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Collecting Spectra with the Microscope

Positioning the Sample

When you use the microscope to collect spectra, you must center the sample on

the sample stage before you collect the background spectrum. This enables you to

set the correct aperture for the sample and then use that aperture when collecting

the background spectrum.

Take out any aperture that is in the retaining well.

Place the sample on the sample stage.
If necessary, secure it with the slide clip:

Figure 18 Parts of the Sample Stage

To set the microscope for viewing a sample, turn the View/IR knob to View.

The detector mirror moves out of the optical path, and the illuminator is

switched on.

Set the Trans/Refl knob to the required position for viewing.

Turn the Illuminator knob to adjust the light to an adequate level for viewing.

NOTE: If you need to increase the illumination during the procedures that follow,

move the knob to a higher setting.

Stage Controls

Slide Clip

Summary of Contents for MultiScope System

Page 1: ...MultiScope System Microscope User s Reference ...

Page 2: ...ors 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 or translated into any language without the prior written permission of PerkinElmer...

Page 3: ...uirements 29 Overview of the MultiScope System Microscope 31 Features of the MultiScope System Microscope 32 Applications 35 The Optical System 36 Specifications 42 Getting Ready to Use the Microscope 45 Getting Ready to Use the Microscope 46 Setting Up the FT IR 47 Cooling the MCT Detector 48 Setting Up the Microscope 51 Viewing the Sample 52 Tutorial Using the Microscope 53 Introduction to the T...

Page 4: ...g the Optional Equipment 96 Visible Polarizer Option 97 Infrared Polarizer Option 103 Collecting a Spectrum in an Inert Atmosphere 107 Applications 109 Applications 110 Reflectance FT IR Microspectroscopy 111 Polymers 115 Criminalistics 117 Biological Materials 118 Product Contaminants 119 Maintenance 123 Maintenance 124 Selecting the Microscope Voltage and Renewing the Fuse 127 Aligning the MCT D...

Page 5: ...Introduction ...

Page 6: ...ins the procedures you follow at the beginning of the day s work to make sure the microscope is set up properly Preparing Samples describes techniques for preparing many types of microscopic samples It includes descriptions of the sample preparation tools provided with or available for the PerkinElmer MultiScope System Microscope Collecting Spectra with the Microscope contains general procedures f...

Page 7: ...T IRs Information on using your FT IR is found in the manuals that were supplied with it Optional equipment Certain items of the optional equipment for the microscope have their own manuals Consult the appropriate manual before attempting to use the equipment ...

Page 8: ...ave some familiarity with operating the FT IR Specifically you must be able to Set the FT IR to use the external beam Monitor the signal Set the gain Collect background and sample spectra This User s Reference does not give detailed procedures for these operations Consult the manual for the FT IR ...

Page 9: ... 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 10: ...o en otros En recuadros éste se proporciona información sobre este tipo de circunstancias F 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 I Caution Attenzione Con il termine CAUTION ATTENZIO...

Page 11: ...ecuadros como éste se proporciona información sobre este tipo de circunstancias F 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 I Warning Pericolo Con il termine WARNING PERICOLO vengono segnalat...

Page 12: ...Instrument Caution hot surface Caution risk of electric shock Caution laser radiation hazard Caution risk of danger Refer to accompanying documents in all cases where this symbol is used to find out the nature of the potential HAZARD and any actions which have to be taken ...

Page 13: ... IRs In this User s Reference we have used Spectrum GX to indicate Spectrum GX System 2000 Spectrum 2000 System 2000R NIR FT Raman Spectrum 2000R NIR FT Raman FT IR and Spectrum GXR spectrometers Spectrum BX The MultiScope System Microscope can be used with Spectrum BX Paragon 1000PC and Spectrum 1000 FT IRs In this User s Reference we have used Spectrum BX to indicate Spectrum BX Paragon 1000PC a...

Page 14: ...14 MultiScope System Microscope User s Reference ...

Page 15: ...Warnings and Safety Information ...

Page 16: ...y glasses and protective gloves when you are filling the detector dewar with liquid nitrogen Slowly pour the liquid nitrogen into the dewar Stand back from the detector during filling since liquid nitrogen may be expelled from the dewar flask Use only liquid nitrogen DO NOT stare into the laser beam Laser radiation will be present when the microscope is connected to an FT IR spectrometer Typically...

Page 17: ...not specified by the manufacturer the protection provided by the microscope may be impaired Only use the MultiScope System Microscope indoors under the following conditions Temperature 15 C to 35 C Relative humidity 75 maximum non condensing If possible avoid any adjustment maintenance and repair of the opened operating instrument If any adjustment maintenance and repair of the opened instrument i...

Page 18: ...designed to be safe under the following conditions Indoor use Altitude up to 2000 m Ambient temperatures of 5 C to 40 C A maximum ambient relative humidity of 80 for temperatures up to 31 C decreasing linearly to 50 relative humidity at 40 C Mains fluctuations not exceeding 10 of the nominal voltage ...

Page 19: ...on for your mains supply The drawer is also the voltage selector When the MultiScope System Microscope is connected to its electricity supply terminals may be live Removing covers other than those which can be removed by hand is likely to expose live parts Capacitors inside the microscope may still be charged even if the microscope has been disconnected from all voltage sources Disconnect the micr...

Page 20: ...y however a temporary conductivity caused by condensation must be expected An IEC Installation Category Overvoltage Category II classification suitable for connection to local level power supplies The instrument is designed to be safe under transient overvoltages typically present on the MAINS supply NOTE The normal level of transient overvoltages is impulse withstand Overvoltage category II of IE...

Page 21: ...stem To allow for adequate cooling the system should not be sited near to room heating equipment for example central heating radiators There should be a minimum gap of at least 15 cm 6 inches from the top and side surfaces of the microscope to permit adequate cooling WARNING Make sure that the switch at the electrical supply inlet at the rear of the microscope is not obstructed ...

Page 22: ...ser s Reference Laser Safety Regulations When connected to a PerkinElmer FT IR spectrometer the MultiScope System Microscope complies with IEC Publication 60825 1 2007 Safety of laser products Equipment classification and requirements ...

Page 23: ...ror and the upper cassegrain mirror when the microscope purge covers are displaced or removed In Transmittance mode the laser radiation propagates upwards from the lower cassegrain input mirror In Reflectance mode the laser radiation propagates downwards from the upper cassegrain mirror a sample reflects the radiation upwards along the same path see Figure 2 on page 25 At the Remote Aperture betwe...

Page 24: ...wn on the following pages Figure 1 and Figure 2 Class II Class 2 laser warning labels are attached to the Model 1600 Spectrum BX Spectrum RX version of the microscope No laser warning labels are required on the Class I Class 1 Spectrum GX Spectrum One and Spectrum 100 Series versions of the microscope The laser apertures are shown in Figure 2 and described in Accessible Levels of Laser Radiation o...

Page 25: ...e environmental conditions verify that all features of the unit are functioning properly Visually inspect the housing periodically to verify that no panels are loose or distorted so as to allow access to laser radiation in the interior Verify that operation of the external beam lever on a Model 1600 Spectrum BX or Spectrum RX blocks laser radiation from entering the microscope Verify that all requ...

Page 26: ...26 MultiScope System Microscope User s Reference Warning Label Near the Lamp Housing Caution hot surface ...

Page 27: ...cope only by the base Do not attempt to lift it by the knobs cassegrain assembly or other attachments We recommend that the microscope is lifted by 2 adults Consult local codes of practice issued by safety advisors before attempting to lift the microscope Do not move the microscope after it has been installed without consulting your local PerkinElmer service department ...

Page 28: ...ith the EMC standards EN 55011 ISM class A rf emissions and the generic immunity standard EN 50082 1 for residential commercial and light industrial environments 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 b...

Page 29: ...requent transient loads on the same supply circuit The microscope can operate on electricity supplies of 50 or 60 Hz and on voltage ranges of either 100 to 120 V or 220 to 240 V The primary fuses 2 A time delay 250 V UL CSA are in the voltage selector drawer on the mains inlet panel One fuse is connected in the live line of each voltage range The voltage selector for the microscope is located on t...

Page 30: ...croscope Place the microscope in an environment that is relatively dust free Make sure that the bench top is free from vibrations or mechanical shocks Do not place the microscope near to room heating equipment for example central heating radiators Leave at least 15 cm 6 inches from any vertical obstacle to the sides of the microscope to permit an adequate flow of cooling air ...

Page 31: ...Overview of the MultiScope System Microscope ...

Page 32: ...pe System Microscope Figure 3 can be used with any of the following PerkinElmer FT IRs Spectrum 100 Series Spectrum One Model 1600 Model 16PC Spectrum RX Spectrum BX or Spectrum GX The microscope enables you to collect the spectra of extremely small samples It is designed around PerkinElmer cassegrain collection optics for high performance infrared microspectroscopy The microscope is combined with...

Page 33: ...ical aperture for efficient collection of radiation Video viewer linked to a framegrabber for optical microscopy MCT detector Gives spectra with high signal to noise ratio No mechanical errors in switching from viewing to infrared The same cassegrain is used to send both infrared radiation and visible light to the remote aperture The location of the image does not change when you switch from viewi...

Page 34: ...e Spectra can be collected in either reflectance or transmittance modes A micro ATR accessory is available as an optional extra Internal coaxial illumination with variable intensity Whole field aperture kit with independent variable knife edge apertures The apertures are transparent to visible radiation but opaque to infrared making it easier to locate the point of interest on the sample ...

Page 35: ... are described fully in Applications on page 109 Reflectance FT IR microscopy including diffuse reflectance spectra of powders specular reflectance spectra of coated and uncoated materials reflection absorption spectra Polymers Textiles Criminalistics forensic work including transmittance spectra of fibers paint chips drugs Biological materials Product contaminants including microcontaminants on s...

Page 36: ... viewing the sample and infrared collecting a spectrum by moving only one control the View IR knob The selection between transmittance and reflectance is equally simple This section describes what happens within the optical system when you make these selections Viewing When you view a sample with the video viewer you are really looking at the conjugate image of the sample located at the remote ape...

Page 37: ...grain C1 Cassegrain C1 condenses the beam to an appropriate size for a microscopic sample and focuses it at the sample position Cassegrain C2 collects light from the sample and sends it upward through the remote aperture The light has an unobstructed path from C2 to the optical microscope Figure 5 Path of the Visible Beam for Viewing a Sample in Transmittance While viewing laser and infrared radia...

Page 38: ...e illuminator and directs it down through the cassegrain C2 M4 is a relay mirror that directs the beam down one side of cassegrain C2 to the sample Cassegrain C2 collects light from the sample and sends it upward through the remote aperture While viewing laser and infrared radiation are blocked from reaching the sample Figure 6 Path of the Visible Beam for Viewing a Sample in Reflectance ...

Page 39: ...itioned for collecting the infrared spectrum Similarly when you adjust the aperture so that the required area of the sample is isolated visually you have also isolated the area of the sample of which the spectrum is to be collected To collect a spectrum you use the View IR knob to move the detector mirror into the beam Figure 7 It blocks the beam from reaching the optical microscope and reflects i...

Page 40: ...ight from the illuminator mirror M3 receives the infrared beam from toroid M2 which is set to direct the beam downward The detector mirror is moved into the beam above the remote aperture The MCT cassegrain focuses the beam on to the MCT detector In transmittance mode the reflectance mirror M4 is completely removed from the beam Figure 7 Path of the Infrared Beam for Collecting a Spectrum in Trans...

Page 41: ...ceive light from the illuminator Instead the infrared beam from M2 is directed to M4 The beam is reflected off the sample and back through the other side of the cassegrain toward the remote aperture The detector mirror is moved into the beam above the remote aperture The MCT cassegrain focuses the beam on to the MCT detector Figure 8 Path of the Infrared Beam for Collecting a Spectrum in Reflectan...

Page 42: ...for cassegrain collection optics magnification 6 0 60 numerical aperture permanently aligned factory set focal separation The substage condenser cassegrain has a variable focusing control MCT detector cassegrain On axis design permanently aligned factory set focal separation Apertures provided Whole field aperture kit with variable independent knife edge aperture Illuminator Mounted in microscope ...

Page 43: ...m Microscope 43 Detector Choice of three 0 25 mm MCT detectors cooled by liquid nitrogen wide band medium band and narrow band spectral ranges Narrow Band 10 000 to 700 cm 1 Medium Band 10 000 to 580 cm 1 Wide Band 10 000 to 450 cm 1 ...

Page 44: ...44 MultiScope System Microscope User s Reference ...

Page 45: ...Getting Ready to Use the Microscope ...

Page 46: ...em Microscope It includes procedures for Setting up the FT IR for use with the microscope Cooling the MCT detector Viewing the sample Use these procedures at the beginning of the day s work or any time the microscope has not been in use or has been used by others At the end of the chapter is a list of continuing adjustments that you can make at any time that you are using the microscope ...

Page 47: ...ched off overnight To save time we suggest that you leave the FT IR switched on at all times 3 Select the external beam of the FT IR Spectrum 100 Series and Spectrum One Select the beampath to the microscope using the Beam tab of the Scan and Instrument Setup dialog Model 1600 Model 16PC Spectrum BX or Spectrum RX Move the external beam lever at the front lower left of the FT IR as far to the left...

Page 48: ...remely low temperature of liquid nitrogen can burn skin and eyes Avoid exposure by wearing heavy gloves and safety goggles whenever you work with it WARNING When liquid nitrogen warms to room temperature nitrogen gas vaporizes so rapidly that resulting pressures can send a funnel or detector cap suddenly and forcefully shooting upward from the top of the microscope WARNING Be sure to wait the spec...

Page 49: ...Funnel Inserted WARNING Stand where you can see the inside of the funnel as you pour the nitrogen in Pour slowly so that neither the funnel nor the dewar overflows If liquid nitrogen runs down the outside of the dewar it can damage the optics of the microscope 4 Carefully fill the funnel with liquid nitrogen Stand back and let the funnel empty completely The liquid nitrogen bubbles rapidly as it d...

Page 50: ...h time the funnel empties The funnel takes longer to empty as the dewar fills This happens after two to three more funnels of liquid nitrogen Because the dewar has now cooled the liquid nitrogen does not vaporize but instead fills the dewar 7 Remove the funnel and wait two minutes The liquid nitrogen settles down and bubbling slows 8 When the nitrogen stops bubbling refit the detector cap The fill...

Page 51: ...switch on the rear The Power On light at the front is lit 2 Make sure that the video camera power supply unit is connected to a mains electrical supply and the video camera is connected to the power supply unit 3 If you are using a monitor switch on the monitor if you are using a PC switch on the PC ...

Page 52: ...video display software enables you to View the sample on the PC screen in Windows Resize the visible image window Store visible images as bitmaps and in other file formats This enables you to archive visible images along with IR data Copy and paste visible images to other Windows packages The field of view of the microscope that is displayed on the PC has dimensions of 600 µm X axis and 400 µm Y a...

Page 53: ...Tutorial Using the Microscope ...

Page 54: ...ctra Getting Ready Before you begin this tutorial Switch on the FT IR and the microscope Switch on the power supply of the video camera Switch on the monitor if used Make sure that the software that controls the FT IR and the Win TV framegrabber software are open on the PC Select the external beam of the FT IR Fill the dewar of the MCT detector with liquid nitrogen Familiarize yourself with the po...

Page 55: ...llotape or Scotch tape The roller knife and forceps are included in the microscope sample preparation kit N187 0151 for more information contact your local PerkinElmer office or agent The sample holder is provided with the Microscope Preparing the flattened fiber sample 1 With forceps place the fiber on the microscope slide 2 Hold the fiber with the forceps and use the knife end of the roller knif...

Page 56: ...aperture in the retaining well 6 The aperture has blades and knife edges that are transparent to visible radiation but opaque to infrared 7 Looking at the visible image select a flat transparent portion of the fiber Adjust the knife edges until this portion fills the aperture Collecting the Background Spectrum You are ready to collect a background spectrum for this sample 1 Using only one of the s...

Page 57: ...yet 3 Adjust the gain to give maximum signal With the Spectrum 100 Series or Spectrum One the number must be as near as possible to but not more than 6000 With the Model 1600 or Spectrum RX the number must be as near as possible to but not more than 100 If the signal does not meet this requirement return to Ready For Next Command and use SETUP SCAN OTHERS GAIN to adjust the gain With the Model 16P...

Page 58: ...nob to View 2 Return the sample to the center of the field Do not change the size of the aperture 3 Switch the View IR knob to IR 4 Use the SCAN command to collect the spectrum of the sample collecting the same number of scans as you collected for the background 5 Remove the variable knife edge aperture and the sample from the microscope Figure 10 Spectrum of a Flattened Poly Ethylene Terephthalat...

Page 59: ... sample to use for these procedures is an aluminum soda drinks can The surfaces of such cans are coated with a polymer film Other equipment needed Scissors Reference mirror Preparing and positioning the sample 1 With scissors cut a piece about 7 mm square from the side of a soda drink can If it is noticeably curved flatten it WARNING Be careful The edges of the cut piece can be sharp ...

Page 60: ...ainted side up 4 Switch the View IR knob to View 5 Switch the Trans Refl knob to Refl 6 Looking at the visible image focus on the surface of the mirror with the Focus knob There are almost always dust particles or scratches on the surface that you can use to focus on 7 Move the stage in the x and y directions with the stage controls until the sample is in the center of the field of view 8 Focus on...

Page 61: ...e gain to give maximum signal see Transmittance Spectrum of a Flattened Fiber on page 54 NOTE If with the gain at its lowest setting the instrument reports overload or gain too high you must adjust the knife edges to make the aperture smaller 5 When the gain is correct collect a background spectrum 16 scans Collecting the Sample Spectrum 1 Switch the illuminator on again 2 Switch the View IR knob ...

Page 62: ...62 MultiScope System Microscope User s Reference Figure 12 Reflectance Spectrum of the Coating on a Soda Can ...

Page 63: ...Preparing Samples ...

Page 64: ...ugh to give an adequate signal otherwise the scan time must be increased Preparing a sample therefore often involves flattening it this both thins it and increases its area Flattening is accomplished by rolling squeezing or pressing the sample This chapter tells you how to prepare samples for spectroscopy with the microscope It includes A list of useful tools A list of window materials commonly us...

Page 65: ...microsampling toolkit Materials to have available Specialized accessories you may want to purchase Tools you can make yourself with procedures for making them Tools Provided with the Microscope The following items for use in sampling are provided supplied with the microscope Holder for 13 mm disks with gold mirror supports 13 mm disks on the sample stage and provides a reference mirror for reflect...

Page 66: ...Gold mirror in holder Reflection measurements Slides glass box Support samples for sample preparation Rotating 13 mm disk holder Supports samples and allows rotation Support for large samples Clips on to the sample stage Supports bulky samples so that the stage clip does not interfere with them KBr windows Support samples 100 µm aperture fixed size circular aperture Low magnification screen Viewin...

Page 67: ...er knife Cutting knife end and flattening roller end Steel tweezers Picking up extremely small objects Tungsten alloy needle Transferring particles Steel probe Pulling samples apart separating fibers Interchangeable handle for micro tools Handle for tungsten needle or steel probe Pin vise Holds needles for sharpening or for flattening samples Figure 13 Tools in the Microsampling Toolkit ...

Page 68: ...eps hooked 0990 8138 Wide tipped forceps flat 0990 8400 1 5 mm microdisk Fits in 13 mm disk holder to support very small samples 0186 1043 Fiber slit 18 µm L116 0581 Fiber slit 33 µm L116 0582 Pinhole 500 µm L116 0586 Pinhole 1000 µm L116 0587 Tool Part Number Microprobe with right angle bend N930 2606 Forceps round tips N930 2607 Forceps narrow needle points N930 2608 Windows All 13 mm diameter B...

Page 69: ...ools You Can Make Yourself This section gives procedures for making the following tools and equipment used in microspectroscopy Micropipettes used for transferring liquids Salt plates used as mounts for a wide variety of samples Tungsten needles used for transferring particles Microbrushes used in pyrolysis and in transferring minute amounts of liquid Micropipettes You can purchase micropipettes o...

Page 70: ... in the Microsampling Toolkit 3 Heat one end of the needle until it is red 4 Quickly insert the hot needle into the sodium nitrite 5 Wash the salt residue from the needle with water 6 For convenience sharpen the other end of the needle also so that you can reverse the needle in its mount when the first tip becomes damaged Microbrushes To make a microbrush for transferring small amounts of liquid o...

Page 71: ... it is hygroscopic so that the windows fog easily BaF2 Barium fluoride is not hygroscopic Its transmittance cut off is 750 cm 1 which means that it is best suited for use with a narrow band MCT detector although not with a wide band MCT 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 hygrosc...

Page 72: ...ective devices for flattening samples It is especially useful for flattening fibers or particles Different types of sample may be treated in different ways If the sample is soft roll it on a small salt window If the sample is hard roll it on a hard surface such as glass or metal A flat black cap from a jar makes a good surface for rolling a light colored sample If the sample is rolled on a small f...

Page 73: ...ture diamond anvil cell Compressing between infrared transmitting windows Pressing two windows together with the sample between them compresses the sample This also provides optical contact between the windows and the sample reducing surface scattering Windows made of NaCl or KBr are relatively soft If your sample is hard or if it is wet use BaF2 or ZnSe Pressing with the heel of a probe Press on ...

Page 74: ...edge from it with a razor blade Taper the wedge to as thin a slice as possible To cut a wedge shaped piece from a relatively thin sample 1 Place the sample between two offset glass slides Allow a triangular portion of the sample to protrude as shown on the left in Figure 14 Figure 14 Cutting a Wedge Shaped Sample 2 Run a razor blade or the roller knife along the edge of the upper slide The triangu...

Page 75: ...bedding material choose it carefully so that it does not alter the sample by reacting with it dissolving it or contaminating it Some commonly used materials are paraffin wax This is the preferred medium for infrared spectroscopy It produces few spectral interferences and it can usually be easily removed from the sample with warm xylene β pinene wax This material is similar to paraffin plastic embe...

Page 76: ...pty area of the cell you can completely compensate for the absorption bands of the diamonds To thin a sample in the miniature diamond anvil cell 1 Loosen and remove the three screws that hold the cell together 2 Lift off the top half of the cell and set it aside 3 Place the sample on the bottom half of the cell The sample must be small 4 Put the top half back on the cell lining up the red dots on ...

Page 77: ...ounts of quick setting nitrocellulose cement to the edges of the salt plates When the cement is dry the sample remains compressed The compression cell see Special Cells on page 81 is designed to compress this kind of sample Filled Polymers When a polymer contains a high concentration of fillers you have to prepare a sample for analysis that is free of filler Often you can obtain a suitable sample ...

Page 78: ...ll use a capillary tube instead of a disposable pipette for the above procedure Use a microbrush to pyrolyze micro amounts Seal the end that is away from the brush fibers and tap the sample particle into this end then heat it gently with a microtorch After pyrolysis break off and discard the end of the tube that contains the ash While holding the fibers of the brush against the salt plate add a dr...

Page 79: ...les under the microscope Transferring w ith a tungsten needle When necessary sharpen the tungsten needle as described in Tools You Can Make Yourself see page 69 Nujol or fluorolube mulls Suspending fine particles of a solid sample in nujol or fluorolube reduces or eliminates the surface reflections that can distort absorption measurements These oils also reduce the amount of radiation lost to refl...

Page 80: ...wo salt plates In the latter case the liquid flows between the plates by capillary action Preventing liquids from spreading If the amount of liquid being transferred to the salt plate is very small restrict it to a small area of the plate There are several ways to do this Use a microbrush to transfer solutions The bristles of the microbrush hold the liquid in a small region of the salt plate until...

Page 81: ...holder on the stage of the microscope 1 mm and 2 mm thick windows of 13 mm outer diameter can be used with the cell two KBr windows 2 mm thickness are included The cell can apply pressure without rotating the windows and therefore avoids scratching them Figure 16 The Compression Cell Although thinning can be accomplished with the compression cell it does not replace the miniature diamond anvil cel...

Page 82: ...up to 250 C in 1 degree increments A target temperature can be selected and maintained The hot stage is held in the slide clip on the sample stage of microscope The microscope requires no modifications to accept the hot stage Figure 17 The Hot Stage Applications of the hot stage include the study of phase transitions and temperature dependent chemical reactions Infrared microscopy can provide deta...

Page 83: ...Collecting Spectra with the Microscope ...

Page 84: ...ting a background spectrum Collecting the spectrum of the sample Also there are procedures that can be used in special situations When the spectrum of the sample must be collected before the background When the sample is too thick to fit on the stage in the usual arrangement These procedures assume that the microscope and the FT IR are ready to use Getting Ready to Use the Microscope on page 45 an...

Page 85: ...aining well 2 Place the sample on the sample stage If necessary secure it with the slide clip Figure 18 Parts of the Sample Stage 3 To set the microscope for viewing a sample turn the View IR knob to View The detector mirror moves out of the optical path and the illuminator is switched on 4 Set the Trans Refl knob to the required position for viewing 5 Turn the Illuminator knob to adjust the light...

Page 86: ...he sample in the y direction forward and back with the upper larger knob 7 Use the Focus knob on the left of the microscope Figure 19 to bring the sample into focus Figure 19 The Focus Knob 8 Look at the visible image as you use the stage control knobs to place the sample as required in the center of the field 9 Adjust the Focus knob again until the sample is in focus 10 Place the whole field aper...

Page 87: ...nife edge Reduce the size of the aperture until it just covers the area of interest in the sample The material of the aperture is transparent so that you can see the surrounding area of the sample This helps in positioning the sample correctly Move the sample out of the field of view using either the x or y stage controls You are now ready to collect a background spectrum for this sample ...

Page 88: ...stage give the x and y coordinates of the center Each scale has a vernier with 100 µm resolution If you note the location of the sample before you move it on the vernier scale you can re position it very near to the same location later 2 To select the type of spectrum to be collected transmittance or reflectance set the Trans Refl knob to Trans or to Refl as required Correcting the microscope for ...

Page 89: ...RS GAIN to adjust the gain With the Model 16PC or Spectrum BX the number must be as near as possible to but not more than 10000 If the signal does not meet this requirement display the Setup menu and choose Instrument then click Gain to increase the gain With the Spectrum GX the number must be as near as possible to but not more than 6000 If the signal does not meet this requirement display the Se...

Page 90: ...ries or Spectrum One display the Instrument menu and choose Scan Select the Scan tab and choose Scan type Background With the Model 1600 or Spectrum RX use SCAN BACKG With the Model 16PC or Spectrum BX display the Instrument menu and choose Scan Background With Spectrum GX display the Instrument menu and choose Scan Background ...

Page 91: ...st once again center the sample in the field visually The following instructions describe how to center the sample and collect its spectrum 1 Return the sample to the center of the field Do not change the size of the aperture 2 Switch the View IR knob to IR 3 Use the SCAN command of the FT IR to collect the spectrum of the sample ...

Page 92: ... to collect the sample spectrum first before you move the sample and collect the background spectrum This example shows how to perform the procedure in reflectance mode 1 With the sample under the microscope set the aperture 2 Collect a spectrum of the sample in single beam mode 3 Remove the sample without changing the aperture 4 Put the reference mirror on the sample stage 5 Still without changin...

Page 93: ...pectrum of a thick sample 1 Release the locking lever at the back of the lower cassegrain assembly on the right Figure 22 Figure 22 The Lower Cassegrain 2 Gently slide the cassegrain assembly forward and out of the dovetail connector NOTE To make withdrawal easier pull the locking lever gently 3 Turn the Correction knob to lower the dovetail connector to the bottom of its range of travel 4 Lower t...

Page 94: ...ge using the Focus knob 2 Turn the Correction knob to raise the dovetail connector 3 Make sure that the cassegrain is correctly seated 4 Slide the cassegrain assembly back into the dovetail connector as far as it goes NOTE To make withdrawal easier pull the locking lever gently 5 Tighten the locking lever ...

Page 95: ...Operating the Optional Equipment ...

Page 96: ...te any optional equipment that you purchased with the MultiScope System Microscope for example The Visible Polarizer option The Infrared Polarizer option The following options for sample preparation are described in Preparing Samples starting on page 63 The hot stage The compression cell The microsampling tool kit The miniature diamond anvil cell ...

Page 97: ... Light Polarization NOTE Conventionally the plane of the light is taken to be the plane of the continuously varying electric vector This is represented in the left hand side of Figure 23 If the light passes through a polarizer the polarizer allows 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 rep...

Page 98: ... the first polarizer oscillates in exactly the plane that is blocked by the second polarizer Figure 24 Polarizers Parallel top and Polarizers Crossed bottom Some materials are anisotropic or birefringent their refractive index depends on their orientation These materials can alter the polarization of light passing through them this is dependent on the wavelength of the transmitted light When you l...

Page 99: ...to determine its composition Rocks minerals and crystals Most crystals are characteristically birefringent and thus are ideally suited to this technique Various components of a mixture consisting of crystals such as an artificial sweetener pharmaceutical powder or an illicit substance can be viewed and then visibly separated by their relative size shape and birefringence The crystals that appear d...

Page 100: ...larization studies consists of two parts the polarizer Figure 25 and the analyzer Figure 26 The polarizer polarizes the incoming beam from the illuminator and the analyzer contains a polarizing element that can be rotated into any orientation Figure 25 The Polarizer Figure 26 The Analyzer ...

Page 101: ...the polarizer into the horizontal slot below the illuminator on the left of the microscope Figure 27 with the angled corner facing towards the front of the microscope so that it pushes in the ball bearing inside the slot Push the polarizer fully in until it stops Figure 27 Polarizer Position ...

Page 102: ...lyzer in with the wheel up and 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 28 Analyzer Position 3 When the polarizing element is in the beam rotate the wheel while observing the sample on the monitor ...

Page 103: ...radiation that is whether the electric vector is 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 nitrile groups tend to be oriented perpendicular to the axis If the spectrum is collected with the infrared radiation polarized perpendicular to the axis t...

Page 104: ...104 MultiScope System Microscope User s Reference Equipment The polarizer has a rotatable silver bromide element in an aluminum mount Figure 29 Figure 29 The Infrared Polarizer ...

Page 105: ... The metal cover is above the View IR knob 2 Slide the analyzer into the vertical slot on the sample holder that can be seen through this aperture NOTE The flat side of the analyzer must be towards the rear of the microscope and the wheel facing outwards Figure 30 Infrared Polarizer Position 3 Push the analyzer fully until it stops ...

Page 106: ...he polarizer element is extremely fragile Do not touch it with anything It cannot be washed dusted or blown upon by air If damaged it cannot be repaired When it is not in use protect it in the case supplied NOTE Both the scribed line and the uneven coloration are normal and do not affect the performance of the element ...

Page 107: ...et connector on the metal plate at the rear of the microscope The transfer optics housing connecting the FT IR to the microscope The lower purge gaiter under the lower cassegrain The purge bellows under the sample stage which enables you to move the stage up and down without breaking the seal The metal ring PTFE coated fitting with an O ring under the nose casing The transparent ring that goes aro...

Page 108: ...the path of the infrared beam and the sample area Purging the system 1 Make sure that all parts of the purge system as listed above are in place 2 Set up the microscope 3 Place the sample in position 4 Purge the system for 15 to 20 minutes at a rate of approximately 10 L min 1 5 Collect the background spectrum and the spectrum of the sample ...

Page 109: ...Applications ...

Page 110: ...erence Applications This chapter contains examples of several applications for which the MultiScope System Microscope is particularly useful Reflectance FT IR microscopy Polymers Textiles Criminalistics Biological materials Product contaminants ...

Page 111: ... angle of the microscope enables it to capture a large proportion of the diffusely reflected radiation and send it to the detector A problem often encountered when using the diffuse reflectance technique is that there is a large specular component in the reflected radiation Figure 33 shows three diffuse reflectance spectra of polymethyl methacrylate PMMA shavings In the top spectrum the shavings w...

Page 112: ...112 MultiScope System Microscope User s Reference Figure 33 Diffuse Reflectance Spectra of PMMA collected with the MultiScope System Microscope and a Spectrum RX with MCT detector ...

Page 113: ...e the absorbance spectrum from the specular reflectance spectrum This integration is performed by the KK command in the Model 1600 and Spectrum BX software and the Spectrum software Figure 34 shows the specular reflectance spectrum of a PMMA plate and the absorption spectrum computed from it with the KK command Collected with an MultiScope System Microscope and a Spectrum RX with MCT detector The ...

Page 114: ...ly a metal and is then reflected back through the film Figure 32 The absorbance spectrum of the film can be collected directly Figure 35 shows the spectrum of residual oil on an electronic contact The sample diameter was 100 µm Figure 35 Reflection Absorption Spectrum of Residual Oil on an Electronic Contact Collected with an MultiScope System Microscope and a Spectrum RX with a medium band MCT de...

Page 115: ...nt that is of interest isolate it with the variable knife edge aperture and collect its spectrum For example Figure 36 shows spectra of the three layers of a laminated food packaging material Figure 36 Cross Sectional Analysis of a Laminated Food Packaging Material Top 200 µm layer of poly propylene Middle 15 µm layer of poly vinylidine chloride Bottom 10 µm layer of poly ethylene vinyl acetate Co...

Page 116: ...nt areas on fabrics or to study single fibers Figure 37 is the transmittance spectrum of a flattened 20 µm poly hexamethylene adipamide fiber Figure 37 Transmittance Spectrum of a Flattened 20 µm Poly Hexamethylene Adipamide Fiber Collected in a single scan with an MultiScope System Microscope and a Spectrum RX with a narrow band MCT detector ...

Page 117: ...aint chips and traces of drugs or explosives Figure 38 is the spectrum of a flattened paint chip from a green 1979 automobile The spectrum indicates that the chip was a modified acrylic Figure 38 Transmittance Spectrum of a Flattened Paint Chip Collected with an MultiScope System Microscope and a Spectrum RX with an MCT detector ...

Page 118: ...m which the absorbance spectrum was calculated with the Kramers Kronig integration The protein band at 1650 cm 1 is from blood the apatite band at 1030 cm 1 is from the tooth enamel Figure 39 Top Reflectance Spectrum of an Extracted Decayed Human Tooth Bottom Absorbance Spectrum Calculated with the KramersKronig Integration Obtained with an MultiScope System Microscope and a Spectrum RX with a med...

Page 119: ...r of a black paper product found it was contaminated with white spots One of the spots was picked from the paper with a probe and placed under the microscope The spectrum in Figure 40 was collected The contaminant was identified as a mixture of glass SiO2 and wax ester of a fatty acid Figure 40 White Spot of Contaminant from the Surface of Black Paper Collected with an MultiScope System Microscope...

Page 120: ... be found in uncontaminated paper The difference between the two spectra bottom spectrum corresponded to carbonate anion CO3 2 the contaminant was probably either MgCO3 or CaCO3 Figure 41 Identifying a Contaminant Top Spectrum of Contaminated Paper Middle Spectrum of Cellulose Fiber Bottom Difference Spectrum Obtained by Subtracting the two Collected with an MultiScope System Microscope and a Spec...

Page 121: ...opier Toner Collected with an MultiScope System Microscope and a Spectrum RX with a narrow band MCT detector Figure 42 shows the spectrum of a spot of photocopier toner which is often encountered as an office or laboratory contaminant ...

Page 122: ...122 MultiScope System Microscope User s Reference ...

Page 123: ...Maintenance ...

Page 124: ...tions Service At the end of the chapter is a list of the available spare parts and optional equipment for the microscope If you need to replace a part only use PerkinElmer approved spare parts NOTE PerkinElmer FT IRs contain diagnostic software If you use the diagnostics with the microscope be aware that it is impossible to fulfill the requirement to clear the beam This is because the microscope i...

Page 125: ...as possible Dust fingerprints and smears on the optics reduce the quality of the images it produces Whenever the microscope is not in use cover it with a plastic cover CAUTION Ensure the power is switched off when the Microscope is covered Cleaning the Optics The microscope was aligned cleaned and sealed at the factory Do not attempt to take it apart If dust settles on the cassegrain mirrors and o...

Page 126: ...atch test on an inconspicuous area of the microscope before you clean the entire instrument Avoid spilling liquid into the microscope Clean all external spills immediately If anything that is spilled enters the main body of the microscope switch off the power and call a PerkinElmer Service Engineer CAUTION Ensure the power is switched off and the supply lead is disconnected before cleaning the cov...

Page 127: ... from the power supply 2 Insert a screwdriver into the slot at the side of the fuse drawer and remove the fuse drawer from the rear panel 3 Pull back the central black prong on the side of the fuse drawer and remove the fuse tray The fuse tray contains two fuses one for use with a 100 V to 120 V power supply and one for use with a 200 V to 240 V power supply 4 Fit the replacement fuse into the fus...

Page 128: ...n will become accessible if the MCT detector is removed If the MCT detector is to be removed from a Spectrum BX or Model 1600 first block off the laser radiation by selecting the FT IR s internal beam path 1 Switch off the microscope and disconnect the mains supply 2 Remove the two screws that secure the microscope top cover one is on the right at the rear and the other at the front underneath the...

Page 129: ...etaining well and set an aperture size of approximately 100 x 100 µm 7 Use the Monitor command to display an energy bar on the FT IR screen 8 Turn the Correction knob at the base of the microscope until the energy bar is at a maximum 9 The MCT dewar is supported by three screws in the top plate of its frame Figure 43 Make sure that the screws in the front two corners rest in the depressions provid...

Page 130: ...ions 4 and 5 of terminal block PL1 remove the connectors The terminal block PL1 is at the top of the power supply board at the back of the microscope next to the mains inlet unit 4 Remove the two screws holding the lamp baffle which surrounds the lamp and lift it off the lamp 5 Loosen the screw holding the lamp retaining bracket to the illuminator tube fixed cylinder and lift off the lamp retainin...

Page 131: ...ws connecting the lamp leads are tight Failure to do this may result in overheating and damage to the microscope 11 Refit the lamp baffle over the lamp refit the screws 12 Re connect the lamp leads to terminals 4 and 5 of terminal block PL 1 13 Refit the top cover and retaining screws The microscope is now ready for use ...

Page 132: ... Plug Pin Wire Color 100 110 120 V Wire Color 220 230 240 V Ground Earth Green or Green Yellow Green Yellow Line Black Brown Neutral White Blue WARNING To ensure safe and satisfactory operation of the microscope it is essential that the green or green yellow ground earth wire of the power cord is connected to a ground that complies with the regulations of the local electricity supply authority or ...

Page 133: ...pply The microscope operates on an electrical supply with a frequency of 50 or 60 Hz and at voltages in the ranges 100 to 120 V or 220 to 240 V Fit the molded connector of the power cable into the inlet at the rear of the microscope Figure 44 Location of the Electrical Supply inlet ...

Page 134: ... from the preamp inside the microscope to a connector marked on the rear of the FT IR Figure 45 MultiScope System Microscope Connected to the Spectrometer The following table shows all of the connections from the pre amp in the microscope to the spectrometer Pl 1 PCB D type Connector Line Power Requirement 1 11 Output signal 2 10 Output signal 0 V 3 9 0 V 4 12 0 V 5 13 12 V 250 mA 6 14 12 V 200 mA...

Page 135: ...um BX The cable from the microscope to the Spectrum BX comes from the preamp inside the microscope through a slot at the rear of the Spectrum BX to a connector inside the FT IR at the rear left hand side Figure 46 The MultiScope System Microscope Connected to a Spectrum BX ...

Page 136: ...l of the connections from the pre amp in the microscope to a Spectrum BX Paragon Pl 1 PCB CONN IDC SKT 15 way Line Power Requirement 1 11 Output signal 2 10 Output signal 0 V 3 9 0 V 4 12 0 V 5 13 12 V 250 mA 6 14 12 V 200 mA 8 12 A1 gain selection 5 V 9 11 A0 gain selection 5 V ...

Page 137: ...cope to a Spectrum GX The cable from the microscope to the Spectrum GX comes from the preamp inside the microscope to an unlabelled 25 way connector on the lower right hand side of the FT IR Figure 47 MultiScope System Microscope Connected to a Spectrum GX ...

Page 138: ...the pre amp in the microscope to a Spectrum GX J1 1 PCB 25 way D type 25 way D type Line Power Requirement 1 1 15 V 150 mA 2 2 15 V 3 3 0 4 4 S2 5 5 S4 6 6 0 7 7 15 V 150 mA 8 8 15 V 9 9 OCBRES 10 10 M0 11 11 M1 12 12 SO 13 13 Output signal 14 14 SK 15 15 0vl 16 16 0vl 17 17 5 V 150 mA 18 18 5 V 21 21 OSX ...

Page 139: ... compensate for wear We recommend that the microscope is cleaned examined and adjusted periodically by a PerkinElmer Service Engineer NOTE If you experience unexpected problems with the microscope contact your PerkinElmer office or representative immediately Care for your video camera as described in the manufacturer s manuals ...

Page 140: ...tment is 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 f...

Page 141: ...ection knob 89 Crushing 78 D Detector 33 43 128 Dewar 49 E Elastomers 77 Electrical connections 132 Electrical safety 19 Epoxy resins 75 F Fibers 55 99 bicomponent 99 Fibrous solids 79 Film thin 59 FT IR 32 setting up 47 Fuse 29 I Illuminator 34 42 Inert atmosphere 107 L Labels warning signs 12 Laminates 99 Lamp changing 130 Laser apertures 25 radiation hazard 24 warning labels 25 Lifting the micr...

Page 142: ...preparation 64 thick 93 thickness 64 wedge 74 Separating by aperturing 79 Service 139 Signal to noise ratio 33 Specifications 42 Spectrum collecting 39 58 84 91 collecting sample first 92 T Temperature dependence 82 Thick sample 93 Tools disk holder 65 fiber slit 68 for sample preparation 65 forceps 67 68 interchangeable handle 67 microbrush 80 microdisk 68 micropipette 69 80 microprobe 68 needle ...

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