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102 . Spotlight 400 Series User’s Guide

Accessories

Description

Part Number

Spare fuse for imager (2 A time-lag, 250 V)

04970839

Spare fuse for stage controller (1.6 A time-lag, 250 V)

09991641

Visible Polarizer Kit

L1860294

Sampling Accessory Kit

L1860250

MCT Detector Accessory Kit

L1860554

IR Polarizer Assembly

L1860408

Holder for 13 mm Sampling Disks

L1860409

Hot Stage Accessory (110 V)

N1870184

Compression Cell

N1870185

Hot Stage Accessory (220 V)

N1870188

Rotatable Sample Disk Holder

N1873039

Holder for Reflection-Transmission Measurements

N1873124

BaF

Window (1 mm thick)

N9302611

BaF

Window (2 mm thick)

N9302612

ZnSe Window

N9302613

NaCl Window

N9302614

KBr Window

N9302615

Miniature Diamond Anvil Cell

N9302618

Spare Germanium crystal

L1860268

Spare Silicon crystal

L1860269

Gold Mirror and white reflector Slide (InGaAs systems

only)

L1860438

Sample Preparation Tools

These are described in

Tools for Sample Preparation

on page 49.

Summary of Contents for Spotlight 400 Series

Page 1: ...Spotlight 400 Series User s Guide MOLECULAR SPECTROSCOPY...

Page 2: ...ot 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...

Page 3: ...ements 24 Safety Specifications 25 Imager 25 Stage Controller 25 Overview of the Spotlight Imaging System 27 A Guided Tour of the Spotlight Imaging System 28 Connections 29 Modes of Operation 31 The O...

Page 4: ...ion 79 Fitting the ATR Crystal Holder to the Imager 80 Measuring the Energy in Reflectance Mode 81 Adjusting the Height of the Crystal 82 Centering the Crystal 82 Checking the Infrared Alignment 84 Re...

Page 5: ...rlier version of SpectrumIMAGE software 108 Installing the SpectrumIMAGE software 109 Appendix 2 Amending the Power Options Display Settings 114 Power Options 114 Display Options 114 Appendix 3 Decont...

Page 6: ......

Page 7: ...Introduction...

Page 8: ...on using and maintaining your imaging system Getting Ready to use the Imaging System gives you information on how to set up your imaging system at the beginning of the day s work to make sure that it...

Page 9: ...at the same time for example ALT F All eight digit numbers are PerkinElmer part numbers unless stated otherwise Spectrometer refers to the Frontier IR System Spectrum 100 Series Spectrum 400 Series Sp...

Page 10: ...s 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 provoq...

Page 11: ...los 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...

Page 12: ...are has on screen Help which you can access by selecting Contents from the Help menu in each SpectrumIMAGE window or by clicking the Help button in a dialog This is a reference manual which assumes th...

Page 13: ...Warnings and Safety Information...

Page 14: ...or Spectrum 400 FT IR FT FIR spectrometer operates in the MIR range only The system does not include a filter box The Spotlight 400 imaging system consists of an FT IR imager an FT IR spectrometer Fro...

Page 15: ...spills immediately If anything that is spilled enters the main body of the imager or spectrometer switch off the power and call a PerkinElmer Service Engineer DO wear safety glasses and protective gl...

Page 16: ...by a skilled person who is aware of the hazard involved Whenever it is likely that the imager and stage controller are unsafe make them inoperative The imager and stage controller may be unsafe if th...

Page 17: ...er only into electricity supply sockets that are provided with a protective ground earth connection The stage controller and the imager must be earthed WARNING Any interruption of the protective groun...

Page 18: ...trical supply inlet at the rear of the imager and of the stage controller are not obstructed To allow nitrogen to disperse WARNING Liquid nitrogen is used to cool the MCT detector Oxygen depletion in...

Page 19: ...Labels Labels are fixed to the imager in the locations shown in Figures 2 5 Figure 2 Label side of imager Caution Risk of Danger When this label is attached to an instrument it means Caution risk of...

Page 20: ...r of imager Figure 4 Label inside dewar lid Refer to Cooling the MCT Detector on page 41 Figure 5 Label rear of stage controller Power 100 230V 50 60Hz 75 VA Warning Disconnect supply cord before open...

Page 21: ...cal Safety WARNING When you are using a motorized stage do not place your fingers between the moving and fixed parts of the stage The motors driving the stage from side to side front to back or up and...

Page 22: ...rkinElmer service department It is necessary to separate the imager from the spectrometer before lifting either instrument If you have a dual range imaging system where a filter box is fitted between...

Page 23: ...d tested to meet the requirements of EMC Directive 2004 108 EC FCC Rules and Regulations This product is classified as a digital device used exclusively as industrial commercial or medical test equipm...

Page 24: ...in the drawer on the mains inlet connector NOTE No voltage selection is required Stage Controller The stage controller can operate on electricity supplies of 50 or 60 Hz and on a voltage range of 100...

Page 25: ...Controller Power supply 100 240 V 10 50 60 Hz Primary fuse 1 6 A T time lag The stage controller is not designed for use with all three motors simultaneously over extended periods Maximum speed 6 mm s...

Page 26: ...26 Spotlight 400 Series User s Guide...

Page 27: ...Overview of the Spotlight Imaging System...

Page 28: ...using reflectance diffuse reflectance or transmittance sampling modes these have different detector gain settings to help optimize the quality of data from a variety of samples Array and single point...

Page 29: ...ler Figure 7 Electrical connections top rear of imager Connections to stage controller connects to PC Ethernet cable communications 10101 connects to PC RS232 debug port for service use only 9 way D t...

Page 30: ...n on the connections Connects to PC RS232 9 way D type Connects to stage controller 15 way D type Stage Z connects to stage controller for Z motor drive control Connects to imager Drive Signals for th...

Page 31: ...ows you to collect data from an area of the sample surface with a spatial resolution up to four times better than conventional reflection or transmittance IR imaging techniques NOTE Diffuse reflectanc...

Page 32: ...n transmittance and reflectance diffuse reflectance operation Dichroic mirrors form part of the optical system The dichroic mirrors used in the imager reflect infrared and transmit visible light Viewi...

Page 33: ...n condenses the beam to an appropriate size for a microscopic sample and focuses it at the sample position The upper cassegrain collects light from the sample and sends it upward through the aperture...

Page 34: ...in collects the reflected light from the sample and sends it upward through the aperture The lower transmission illuminator is also active in reflectance and diffuse reflectance modes giving simultane...

Page 35: ...te the sampling area and the visible image is used to determine the dimensions of the IR image Collecting an Image in Transmittance Collecting an image in transmittance differs from viewing in transmi...

Page 36: ...of the infrared beam for collecting an image in reflectance diffuse reflectance Changing the IR Magnification Between the upper cassegrain and the variable aperture there is a mechanism for changing t...

Page 37: ...d disk with at least 1 GB free space as an NTFS drive NOTE We have locked the system into using an NTFS drive because the alternative FAT32 file system doesn t provide enough protection at a folder an...

Page 38: ...Windows XP Professional Service Pack 3 or later or Windows 7 Professional Service Pack 1 or later Internet Explorer Internet Explorer 6 or later is used for displaying the HTML help pages QuickTime Qu...

Page 39: ...Getting Ready to use the Imaging System...

Page 40: ...pectrometer is switched on Switch the stage controller and imager on Cool the detector if using an MCT detector the InGaAs detector does not require cooling Set up the imager Focus the imager We recom...

Page 41: ...on or unconsciousness can occur in seconds and without warning See Location and Ventilation on page 18 WARNING The extremely low temperature of liquid nitrogen can burn skin and eyes Avoid exposure by...

Page 42: ...war 4 Add another one and a half funnels of liquid nitrogen Stand back and wait two minutes This nitrogen also vaporizes as the dewar continues to cool The two minute wait enables the bubbling to sett...

Page 43: ...e stage controller A light at the front comes on 4 At your PC click Start and then select SpectrumIMAGE in the SpectrumIMAGE group in the PerkinElmer Applications group under Programs The SpectrumIMAG...

Page 44: ...are examining the sample in transmission mode you may need to adjust the position of the lower cassegrain so that the field of view is evenly illuminated Adjust the Correction control by clicking on t...

Page 45: ...nuator kit part number L1160560 containing 1 T 4 T 6 T 14 T and 32 T attenuators The attenuators attach magnetically to the external beam window of the spectrometer Use of the 32 T attenuator is recom...

Page 46: ...46 Spotlight 400 Series User s Guide...

Page 47: ...Preparing Samples...

Page 48: ...il and undistorted absorption bands The area of the sample must be large enough to give an adequate signal or the scan time must be increased Preparing a sample therefore often involves flattening it...

Page 49: ...d Item Use Holder for 13 mm disks Supporting 13 mm disks on the sample stage Slides glass box Supporting samples for sample preparation Rotating 13 mm disk holder Supporting samples and allows rotatio...

Page 50: ...cking up extremely small objects Roller knife Cutting knife end and flattening roller end Steel probe Pulling samples apart separating fibers Forceps 4 inch Cd plated Picking up small objects Tungsten...

Page 51: ...Preparing Samples starting on page 54 Miniature Diamond Anvil Cell part number N9302618 Fiber Optic Illuminator part number N9302602 Microtome Tool Part Number Microprobe with right angle bend N930260...

Page 52: ...ddition to the items provided with the Spotlight imaging system we recommend that you have the following available Tape with adhesive on both sides double sided tape for holding long or large samples...

Page 53: ...0 cm 1 It can break or crack easily NaCl Sodium chloride transmits infrared down to 600 cm 1 Otherwise its properties are similar to KBr ZnSe Zinc selenide is not hygroscopic Its transmittance cut off...

Page 54: ...ra in reflectance or diffuse reflectance mode Samples rolled on windows transparent to infrared can be examined in transmittance If you flatten fibers on a glass microscope slide they can then be peel...

Page 55: ...sed with laminates plastics films paint chips and paper To cut a wedge shaped piece from a relatively thick sample Hold the sample in tweezers as you slice a thin wedge from it with a razor blade Tape...

Page 56: ...the size and porosity of the sample acrylic and epoxy resins Although these are commonly used in light microscopy they are not recommended for infrared because they are hard to remove and can cause sp...

Page 57: ...es place some KBr in the cell and collect a background spectrum through it Figure 18 The miniature diamond anvil cell Pressing elastomers between windows If your sample is elastic and you are compress...

Page 58: ...end cools tap the polymer into it then heat the sample gently The pyrolyzed polymer condenses on the walls of the pipette The filler is left behind as ash 3 Score and break the pipette between the as...

Page 59: ...eld of view 4 Adjust the infrared aperture until only the particle that is of interest is visible You can easily pick up extremely small particles and transfer them with a very fine pointed tungsten n...

Page 60: ...can analyze the sample in reflectance If the sample is only weakly reflective or scatters the signal strongly use the diffuse reflectance sampling mode If the substrate is opaque scrape off a sample o...

Page 61: ...of the salt plate until the solvent evaporates Repeatedly jab a small area of the salt plate with a tungsten probe Leave the resulting small salt particles in the well that is produced The capillary...

Page 62: ...62 Spotlight 400 Series User s Guide...

Page 63: ...Techniques for Collecting IR Images and Spectra...

Page 64: ...is in the center 4 To focus the visible image displayed in the Monitor Visible window use the Z control on the joystick or the Focus control on the Control window 5 The Monitor Visible window displays...

Page 65: ...pt salt windows with window retainers and a special wrench to apply pressure across the windows The sample is held between the two windows The compression cell fits into the sample slide holder on the...

Page 66: ...phase transitions and temperature dependent chemical reactions Infrared microscopy can provide detailed molecular structural information for systems undergoing phase transitions this information is no...

Page 67: ...lick Park again The lower cassegrain bracket moves to its lowest position 7 Lower the stage using the Z control on the joystick CAUTION Once the lower cassegrain is removed lowering the stage when at...

Page 68: ...Raise the stage using the Z control on the joystick to its highest position 3 Click Zero on the Control dialog 4 Slide the cassegrain assembly back into the dovetail connector as far as it goes NOTE T...

Page 69: ...tem enables you to purge the spaces around the sample and the infrared beam typically with nitrogen or dry air to provide a dry controlled atmosphere WARNING Do not use flammable gases for purging Par...

Page 70: ...isplaces air from the path of the infrared beam Purging the system 1 Make sure that all parts of the purge system as listed above are in place 2 Set up the imager See Getting Ready to use the Imaging...

Page 71: ...ws the passage of only those waves that have their plane of vibration in one particular direction The light that emerges is said to be polarized and is represented on the right side of Figure 24 Figur...

Page 72: ...ange in polarization is dependent on the wavelength the color of the light emerging changes with the distance traveled through the sample and the amount of birefringence encountered Applications Diffe...

Page 73: ...thick and their cylindrical shape can cause lensing effects For these reasons fibers are usually flattened in preparation for infrared microspectroscopy This flattening affects the birefringence of t...

Page 74: ...lyzer in with the wheel facing towards you It has two positions The first position allows the full beam to pass through When the analyzer is inserted fully the polarizing element is in the beam Figure...

Page 75: ...parallel to or perpendicular to the bond direction For example stretching an acrylic fiber aligns the molecules with the general direction of the polymer chains parallel to the fiber axis and the nit...

Page 76: ...perture for the infrared polarizer Figure 29 Figure 29 Infrared polarizer position 2 Slide the analyzer into the vertical slot on the sample holder that can be seen through this aperture The flat side...

Page 77: ...as a high refractive index An infrared beam enters the crystal and is internally reflected within the crystal creating an evanescent wave At each reflection inside the crystal the wave continues beyon...

Page 78: ...he upper cassegrain and is focused at the sample position It is reflected once within the crystal then the totally internally reflected beam is collected by the rear portion of the upper cassegrain wh...

Page 79: ...00 cm 1 Si 7800 cm 1 to 800 cm 1 Area of contact with sample Nominally 100 m diameter flat surface Single internal reflection from surface Maintenance The ATR assembly may be removed see Removing the...

Page 80: ...mation on how to do this see the Spectrum software on screen Help 3 Hold the crystal assembly under the upper cassegrain Be careful not to change the alignment of the two adjusting levers 4 Fit the tw...

Page 81: ...focus the beam on the surface of the mirror using the Z control on the joystick There are usually dust particles or scratches on the surface that you can use to focus on 7 Click Aperture on the Contr...

Page 82: ...ng the bar clockwise and slowly lowering the toggle bar 2 Using the knurled height adjustment nut adjust the height of the crystal so that it just rests on the mirror under positive pressure Figure 32...

Page 83: ...If the impression is in the center of the field of view the assembly is aligned If the impression is not in the center of the field of view 1 Loosen the two knurled thumb nuts under the ATR crystal h...

Page 84: ...on 3 Lower the crystal onto the reference mirror 4 Select Aperture on the Control dialog The IR Aperture dialog is displayed 5 Enter 100 in the Width and Height text boxes 6 Click OK The IR Aperture...

Page 85: ...rometer to the internal sample compartment See the Spectrum on screen Help for further information 3 Make sure that the ATR crystal is in the raised position 4 Screw the plastic protective cover in pl...

Page 86: ...adjusting nut The crystal assembly is under spring pressure If you do not hold the assembly in place the spring may be lost 4 Remove the crystal assembly Leave the spring in the ATR crystal holder 5...

Page 87: ...ean the crystal NOTE Do not use acetone or xylene to clean the crystal 1 Pour a small volume of a solvent into a shallow dish 2 Using the Z control on the joystick lower the sample stage to allow the...

Page 88: ...n the Monitor Visible window and focus on the surface of the mirror using the Z control on the joystick There are usually dust particles or scratches on the surface that you can use to focus on 5 Lowe...

Page 89: ...e mirror slide from the stage and put a new slide with the sample on it on the stage 3 Make sure that Point mode is selected on the Control dialog 4 Make sure that the imager is in reflectance mode by...

Page 90: ...ntact raise the stage slightly using the arrows in the Focus section of the Control dialog 6 When you are happy with the displayed spectrum click 7 Display the Scan menu in the Stage Control window an...

Page 91: ...it to the detector In addition the diffuse reflectance sampling mode compensates for any loss of signal by increasing the gain of the detector A problem often encountered when using the diffuse reflec...

Page 92: ...pplicable to mid infrared applications Specular reflectance is reflection in one direction Figure 35 This is the type of reflection that occurs from a smooth polished surface Absorption information ca...

Page 93: ...E Reflection absorption is mainly applicable to mid infrared applications Reflection absorption occurs when the incident radiation passes through a thin absorbent film that is on a reflective surface...

Page 94: ...94 Spotlight 400 Series User s Guide...

Page 95: ...Maintenance...

Page 96: ...ll This involves Inspecting the imager Protecting the imager Cleaning the optics Cleaning the imager cover Renewing the fuse Testing the stage controller Renewing the stage controller fuse Service Thi...

Page 97: ...n the imager is covered Cleaning the Optics The imager was aligned cleaned and sealed at the factory Do not attempt to take it apart CAUTION Avoid the excessive use of solvents Flowing solvents dissol...

Page 98: ...it from the power supply 2 Insert a screwdriver into the slot at the side of the fuse drawer pull out and flip to one side over the mains inlet The fuse may now be removed 3 Fit the replacement fuse...

Page 99: ...stage are powerful and do not stall easily The joystick operates in the following manner Left Right joystick movement gives X movement of the stage Top Bottom joystick movement gives Y movement of th...

Page 100: ...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 inlet The fuse may now be removed 3 Fit the replacement fuse...

Page 101: ...it performing properly and to compensate for wear We recommend that the Spotlight imaging system is cleaned examined and adjusted periodically by a PerkinElmer Service Engineer NOTE If you experience...

Page 102: ...e Accessory 110 V N1870184 Compression Cell N1870185 Hot Stage Accessory 220 V N1870188 Rotatable Sample Disk Holder N1873039 Holder for Reflection Transmission Measurements N1873124 BaF2 Window 1 mm...

Page 103: ...100 110 120 V Wire Color 220 230 240 V Ground Earth Green or Green Yellow Green Yellow Live Black Brown Neutral White Blue WARNING To ensure safe and satisfactory operation of the instrument it is es...

Page 104: ...or 60 Hz and at voltages in the range 100 to 240 V without adjustment The stage controller will operate at all voltages in the range 100 240 V and frequencies of 50 or 60 Hz without adjustment Fit the...

Page 105: ...meter The connection labeled MOTOR X on the stage controller plugs into the connector next to the red dot on the motorized stage Figure 40 Electrical connections for the imager with USB camera dual ra...

Page 106: ...106 Spotlight 400 Series User s Guide...

Page 107: ...Appendices...

Page 108: ...imaging system If you believe a hardware or firmware upgrade may be required consult a PerkinElmer Service Engineer Before installing the SpectrumIMAGE software you must uninstall any existing Spectru...

Page 109: ...and print the release notes which can be found as a rtf file at the root of the SpectrumIMAGE Software DVD These notes contain important information that may not be in this User s Guide or the on scre...

Page 110: ...de 4 Select I accept the terms of the license agreement and then click Next The Customer Information page is displayed 5 Complete the User Name Organization and Licence Number fields and then click Ne...

Page 111: ...file in C Windows CAUTION Do not select Default calibration settings not generally recommended This option is only for PerkinElmer Service Engineers For a new installation the default calibration sett...

Page 112: ...the calibration media must remain inserted until the installation is complete OR If you are upgrading an earlier SpectrumIMAGE installation the Keep existing ini file settings page is displayed This o...

Page 113: ...0 Click Next During installation C Windows pelimage ini is created If a previous installation of SpectrumIMAGE has already created this file on your PC any new settings such as those required for the...

Page 114: ...ay after Turn off hard disk after Sleep after and Hibernate after Display Options Windows 7 1 Place the mouse pointer in a clear area of the desktop click the right mouse button and then select Screen...

Page 115: ...for the graphics card is displayed 4 Select the Monitor tab and then set the Screen refresh rate to 75 Hertz 5 Click Apply and then click OK 6 Close the settings dialog for the graphics card and then...

Page 116: ...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 Per...

Page 117: ...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...

Page 118: ...tors 45 C Cleaning ATR crystal 87 imager optics 97 Compliance EC directive 23 EMC 23 FCC 23 Connections imager 105 microscope 29 power supply 103 stage 29 stage controller 30 Conventions 9 Cooling 18...

Page 119: ...bers 60 73 fibrous solids 60 filled polymers 58 flattening 48 holder 49 laminates 72 large 49 micro amounts 58 microsampling toolkit 50 minerals crystals 73 other useful tools 51 particles 59 polymer...

Page 120: ...ation 18 Viewing in reflectance 34 in transmittance 33 sample 32 Visible Polarizer biological substances 73 equipment 73 fibers 73 films 73 laminate structures 72 minerals crystals 73 operation 74 the...

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