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Perkin-Elmer MultiScope System User Reference

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Summary of Contents for Perkin-Elmer MultiScope System

  • Page 1 MultiScope System Microscope User's Reference...
  • Page 2 Release History Part Number Release Publication Date L1050041 December 2013 Any comments about the documentation for this product should be addressed to: User Assistance PerkinElmer Ltd Chalfont Road Seer Green Beaconsfield Bucks HP9 2FX United Kingdom Or emailed to: info@perkinelmer.com Notices The information contained in this document is subject to change without notice.

  • Page 3: Table Of Contents

    Warning Label Near the Lamp Housing ............ 26 Lifting the Microscope ................27 EMC Compliance ..................28 System Requirements ................29 Overview of the MultiScope System Microscope ....... 31 Features of the MultiScope System Microscope ......... 32 Applications ................... 35 The Optical System ................36 Specifications ..................
  • Page 4 Collecting Spectra with the Microscope ..........83 Collecting Spectra with the Microscope ............. 84 Positioning the Sample ................85 Collecting a Background Spectrum ............88 Collecting the Spectrum of the Sample ............. 91 If You Must Collect the Sample Spectrum First .......... 92 Collecting the Spectrum of a Thick Sample ..........

  • Page 5: Introduction

    I ntroduction...

  • Page 6: Introduction To This Guide

    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 for collecting spectra with the microscope.

  • Page 7: Related Documents

    Introduction . 7 R elated Docum ents M anuals for P erkinElm er FT-I Rs Information on using your FT-IR is found in the manuals that were supplied with it. Optional equipm ent Certain items of the optional equipment for the microscope have their own manuals.

  • Page 8: What Am I Expected To Know

    8 . MultiScope System Microscope User's Reference W hat am I Ex pected to Know ? We assume that you have some familiarity with operating the FT-IR. Specifically, you must be able to: Set the FT-IR to use the external beam;...

  • Page 9: Conventions Used In This Manual

    Introduction . 9 Conventions Used in this M anual Normal text is used to provide information and instructions. Bold text refers to text that is displayed on the screen. UPPERCASE text, for example ENTER or ALT, refers to keys on the PC keyboard. '+' is used to show that you have to press two keys at the same time, for example, ALT+F.
  • Page 10 10 . MultiScope System Microscope User's Reference We use the term CAUTION to inform you about situations that could result in serious dam age to the instrum ent or other CAUTION equipment. Details about these circumstances are in a box like this one.
  • Page 11 Introduction . 11 We use the term WARNING to inform you about situations that could result in personal injury to yourself or other persons. Details about these circumstances are in a box like this one. WARNING W arning (W arnung) Bedeutet, daß...

  • Page 12: Warning Signs On The Instrument

    12 . MultiScope System Microscope User's Reference W arning Signs on the I nstrum ent 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 Spectrum One The MultiScope System Microscope can be used with Spectrum One spectrometers. Spectrum GX The MultiScope System Microscope can be used with Spectrum GX, System 2000, Spectrum 2000, System 2000R NIR FT-Raman, Spectrum 2000R NIR FT-Raman User's Reference FT-IR, and Spectrum GXR FT-IRs. In this...
  • Page 14 14 . MultiScope System Microscope User's Reference...

  • Page 15: Warnings And Safety Information

    W arnings and Safety I nform ation...

  • Page 16: Summary

    DO NOT use a flammable gas to purge the MultiScope System Microscope. The microscope contains a hot lamp, and fire or explosion may result. Use only clean, dry oil-free nitrogen or air to purge the instrument.

  • Page 17: General Operating Conditions

    Warnings and Safety Information General Operating Conditions The MultiScope System Microscope has been designed and tested in accordance with PerkinElmer specifications and in accordance with the safety requirements of the International Electrotechnical Commission (IEC). The MultiScope System Microscope conforms to IEC 61010-1 (Safety requirements for electrical equipment for measurement, control, and laboratory use) as it applies to IEC Class 1 (earthed) appliances and therefore meets the requirements of EC Directive 2006/95/EC.

  • Page 18: Environmental Conditions

    18 . MultiScope System Microscope User's Reference Environm ental Conditions The microscope has been designed to be safe under the following conditions: Indoor use; • • Altitude up to 2000 m; Ambient temperatures of 5 °C to 40 °C; •...

  • Page 19: Electrical Safety

    Warnings and Safety Information Electrical Safety Connect the MultiScope System Microscope to a power supply line that includes a switch or other adequate means of disconnection from the electricity supply. Plug the microscope only into an electricity-supply socket that is provided with a protective ground (earth) connection.
  • Page 20 20 . MultiScope System Microscope User's Reference The MultiScope System Microscope has: An IEC Pollution Degree 2 classification - usually only non-conductive • atmospheric pollution of the equipment occurs; occasionally, however, a temporary conductivity caused by condensation must be expected.

  • Page 21: Location And Ventilation

    Warnings and Safety Information Location and Ventilation The microscope is installed by a PerkinElmer Service Representative, who will be able to advise on the siting of the system. To allow for adequate cooling, the system should not be sited near to room heating equipment, for example, central- heating radiators.

  • Page 22: Laser Safety Regulations

    22 . MultiScope System Microscope User'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 Warnings and Safety Information Laser P roduct Classification The MultiScope System Microscope is not a laser product because it does not contain a laser system. However, the microscope forms part of a laser product when it is assembled to an FT-IR spectrometer (which does contain a laser system).

  • Page 24: Laser Labels And Laser Apertures

    24 . MultiScope System Microscope User's Reference Laser Labels and Laser Apertures This manual contains information and warnings that you must follow to make sure that you use the microscope safely. Warning labels are fixed to the microscope in the locations shown 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.
  • Page 25 Warnings and Safety Information Figure 2 Position of laser radiation warning labels and laser apertures To maintain compliance with laser safety regulations, at least once a year, or whenever the unit has been subjected to adverse 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.

  • Page 26: Warning Label Near The Lamp Housing

    26 . MultiScope System Microscope User's Reference W arning Label Near the Lam p Housing Caution, hot surface.

  • Page 27: Lifting The Microscope

    Warnings and Safety Information Lifting the M icroscope The MultiScope System Microscope weighs approximately 27.5 kg (approximately 33 kg with packaging). Lift the microscope only by the base. Do not attempt to lift it by the knobs, cassegrain assembly or other attachments.

  • Page 28: Emc Compliance

    EM C Com pliance EC Directive The MultiScope System Microscope has been designed and tested to meet the requirements of the EMC Directive 2004/108/EC. The microscope complies with 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.

  • Page 29: System Requirements

    Warnings and Safety Information System R equirem ents Give attention to the following points before installing the MultiScope System Microscope. Electrical R equirem ents The power consumption of the microscope does not exceed 80 VA. The line supply must be within 10% of the nominal voltage.
  • Page 30 30 . MultiScope System Microscope User's Reference Site R equirem ents Minimum bench dimensions of 55 x 36 cm to accommodate the microscope. To get the best performance from your microscope: Place the microscope in an environment that is relatively dust-free.

  • Page 31: Overview Of The Multiscope System Microscope

    Overview of the M ultiScope System M icroscope...

  • Page 32: Features Of The Multiscope System Microscope

    The PerkinElmer MultiScope 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.
  • Page 33 The MultiScope System Microscope (Figure 4) includes the following features: • High-performance PerkinElmer collection optics for infrared microspectroscopy. The cassegrain mirror systems used in the MultiScope System Microscope have a wide collection angle (high numerical aperture) for efficient collection of radiation.
  • Page 34 34 . MultiScope System Microscope User's Reference Larger working distance for thick samples. The lower cassegrain can be • removed to provide space for thick samples to be studied in reflectance. Spectra can be collected in either reflectance or transmittance modes.

  • Page 35: Applications

    Overview of the MultiScope System Microscope Applications Because the microscope enables you to collect spectra of very small samples, and can collect both reflectance and transmittance spectra, it is useful in a wide variety of applications. Some examples are listed below, and several of these are described...

  • Page 36: The Optical System

    36 . MultiScope System Microscope User's Reference The Optical System The MultiScope System Microscope combines two optical systems: PerkinElmer optics for infrared microspectroscopy and a video viewer. The two systems intersect at the remote aperture (Figure 5). When a sample on the sample stage is in focus, its conjugate image is focused at the remote aperture.
  • Page 37 Overview of the MultiScope System Microscope View ing in transm ittance When the microscope is set for viewing in transmittance (Figure 5): Mirror M3, beneath the cassegrains, receives light from the illuminator and • directs it up through cassegrain C1.
  • Page 38 38 . MultiScope System Microscope User's Reference View ing in reflectance When the microscope is set for viewing in reflectance (Figure 6): Mirror M4, above the cassegrain, receives light from the 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.
  • Page 39 Overview of the MultiScope System Microscope Collecting a Spectrum The same cassegrain is used for both visible light and infrared radiation. For this reason, when you adjust the sample position so that the visible image of the sample is in focus, the sample is also correctly positioned for collecting the infrared spectrum.
  • Page 40 40 . MultiScope System Microscope User's Reference Collecting a spectrum in transm ittance Collecting a spectrum in transmittance differs from viewing in transmittance as follows (Figure 7): • Instead of receiving light from the illuminator, mirror M3 receives the infrared beam from toroid M2, which is set to direct the beam downward.
  • Page 41 Overview of the MultiScope System Microscope Collecting a Spectrum in Reflectance Collecting a spectrum in reflectance differs from viewing in reflectance as follows (Figure 8): • The sample does not receive light from the illuminator. Instead, the infrared beam from M2 is directed to M4.

  • Page 42: Specifications

    42 . MultiScope System Microscope User's Reference Specifications Sam ple stage Manual stage: Range of travel = 75 mm × 50 mm Working distance: 25 mm Working distance for thick samples: 30 mm (with lower cassegrain removed) The manual stage is equipped with a sample clip and is calibrated in 1 mm increments.
  • Page 43 Overview of the MultiScope System Microscope 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 Medium Band 10 000 to 580 cm...
  • Page 44 44 . MultiScope System Microscope User's Reference...

  • Page 45: Getting Ready To Use The Microscope

    Getting Ready to Use the M icroscope...

  • Page 46: Getting Ready To Use The Microscope

    46 . MultiScope System Microscope User's Reference Getting R eady to Use the M icroscope This chapter gives the routine procedures for getting ready to collect spectra with the MultiScope System Microscope. It includes procedures for: Setting up the FT-IR for use with the microscope; •...

  • Page 47: Setting Up The Ft-Ir

    Getting Ready to Use the Microscope . 47 Setting Up the FT-I R 1. If necessary switch on the FT-IR. 2. Leave the source to warm up as directed in the manual for the FT-IR. The power supply to the detector of the microscope is also switched on through the FT-IR.

  • Page 48: Cooling The Mct Detector

    48 . MultiScope System Microscope User's Reference Cooling the M CT Detector An MCT (Mercury Cadmium Telluride) detector is standard in the MultiScope System Microscope. The MCT detector must be cooled to 77 K before you can operate it. It is mounted in a dewar that can be filled with liquid nitrogen.
  • Page 49 Getting Ready to Use the Microscope . 49 Cooling the M CT detector 1. Press on the front edge of the lid of the dewar, which then opens. 2. Lift off the cap of the dewar. 3. Place the small funnel supplied with the microscope in the opening in the red detector dewar (Figure 9).
  • Page 50 50 . MultiScope System Microscope User's Reference 5. 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 settle down and the pressure of the vaporizing nitrogen to dissipate.

  • Page 51: Setting Up The Microscope

    Getting Ready to Use the Microscope . 51 Setting Up the M icroscope 1. Switch on the microscope at the 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.

  • Page 52: Viewing The Sample

    52 . MultiScope System Microscope User's Reference View ing the Sam ple You can view the visible image of a sample in a window on a PC screen by using the video viewer, which comprises a video camera that is linked to a framegrabber board in the PC.

  • Page 53: Tutorial: Using The Microscope

    Tutorial: Using the M icroscope...

  • Page 54: Introduction To The Tutorial

    54 . MultiScope System Microscope User's Reference I ntroduction to the Tutorial This tutorial describes how to prepare two frequently-studied types of samples (fibers and thin films) and collect their spectra. In this tutorial you will: Learn some techniques for preparing samples;...

  • Page 55: Transmittance Spectrum Of A Flattened Fiber

    Tutorial: Using the Microscope . 55 Transm ittance Spectrum of a Flattened Fiber In this section you prepare a flattened fiber sample and collect its transmittance spectrum. You can use any convenient organic fiber as the sample in these procedures, provided it is small enough in diameter to give a transmittance spectrum.
  • Page 56 56 . MultiScope System Microscope User's Reference P osition and focusing the sam ple 1. Set the microscope for viewing a sample in transmitted light: switch the Trans/Refl knob to Trans and the View/IR knob to View. 2. To position the sample stage correctly, look from the front with your naked eye and adjust the stage in the x and y directions until you see light striking the sample.
  • Page 57 Tutorial: Using the Microscope . 57 Correcting the m icroscope for focal shifts sample When the for a transmittance spectrum is mounted on a window of KBr (or another substance), you must correct the microscope optics for focal shifts that occur as the infrared beam comes through the window.
  • Page 58 58 . MultiScope System Microscope User's Reference Collecting the Sam ple Spectrum Before you can collect the sample spectrum, you must once again center the sample in the field visually. 1. Switch the View/IR knob to View. 2. Return the sample to the center of the field. Do not change the size of the aperture.

  • Page 59: Reflectance Spectrum Of A Thin Film

    Tutorial: Using the Microscope . 59 R eflectance Spectrum of a Thin Film Now you are going to collect the reflectance spectrum of a thin polymer coating on a reflective surface. A convenient sample to use for these procedures is an aluminum soda (drinks) can.
  • Page 60 60 . MultiScope System Microscope User's Reference 2. Place the 3 x 1 sample holder on the sample stage of the microscope, reflective side up, as in Figure 11. Figure 11 Reference Mirror on the Sample Stage 3. With forceps, set the sample over one of the unused holes on the 3 x 1 sample stage, outer (painted) side up.
  • Page 61 Tutorial: Using the Microscope . 61 Because the sample is large and has uniform areas, you do not need to use it all or to isolate the best portion; just adjust the knife edges to give a convenient aperture size (50 µm). 1.
  • Page 62 62 . MultiScope System Microscope User's Reference Figure 12 Reflectance Spectrum of the Coating on a Soda Can...

  • Page 63: Preparing Samples

    P reparing Sam ples...

  • Page 64: Preparing Samples

    64 . MultiScope System Microscope User's Reference P reparing Sam ples Using a microscope for infrared spectroscopy can simplify sample preparation, because you can examine the sample visually and select the best part to use. Proper sample preparation is still important, however, if you are to collect good quality spectra.

  • Page 65: Tools For Sample Preparation

    Sample Preparation Tools for Sam ple P reparation This section lists the tools you need for preparing samples: Sampling accessories provided with the microscope; • • Sampling accessories available as options; Tools in the microsampling toolkit; • Materials to have available; •...

  • Page 66: Sampling Accessories Available As Options

    66 . MultiScope System Microscope User's Reference Sam pling Accessories Available as Options The following items for use in sampling are available in accessories kit, part number L186 0250: Item Holder for 13 mm disks Supports 13 mm disks on the sample...
  • Page 67 Sample Preparation The following tools are in the sample preparation kit for infrared microscopy N187 0151, see Figure 13. Tool Forceps, 4½ inch, Cd plated Picking up small objects Cutting (knife end) and flattening Roller knife (roller end) Steel tweezers Picking up extremely small objects Tungsten alloy needle Transferring particles...
  • Page 68 68 . MultiScope System Microscope User's Reference Other Useful Tools Depending on the type of samples that you usually work with, it may be helpful to have some of the following tools: Tool Part Number Wide-tipped forceps, hooked 0990 8138...
  • Page 69 Sample Preparation Specialized Accessories The following accessories are extremely useful in preparing certain types of Techniques for Preparing Samples samples (as described in , on page 72): Miniature Diamond Anvil Cell (N930 2618) • • Microtome I tem s to Have Available In addition to the items provided with the microscope, we recommend that you have the following available: •...
  • Page 70 70 . MultiScope System Microscope User's Reference Tungsten N eedles You can make tungsten needles by sharpening 24 to 26 gauge (0.5 mm) tungsten wire. This is done chemically, by etching the wire with sodium nitrite (or ammonium nitrite) to produce a smooth, fine, stiff-pointed needle.

  • Page 71: Common Window Materials

    Sample Preparation Com m on W indow M aterials Both liquid and solid samples are often mounted on salt windows. Very thin windows, 1 to 2 mm thick, give the best spectra. The following materials are commonly used in windows: KBr: Potassium bromide is inexpensive, and it transmits infrared radiation to •...

  • Page 72: Techniques For Preparing Samples

    72 . MultiScope System Microscope User's Reference Techniques for Preparing Sam ples This section describes some useful techniques for preparing various types of samples. Flattening Solids Samples that are too thick to give good infrared spectra can often be flattened by pressing or squeezing.
  • Page 73 Sample Preparation Squeezing w ith a pellet press Samples can be squeezed between the polished anvils of a KBr pellet press without KBr. To collect the spectrum use either of the following methods: • Peel the flattened sample off the anvil with a probe or knife and place it on a sample mount.
  • Page 74 74 . MultiScope System Microscope User's Reference Slicing Sam ples from Solids Cutting a w edge of sam ple If a solid sample is too thick to give good spectra, cutting a wedge-shaped piece from its edge produces a thin sample while destroying very little of the original.
  • Page 75 Sample Preparation M icrotom ing A microtome is a device for slicing a sample into thin cross-sections, 0.5 to 20 µm thick. It is commonly used to prepare samples for light microscopy; the same range of thicknesses is also appropriate for infrared microscopy. If you are trying to identify the individual components of a laminate, microtomed samples give the best results.
  • Page 76 76 . MultiScope System Microscope User's Reference P olym ers Diam ond anvil cell Polymer samples such as paint chips, thick films, elastomers, or fibers can be pressed or squeezed to reduce their pathlength. A convenient device for pressing polymers (or other compressible samples) is the miniature diamond anvil cell, shown in Figure 15.
  • Page 77 Sample Preparation Figure 15 The Miniature Diamond Anvil Cell P ressing elastom ers betw een w indow s If your sample is elastic and you are compressing it between windows, you need a way to apply pressure continuously. Use the following procedure: 1.
  • Page 78 78 . MultiScope System Microscope User's Reference Pyrolysis can be used to remove the fillers. As you heat the sample, the polymer volatilizes, and the fillers are reduced to ash. The pyrolysis can be accomplished in any of the following ways: Place the polymer in a disposable pipette and seal the large end.
  • Page 79 Sample Preparation Separating by aperturing Powders and other particulate solids may contain several different components. Instead of separating them, use the variable knife-edge aperture to isolate the component you want to sample: 1. Spread the sample out with a probe so that you can visually distinguish the components.
  • Page 80 80 . MultiScope System Microscope User's Reference Coatings on Substrates If the sample is coated on a substrate, the method for collecting its spectrum depends on the nature of the substrate: • If the substrate is reflective, you can analyze the sample in reflectance.

  • Page 81: Special Cells

    Sample Preparation Special Cells Polymers For discussion of the diamond anvil cell, see on page 76. Com pression Cell The compression cell (N187 0185, Figure 16) is a device for flattening soft materials and holding specimens flat and in optical contact with salt windows. The cell consists of an aluminum block, machined to accept salt windows, with window retainers and a special wrench to apply pressure across the windows.
  • Page 82 82 . MultiScope System Microscope User's Reference Hot Stage The hot stage for the MultiScope System Microscope (N187 0184, Figure 17) is used to study temperature-dependent phenomena in microsamples. The hot stage consists of a temperature controller and a heating block that accepts infrared windows.

  • Page 83: Collecting Spectra With The Microscope

    Collecting Spectra w ith the M icroscope...

  • Page 84: Collecting Spectra With The Microscope

    84 . MultiScope System Microscope User's Reference Collecting Spectra w ith the M icroscope Usually, the MultiScope System Microscope is used for collecting the spectra of microscopic samples. This chapter contains the necessary procedures for: Positioning the sample correctly on the sample stage;...

  • Page 85: Positioning The Sample

    Collecting Spectra with the Microscope P ositioning the Sam ple 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.
  • Page 86 86 . MultiScope System Microscope User's Reference 6. Looking from the front, adjust the stage in the x and y directions with the stage controls (under the stage on the right, Figure 18) until the sample is illuminated. Move the sample in the x direction (left and right) with the lower, smaller •...
  • Page 87 Collecting Spectra with the Microscope Figure 20 Inserting the Variable Knife-edge Aperture in the Retaining Well 11. Look at the visible image as you turn each of the four knobs of the knife-edge. Reduce the size of the aperture until it just covers the area of interest in the sample.

  • Page 88: Collecting A Background Spectrum

    88 . MultiScope System Microscope User's Reference Collecting a Background Spectrum We recommend that you collect a new background spectrum for each sample, because the aperture size and FT-IR settings can vary from sample to sample. Collect the background spectrum using the same conditions that you used to collect the sample spectrum.
  • Page 89 Collecting Spectra with the Microscope 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 •...
  • Page 90 90 . MultiScope System Microscope User's Reference 5. When the gain is set, collect a background spectrum: With the Spectrum 100 Series or Spectrum One, display the Instrument • menu and choose Scan. Select the Scan tab and choose Scan type: Background.

  • Page 91: Collecting The Spectrum Of The Sample

    Collecting Spectra with the Microscope Collecting the Spectrum of the Sam ple Before you can collect the sample spectrum, you must once again center the sample in the field visually. The following instructions describe how to center the sample and collect its spectrum. 1.

  • Page 92: If You Must Collect The Sample Spectrum First

    92 . MultiScope System Microscope User's Reference I f You M ust Collect the Sam ple Spectrum First To collect the background spectrum with the same aperture as the sample spectrum, you usually set the aperture with the sample in place, move the sample before you collect the background spectrum, and finally return the sample and collect its spectrum.

  • Page 93: Collecting The Spectrum Of A Thick Sample

    Collecting Spectra with the Microscope Collecting the Spectrum of a Thick Sam ple You can lower the stage in order to focus on a thick sample. For very thick samples, this requires the removal of the lower cassegrain assembly and then the reflectance method can be used to view the sample and collect its spectrum.
  • Page 94 94 . MultiScope System Microscope User's Reference To refit the low er cassegrain after use 1. Raise the stage using the Focus knob. 2. Turn the Correction knob to raise the dovetail connector. 3. Make sure that the cassegrain is correctly seated.

  • Page 95: Operating The Optional Equipment

    Operating the Optional Equipm ent...

  • Page 96: Operating The Optional Equipment

    96 . MultiScope System Microscope User's Reference Operating the Optional Equipm ent This chapter contains the special instructions you need to operate any optional equipment that you purchased with the MultiScope System Microscope, for example: The Visible Polarizer option; •...

  • Page 97: Visible Polarizer Option

    Operating the Optional Equipment Visible P olarizer Option This section describes how polarization of visible light can be useful in identifying areas or structures that differ chemically, and how this technique can be used in solving problems commonly found in infrared microspectroscopy applications. Ordinary light and infrared radiation consists of waves vibrating in all possible planes perpendicular to the direction of propagation.
  • Page 98 98 . MultiScope System Microscope User's Reference If a second polarizer is placed in the path of the polarized light two things may result: If the second polarizer is placed in the same direction as the first (as at the •...
  • Page 99 Operating the Optional Equipment Applications Differences in the birefringence of an object or area may be an indication of chemical disparity. This can be useful in visibly separating or identifying an object or area of interest before collecting an infrared spectrum. Some examples are given below: Lam inates Many polymer structures consist of different layers of material and adhesives of...
  • Page 100 100 . MultiScope System Microscope User's Reference Equipm ent The equipment for visible polarization 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.
  • Page 101 Operating the Optional Equipment Operation To use the analyzer and polarizer: 1. Insert 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.
  • Page 102 102 . MultiScope System Microscope User's Reference 2. Insert the analyzer into the slot under the video camera (Figure 28). Push the analyzer in with the wheel up and facing towards you. It has two positions: The first position allows the full beam to pass through.

  • Page 103: Infrared Polarizer Option

    Operating the Optional Equipment I nfrared P olarizer Option An absorption band in the infrared range occurs when a vibration is accompanied by a change in dipole moment. The electric vector of the incident radiation must have a component in the direction of the dipole moment change. In polarization spectroscopy, the absorption bands of greatest interest are those in which the direction of dipole moment change is related to a bond direction, for example, the nitrile stretching vibration.
  • Page 104 104 . MultiScope System Microscope User's Reference Equipm ent The polarizer has a rotatable silver bromide element in an aluminum mount (Figure 29) Figure 29 The Infrared Polarizer...
  • Page 105 Operating the Optional Equipment Using the P olarizer 1. Remove the metal cover that masks the aperture for the Infrared polarizer. 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.
  • Page 106 106 . MultiScope System Microscope User's Reference 4. Turn the wheel in order to orient the polarizing element. The 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.

  • Page 107: Collecting A Spectrum In An Inert Atmosphere

    Operating the Optional Equipment Collecting a Spectrum in an I nert Atm osphere The spaces around the sample and the infrared beam can be purged (typically with nitrogen or dry air) to provide an inert atmosphere. P arts of the purging system Some parts of the purging system are shown in Figure 31.
  • Page 108 108 . MultiScope System Microscope User's Reference When all of these parts are in place, the gas entering through the inlet displaces air from the path of the infrared beam and the sample area. P urging the system 1. Make sure that all parts of the purge system, as listed above, are in place.

  • Page 109: Applications

    Applications...

  • Page 110: Applications

    110 . MultiScope System Microscope User's Reference 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: Reflectance Ft-Ir Microspectroscopy

    Applications R eflectance FT-I R M icrospectroscopy The MultiScope System Microscope can be used with samples that display any of the three types of reflectance: diffuse reflectance, specular reflectance, or reflection-absorption. Figure 32 Three Types of Reflectance Figure 32 shows how the incident radiation (I ) is reflected in each type of reflectance.
  • 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 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 greatest limitation to this method is the presence of an interfering diffuse reflection signal.
  • Page 114 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 detector.

  • Page 115: Polymers

    Applications P olym ers In multicomponent polymeric structures such as laminates, or when one material is embedded in another, you do not need to separate the various components in order to identify them. If you obtain a microscopic cross-section, you can visually locate the component that is of interest, isolate it with the variable knife-edge aperture, and collect its spectrum.
  • Page 116 116 . MultiScope System Microscope User's Reference Textiles Textile scientists have used the MultiScope System Microscope to identify contaminant areas on fabrics or to study single fibers. Figure 37 is the transmittance spectrum of a flattened 20 µm poly(hexamethylene adipamide) fiber.

  • Page 117: Criminalistics

    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: Biological Materials

    1030 cm 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 medium-band MCT detector.

  • Page 119: Product Contaminants

    (SiO ) 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 and a Spectrum RX with a narrow-band MCT detector.
  • Page 120 CaCO 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 Spectrum RX with a narrow-band MCT detector.
  • Page 121 Applications Figure 42 Photocopier 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

    M aintenance...

  • Page 124: Maintenance

    124 . MultiScope System Microscope User's Reference M aintenance Switch off the mains voltage and remove the mains cord before cleaning. WARNING This chapter gives you the routine procedures you must follow to keep your microscope performing well: • Inspecting the microscope;...
  • Page 125 Maintenance I nspecting the M icroscope The covers of the MultiScope must only be removed by a CAUTION PerkinElmer Service Engineer. At least once a year, or whenever the microscope has been subjected to adverse environmental conditions, visually inspect the housing to verify that no covers are loose or distorted so as to allow access to the laser radiation in the interior.
  • Page 126 126 . MultiScope System Microscope User's Reference Cleaning the M icroscope Cover Ensure the power is switched off and the supply lead is CAUTION disconnected before cleaning the cover. You can clean the outside of the microscope using a damp cloth. Mild detergent may be used, if necessary.

  • Page 127: Selecting The Microscope Voltage And Renewing The Fuse

    Maintenance Selecting the M icroscope Voltage and R enew ing the Fuse The microscope is dual-voltage and can be supplied with 100 V to 120 V or 200 V to 240 V; make sure that it is set to the correct voltage. The voltage selector is on the rear panel of the microscope, under the mains inlet and power switch.

  • Page 128: Aligning The Mct Detector

    MCT detector cover. Lift off the cover vertically. The red MCT dewar and the metal frame and springs that support it become visible (Figure 43). Figure 43 Interior of the Detector Area of the MultiScope System Microscope...
  • Page 129 Maintenance 3. If the dewar is not already filled with liquid nitrogen, fill it as described Cooling the MCT detector on page 48. 4. Set the microscope for infrared transmittance: switch the View/IR knob to IR and the Trans/Refl knob to Trans. NOTE: If a Model 1600 or Spectrum BX is being used, select the external beam.

  • Page 130: Changing The Lamp

    130 . MultiScope System Microscope User's Reference Changing the Lam p Switch off the microscope and remove the mains cord from the microscope. The areas surrounding the lamp and some components of the lamp power supply board may still be hot; allow a few minutes for these to cool before proceeding.
  • Page 131 Maintenance 10. Pass the lamp leads through the opening in the top of the lamp baffle. Make sure that the screws connecting the lamp leads are tight. Failure to do this may result in overheating and damage to the microscope. WARNING Refit the lamp baffle over the lamp, refit the screws.

  • Page 132: Electrical Connections

    132 . MultiScope System Microscope User's Reference Electrical Connections Fitting the P lug The power cable for the electrical supply plugs into the back of the microscope. It has a molded connector at one end. If it is necessary to fit a plug on the power...
  • Page 133 Maintenance Connecting the M ultiScope System M icroscope to the Electrical Supply 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.
  • Page 134 The cable from the microscope to the spectrometer comes 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:...
  • Page 135 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...
  • Page 136 136 . MultiScope System Microscope User's Reference The following table shows all of the connections from the pre-amp in the microscope to a Spectrum BX (Paragon): Pl 1 (PCB) CONN-IDC SKT 15 Line Power Requirement Output signal Output signal (0 V)
  • Page 137 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 138 138 . MultiScope System Microscope User's Reference The following table shows all of the connections from the pre-amp in the microscope to a Spectrum GX: J1 1 (PCB), 25-way 25-way Line Power D-type D-type Requirement +15 V 150 mA +15 V...
  • Page 139 Maintenance Service All optical and mechanical equipment requires periodic servicing to keep it performing properly and to 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.

  • Page 140: Appendix: Weee Instructions For Perkinelmer Products

    140 . MultiScope System Microscope Reference Guide Appendix: W EEE I nstructions for P erkinElm er P roducts A label with a crossed-out wheeled bin symbol and a rectangular bar indicates that the product is covered by the Waste Electrical and Electronic Equipment (WEEE) Directive and is not to be disposed of as unsorted municipal waste.

  • Page 141: Index

    Index . 141 I ndex Accessories Fibers ........55, 99 compression cell ...... 81 bicomponent ......99 diamond anvil cell ....69, 76 Fibrous solids ......79 hot stage ........ 82 Film, thin........59 microtome ......69, 75 FT-IR ......... 32 Acrylic resins ......
  • Page 142 142 . MultiScope System Microscope User's Reference nujol........79 Service ........139 Signal-to-noise ratio ....33 Specifications ......42 Spectrum Optical system ....33, 36, 42 collecting ....39, 58, 84, 91 cleaning ........ 125 collecting sample first ....92 Paraffin wax .......

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