion is only applicable to RamanMicro 200F systems equipped with a fiber optic probe The fiber optic probe body incorporates a number of important safety features including Beam attenuator cover Emiss...

Страница 22: ...rt number L1323518 Ensure that the attenuator cap is attached Triggered Fiber Optic Probe Safety When attached to the RamanMicro 200 a triggered fiber optic probe TFOP provides a focused beam of Class...

Страница 23: ...e of Fiber Optic Probe The following calculations show how to calculate a nominal hazard zone These calculations are taken from ANSI Z136 1 1933 A laser safety officer uses these calculations to help...

Страница 24: ...vailable 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 ar...

Страница 25: ...VELENGHS 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...

Страница 26: ...tarted Guide Labels on the Exterior of the Microscope Figure 5 Labels on the microscope LASER APERTURE CAUTION CLASS 3B LASER RADIATION WHEN OPEN AVOID EXPOSURE TO BEAM CAUTION CLASS 3B LASER RADIATIO...

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

Страница 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 underly...

Страница 29: ...scattered and will be detected at either longer wavelengths lower frequencies Stokes scattering or shorter wavelengths higher frequencies Anti Stokes scattering With Stokes scattering some of the inc...

Страница 30: ...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...

Страница 31: ...module by two fiber optic cables The spectrometer module contains the spectrograph and CCD detector The laser supplies light through an objective lens onto the sample The scattered light from the sam...

Страница 32: ...ted and shone on a grating which disperses that light in one dimension The light is then focused onto a photo sensitive CCD detector typically 1024 pixels wide which detects the Raman spectrum Figure...

Страница 33: ...Preparing Your Facility...

Страница 34: ...60 Hz 100 120 V 220 240 V 50 60 Hz 100 240 V 50 60 Hz Primary Fuse See Olympus manual 1 6 A T time lag Laser Class Class 3B Operational Temperature 15 C 30 C Recommended Temperature 20 C 25 C If the e...

Страница 35: ...nch 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...

Страница 36: ...scope module weighs approximately 20 kg Laboratory benching must be strong enough to support the combined weight of the microscope spectrometer module and any ancillary equipment without warping or wo...

Страница 37: ...Installing Your RamanMicro 200 Series...

Страница 38: ...camera module and the spectrometer module LX108870 Spectrum Std for Raman Software Kit Contains the Spectrum Std Software CD LX100877 the Raman Instrument Configuration Disk LX108869 the Raman Spectr...

Страница 39: ...pectrometer and microscope modules each weigh 20 kg To avoid injury or damage to the instrument please use proper lifting techniques WARNING To lift and or move the instrument safely requires two peop...

Страница 40: ...rlock must be 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 L132026...

Страница 41: ...To fit the stage 1 Unpack the stage from the shipping material 2 Remove the objective nosepiece from the microscope by unfastening the grub screw on the right hand side of the nosepiece 3 Carefully l...

Страница 42: ...ck to the socket labeled JOYSTICK on the rear panel of the stage controller box Figure 15 Figure 15 Rear panel of the Stage Controller 2 Connect the cable from the socket on the right side of the stag...

Страница 43: ...ve control knob on the left side of the microscope and then tighten the connections using a hexagonal key 2 Push the focus motor into the sleeve until it touches the drive control and then tighten the...

Страница 44: ...e illumination source in position against the rear of the illuminator module 2 Using the allen key supplied Figure 17 fasten the two screws so that the source is supported 3 Connect the black cable fr...

Страница 45: ...cting the Raman module Connecting the Alignment Camera to the Raman Module The alignment camera module is then connected into the mounting bracket on top of the Raman module and the screws tightened N...

Страница 46: ...s the collected Raman data back to the detector 1 Connect the excitation cable L1323331 from the Raman module to the EXC coupler under LED FIBER 1 on the rear panel of the spectrometer Ensure that the...

Страница 47: ...ure that the end of the fiber with the white cable marker is attached to the Raman module Make sure that the polarizing ridge on the fiber optic cable is aligned with the slot in the coupler casing be...

Страница 48: ...pplied with two keys One should be placed in the instrument and the other should be stored in a safe place Replacement keys L1323503 can be obtained from PerkinElmer A laser safety officer or lab mana...

Страница 49: ...few moments for your instrument to initialize and then connect the microscope alignment camera USB cable to the PC The instrument then needs to be added to the software See Installing a Raman Instrume...

Страница 50: ...agnification Do not push on an objective to rotate the nosepiece but use the revolving plastic ring The microscope objective nosepiece can fit up to 4 objectives 1 Select the highest magnification obj...

Страница 51: ...ment of the Raman coupler Level ii and level iii may be carried out without removing any instrument paneling Level i requires removal of instrument paneling and must only be carried out by a PerkinElm...

Страница 52: ...video camera is required 1 Select the 20x objective lens on the microscope 2 Place a flat sample on a microscope slide We recommend that you purchase the sCAL Raman Calibration Standard L1321843 for...

Страница 53: ...tinue at step 16 to perform a fine adjustment to align the cross hairs with the laser spot OR If no spot is visible a physical adjustment of the camera module is required Continue at step 13 13 Loosen...

Страница 54: ...e see Figure 25 The procedure for alignment is as follows 1 Place a flat sample of silicon on the sample stage We recommend that you purchase the sCAL Raman Calibration Standard L1321843 for this alig...

Страница 55: ...The RamanMicro 200 will start collecting data in the Live display 15 Observe the data displayed in the Live display 16 Very slowly move one of the coupler knobs clockwise and counter clockwise until t...

Страница 56: ...Elmer for advice about removing the fiber optic cables that connect the spectrometer and microscope modules If you need to ship your instrument you must use the original supplied packing materials to...

Страница 57: ...Using the RamanMicro 200 Series...

Страница 58: ...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 ill...

Страница 59: ...e probe body DO NOT ATTEMPT TO USE THE PROBE BODY IN SUCH AN ENVIRONMENT WITHOUT THE USE OF AN IMMERSION SLEEVE L1320003 If required contact PerkinElmer for further details Attaching and Removing the...

Страница 60: ...t in the coupler casing before carefully pushing the cable into the coupler 7 Screw the screw caps from the fiber optic cables onto the coupler casings 8 If you have a standard probe connect the DIN c...

Страница 61: ...on a stand and adjusting the focal spot on the surface of the sample Whenever possible powders should be compacted down and thin films of materials should be folded so that the sample covers the enti...

Страница 62: ...ntainer If this glass fluorescence is a problem and it is not possible to use quartz containers then it is possible to acquire a spectrum of the container and spectrally subtract this from any spectra...

Страница 63: ...SOPs demonstrate how to collect data when your samples are on the microscope stage For SOPs that demonstrate how to collect data using a fiber optic probe please refer to Fiber Optic Probe SOPs on pag...

Страница 64: ...quired enter your User name and Password and then click OK An instrument selection dialog is displayed 11 Select the Instrument you want to use OR If you want to work with data that has been collected...

Страница 65: ...he instrument is used 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 las...

Страница 66: ...ct the Setup Instrument Basic tab 4 Ensure that Microscope XYZ Stage is selected in the Accessory drop down list The options available will depend upon your instrument configuration 5 Ensure that the...

Страница 67: ...ftware to move the microscope stage up to 0 mm approximately 25 mm travel The stage will stop at some point between 0 mm and 1 mm at the maximum length of travel for the z axis motor 14 Ensure that yo...

Страница 68: ...ate you will need to reset the stage If you continue to move the stage the cable can become trapped and the motor could be damaged SOP 4 Sample Positioning using a Manual Stage 1 Lower the microscope...

Страница 69: ...down list The microscope is supplied with 5x 20x and 50x objective lenses 12 Select the appropriate Sample Holder from the drop down list 13 Select the Setup Microscope tab Figure 35 Setup Microscope...

Страница 70: ...ave data you must collect spectra Click to exit the Live display You are now ready to acquire data For more information see SOP 6 The most appropriate microscope objective for your analyses will depen...

Страница 71: ...s available will depend upon your instrument configuration 7 Select 5x from the Microscope Objective drop down list The microscope is supplied with 5x 20x and 50x objective lenses 8 Load your sample i...

Страница 72: ...ideo Autofocus to perform an automatic video focus when you are close to the sample surface when the microscope illumination is on and the switch position set to Bright Field Alternatively select the...

Страница 73: ...he most efficient Raman collection from thin samples such as films or wafers but low magnification objectives are better for macro samples such as tablets bulk plastics and tissue samples NOTE Raman s...

Страница 74: ...the data collection parameters such as how background scans are collected select the Setup Instrument Data Collection tab To display the Setup Instrument tabs select Raman Instrument from the Setup m...

Страница 75: ...epeat collections If you exit Spectrum software the instrument settings will be remembered when you restart Spectrum providing that they have been used to collect data If you want to return to the def...

Страница 76: ...321940 SOP 7 Selecting the Fiber Optic Probe 1 Ensure that the RamanMicro 200 is switched on and that the fiber optic probe is connected to the instrument If not follow SOP 1 2 Select Raman Instrument...

Страница 77: ...live display option must be selected on the Setup Instrument Data Collection tab 1 Click The Live tab will be displayed and real time spectral acquisition will commence 2 Adjust the Laser power on the...

Страница 78: ...ion 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...

Страница 79: ...alibration verification to ensure that instrument has been brought back within specification If the instrument fails the wavelength calibration verification again please contact PerkinElmer NOTE Stray...

Страница 80: ...ries to minimize stray light from interfering with the calibration verification 11 Focus on the polystyrene sample If you have a motorized stage you can use the joystick or Stage Position controls on...

Страница 81: ...connector Figure 42 Attaching the calibration accessory NOTE As wavelength calibration is not required on a regular basis the external neon calibration accessory is not included in the basic RamanMicr...

Страница 82: ...croscope 3 Place a polystyrene sample L1181228 in a suitable sample holder 4 Select Raman Instrument from the Setup menu The Setup Instrument tabs are displayed 5 On the Setup Instrument Basic tab sel...

Страница 83: ...n the unlikely event that the laser frequency calibration routine should fail please perform a wavelength calibration and repeat the laser frequency calibration NOTE If the calibration fails again ple...

Страница 84: ...ect Microscope or Microscope XYZ Stage as appropriate from the Accessory drop down list 7 Select Microscope 50x from the Objective drop down list 8 Select the appropriate Sample Holder in the drop dow...

Страница 85: ...the NIST sample is correctly positioned and that the laser key switch is set to on ARM 16 Repeat steps 2 15 for each objective lens 17 Remove the intensity correction standard and store safely Summary...

Страница 86: ...istance objective lens Sampling Accessories Part Number Description L1323514 Quartz microscope slide 25 75 1 mm L1860335 Tablet holder kit for motorized stage L1860336 Powder holder kit for motorized...

Страница 87: ...andard crystal violet pigment 0 25 ml L1329304 Disposable micropipettes 200 l 100 pack L1329305 Disposable micropipettes 50 l 100 pack L1329306 Disposable micropipettes 2 l 100 pack Safety and Calibra...

Страница 88: ...emperature 500 C maximum working pressure 3000 psi 5 M cabling L1320013 Purge Jacket for Raman probe max required to enable max probe operation at temperatures between 200 C and 500 C L1320030 Trigger...

Страница 89: ...Maintenance and Troubleshooting...

Страница 90: ...cleaning materials Always perform a patch test on an inconspicuous area before you clean the entire instrument Avoid spilling liquid into the instrument or accessories Clean all external spills immed...

Страница 91: ...wer supply unit 2 Disconnect the line power cord 3 Remove the 4 screws holding the top cover in position and then lift off the cover Figure 43 Removing the top cover of the spectrometer module 4 Uncli...

Страница 92: ...odification by anyone other than PerkinElmer will invalidate the warranty Refer to the Olympus manual provided with your microscope for the replacement of the light bulb Maintenance and Service of the...

Страница 93: ...e stage controller disconnect it from the power supply and remove the mains cord 2 Insert a screwdriver into the slot at the side of the fuse drawer and pull out and flip to one side over the mains in...

Страница 94: ...tion This means that for some reason the interlock system is detecting an open circuit Solution 1 Ensure all interlocks including any remotely interlocked doors are closed properly Solution 2 Ensure y...

Страница 95: ...tup Microscope XYZ Stage tab click Toolbox and then select Reset Stage The motorized accessory will now reset itself Solution 4 If the above solutions do not solve your problem you should contact your...

Страница 96: ...om 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 Perk...

Страница 97: ...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...

Страница 98: ...98 RamanMicro 200 Series Getting Started Guide...

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