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Techniques for Collecting Spectra . 93

The greatest limitation to this method is the presence of an interfering diffuse reflection

signal. This occurs when the sample surface is not perfectly smooth. The Kramers–Kronig

integration is not appropriate for spectra from such samples.

Reflection-Absorption

Reflection-absorption occurs when the incident radiation passes through a thin, absorbent film

that is on a reflective surface (typically a metal) and is then reflected back through the film

(see Figure 40). The absorbance spectrum of the film can be collected directly. Figure 43

shows the spectrum of residual oil on an electronic contact. The sample diameter was 100 µm.

Figure 43 Reflection-absorption spectrum of residual oil on an electronic contact

Summary of Contents for Spotlight 150

Page 1: ...Spotlight 150 User s Guide MOLECULAR SPECTROSCOPY ...

Page 2: ...r errors contained herein for incidental consequential damages in connection with furnishing performance or use of this material Copyright Information This document contains proprietary information that is protected by copyright All rights are reserved No part of this publication may be reproduced in any form whatsoever or translated into any language without the prior written permission of Perkin...

Page 3: ...f the Spotlight 150 24 Connections 25 Operation 26 The Optical System 27 Visible Light Optics 27 Infrared Optics 30 Getting Ready to Use the Spotlight 150 33 Before Using the Spotlight 150 34 Cooling the MCT Detector 35 Setting up the Spotlight 150 38 Focusing the Microscope 39 Fitting an Attenuator to the Spectrometer 41 Setting Scan Parameters 42 Preparing Samples 45 Preparing Samples 46 Tools f...

Page 4: ... ATR Objective 80 Manual ATR Objective 80 Automated ATR Objective 80 Cleaning the ATR Objective Crystal 82 Auto ATR Cleaning Procedure 83 Materials Needed 83 Cleaning Procedure 83 Collecting Spectra with the ATR Crystal 88 Manual ATR Objective 88 Automated ATR Objective 89 Reflectance FT IR Microspectroscopy 91 Diffuse Reflectance 91 Specular Reflectance 92 Reflection Absorption 93 Maintenance 94 ...

Page 5: ...Introduction ...

Page 6: ... s Guide contain information on using and maintaining your Spotlight 150 Getting Ready to Use the Spotlight 150 gives you information on how to set up your Spotlight 150 at the beginning of the day s work to make sure that it is working properly Preparing Samples describes techniques for preparing many types of microscopic samples It includes descriptions of the sample preparation tools provided w...

Page 7: ...ess two keys at the same time for example ALT F All eight digit numbers are PerkinElmer part numbers unless stated otherwise Spectrometer refers to the Frontier IR Systems Spectrum 400 Series Spectrum 100 Series Spectrum 65 or Spectrum One spectrometer supplied with your Spotlight 150 Notes Cautions and Warnings Three terms in the following standard formats are also used to highlight special circu...

Page 8: ...los recuadros como éste se proporciona información sobre este tipo de circunstancias Caution Attention Nous utilisons le terme CAUTION ATTENTION pour signaler les situations susceptibles de provoquer de graves détériorations de l instrument ou d autre matériel Les détails sur ces circonstances figurent dans un encadré semblable à celui ci Caution Attenzione Con il termine CAUTION ATTENZIONE vengon...

Page 9: ...recuadros como éste se proporciona información sobre este tipo de circunstancias Warning Danger Nous utilisons la formule WARNING DANGER pour avertir des situations pouvant occasionner des dommages corporels à l utilisateur ou à d autres personnes Les détails sur ces circonstances sont données dans un encadré semblable à celui ci Warning Pericolo Con il termine WARNING PERICOLO vengono segnalate s...

Page 10: ...reen Help system which you can access by selecting Contents from the Help menu by using the F1 key or by clicking the Help button in a dialog The Help information assumes that you are familiar with the hardware components of the Spotlight 150 microscope contained in this guide Requirements for using the Spotlight 150 We assume that the Spotlight 150 has been properly set up and aligned This instal...

Page 11: ...Warnings and Safety Information ...

Page 12: ... User s Guide The Spotlight 150 The Spotlight 150 consists of a microscope FT IR spectrometer and a PC Figure 1 Spotlight 150 Microscope and Frontier IR System Figure 2 Spotlight 150 Microscope and Spectrum Two System ...

Page 13: ...enters the main body of the microscope or spectrometer switch off the power and call a PerkinElmer Service Representative If your Spotlight 150 is fitted with an MCT mercury cadmium telluride detector DO wear safety glasses and protective gloves when you are filling the detector dewar in the microscope with liquid nitrogen Slowly pour the liquid nitrogen into the dewar Stand back from the detector...

Page 14: ... C Relative humidity 80 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 is necessary this must be done by a skilled person who is aware of the hazard involved Whenever it is likely that the microscope is unsafe make it inoperative The microscope may be unsafe if it Sh...

Page 15: ... live parts NOTE There are no user serviceable parts in the microscope Capacitors inside the microscope may still be charged even if the microscope has been disconnected from all voltage sources Disconnect the microscope from all voltage sources before opening for any adjustment replacement maintenance or repair Any adjustment replacement maintenance or repair must be performed by a PerkinElmer Se...

Page 16: ...ystem 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 17: ...out the nature of the potential hazard and any actions which have to be taken Microscope Safety Labels The following safety labels are fixed to the microscope Figure 3 Rear of Microscope Figure 4 Inside Dewar lid MCT detector versions only NOTE See Cooling the MCT Detector on page 35 for information on how to fill the Dewar Power 100 230 V 50 60 Hz 75 VA ...

Page 18: ... User s Guide Warning Signs on the Microscope Caution risk of electric shock Caution risk of danger Refer to accompanying documents to find out the nature of the potential hazard and any actions which have to be taken ...

Page 19: ...ft these instruments Take care not to injure yourself or others or to drop the instruments The microscope weighs approximately 32 kg Lift the microscope only by the base Do not attempt to lift it by the stage cassegrain assembly or other attachments The spectrometer weighs approximately 34 kg unpacked and has a lifting recess on either side Do not move the Spotlight 150 after it has been installed...

Page 20: ...EMC standard EN61326 EMC standard for electrical equipment for measurement control and laboratory use and EN55011 ISM class A rf emissions FCC rules and regulations This product is classified as a digital device used exclusively as industrial commercial or medical test equipment It is exempt from the technical standards specified in Part 15 of the FCC Rules and Regulations based on Section 15 103 ...

Page 21: ... Microscope The microscope can operate on electricity supplies of 50 or 60 Hz and in a voltage range of 100 to 240 V The primary fuse 2 A T 250 V part number 04970839 for the microscope is in the drawer on the mains inlet connector NOTE No voltage selection is required Site Requirements A minimum bench space of 170 75 cm 68 30 inches is required to accommodate the microscope spectrometer PC and an...

Page 22: ...22 Spotlight 150 User s Guide Safety Specifications Microscope Power supply 100 230 V 10 50 60 Hz 10 Primary fuse 2 0 A T time lag 250 V Weight 32 kg without the sample stage ...

Page 23: ...Overview of the Spotlight 150 ...

Page 24: ...perture that closes to the size and rotation selected when you select a scan or monitor command Spectrum software controls the operation of the microscope for example the illumination of the sample adjusting the correction and changing to reflectance or transmittance Some versions of the microscope also feature LED lighting of the stage area which is controlled from the software An optional micro ...

Page 25: ... show the connections on the microscope Figure 5 Connections top rear of microscope Figure 6 Connections bottom rear of microscope SP1 connects to spectrometer external left port Single element detector output 9 way D type male Video Connects to PC RS232 9 way D type ...

Page 26: ...een 50 µm and 200 µm InGaAs detector Between 10 µm and 200 µm Reflectance Single areas of coatings and thick solids The optimal aperture range depends upon the detector type as follows MCT detector Between 10 µm and 100 µm DTGS detector Between 50 µm and 200 µm InGaAs detector Between 10 µm and 200 µm With ATR objective Thick non reflecting samples NOTE In general the larger the aperture setting t...

Page 27: ...bles you to select between transmittance and reflectance operation This section describes what happens within the optical system when the system changes from visible light to infrared mode in transmittance and reflectance operation Dichroic mirrors form part of the optical system The dichroic mirrors used in the microscope reflect infrared and transmit visible light Visible Light Optics When you v...

Page 28: ...es it at the sample position The upper cassegrain collects light from the sample and sends it upward through the aperture and the upper dichroic mirror Figure 7 Path of the visible beam for viewing a sample in transmittance NOTE Figure 7 above illustrates a Spotlight 150 with an MCT detector Other detector types may look different but the optical arrangement is the same in all cases Detector Camer...

Page 29: ...gh the aperture The lower transmission illuminator is also active in reflectance mode giving simultaneous illumination from above and below Figure 8 Path of the visible beam for viewing a sample in reflectance NOTE Figure 8 above illustrates a Spotlight 150 with an MCT detector Other detector types may look different but the optical arrangement is the same in all cases Mirror pair Visible focus le...

Page 30: ...when viewing a sample in transmittance as follows Figure 9 Instead of receiving light from the illuminator light from the spectrometer is reflected off the toroid onto the lower dichroic mirror which sends it through the lower cassegrain The upper dichroic mirror reflects the beam onto the detector cassegrain The detector cassegrain focuses the beam on to the detector Figure 9 Path of the infrared...

Page 31: ...ough the other side of the cassegrain toward the remote aperture The detector cassegrain focuses the beam on to the detector Figure 10 Path of the infrared beam for collecting IR spectra in reflectance NOTE Figure 10 above illustrates a Spotlight 150 with an MCT detector Other detector types may look different but the optical arrangement is the same in all cases Dichroic mirror Variable aperture R...

Page 32: ...32 Spotlight 150 User s Guide ...

Page 33: ...Getting Ready to Use the Spotlight 150 ...

Page 34: ...ke sure the spectrometer is switched on Switch the microscope on Cool the detector MCT detector versions only Set up the microscope Focus the microscope We recommend that you use these procedures at the beginning of the day s work or any time the Spotlight 150 has not been in use or has been used by others ...

Page 35: ...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 specified time when filling the funnel and before replacing the detector cap This en...

Page 36: ...h liquid nitrogen Stand back and let the funnel empty completely The liquid nitrogen bubbles rapidly as it drains into the dewar This first amount of liquid nitrogen vaporizes completely as it cools the dewar 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...

Page 37: ...g refit the detector cap The filled dewar cools the MCT to the correct operating temperature for several hours After that the dewar begins to return to room temperature and the preamp switches off power to the MCT NOTE If the level of coolant is low a message prompting you to refill the dewar will be displayed in the Status bar at the bottom of the Spectrum workspace ...

Page 38: ...n The Spectrum start up splash screen is displayed followed by a dialog that may require your login details 4 If required enter your User name and Password and then click OK An instrument selection dialog is displayed 5 Select the Instrument you want to use OR If you want to work with data that has been collected previously without connecting to an instrument select to work offline NOTE Working of...

Page 39: ...ment at this time you can click Cancel You will not be able to use any of the microscope controls on the Setup Microscope tab until you have initialized the microscope To initialize the microscope later click Initialize on the Setup Microscope tab Focusing the Microscope Microscope sample positioning and focus controls The focus of the microscope is changed by moving the sample stage up or down Wh...

Page 40: ...ing the Sampling Mode group expanded 3 Position your sample using the stage controls on the microscope so that you can see the live image of the object of interest 4 Focus on the sample using the microscope focus controls You may also need to change the illumination of the sample or the correction when focussing the image Coarse outer and fine inner focus controls X axis stage control left to righ...

Page 41: ...mination to give good illumination of your sample Fitting an Attenuator to the Spectrometer If your Spotlight 150 is supplied with a Frontier or Spectrum 400 FT IR FT NIR dual range spectrometer or if your Spotlight 150 has an InGaAs detector you will be provided with an Attenuator kit part number L1160560 containing 1 T 4 T 6 T 14 T and 32 T attenuators The attenuators attach to the external beam...

Page 42: ...vise you of the lower limit to the low wavenumber at the time of installation or it will be recorded on the Service Installation test spectra For near IR measurements on a system fitted with an InGaAs detector the upper wavenumber value is typically set to between 15800 and 8000 cm 1 and the lower limit to 4000 cm 1 NOTE To work in the near IR range of the spectrum the Spotlight 150 must be attach...

Page 43: ... on page 41 for details This attenuator should be kept in place during data acquisition 13 If for any reason you want to stop scanning your sample click Optimizing Transmission measurements In most cases samples for transmission measurements are placed flat on top of an IR transmitting window such as NaCl KBr BaF2 ZnSe or diamond In some cases such as flattened fibers the sample is simply secured ...

Page 44: ...ent toolbar 7 Collect a background spectrum through this point on the window or aperture using the correct aperture size as selected previously 8 Return the stage to the selected sample position adjust the correction and then record the sample spectrum NOTE If a detector overload error is reported in the Status Bar when monitoring or collecting data then fit an attenuator to the external beam wind...

Page 45: ...Preparing Samples ...

Page 46: ...o collect transmission spectra the sample should ideally be thin enough approximately 5 to 20 µm to give good detail and undistorted absorption bands The area of the sample must be large enough 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 The sample can be flattened by rollin...

Page 47: ...mm disk holder Supporting samples and allows rotation of the sample Support for large samples Clips on to the sample stage supporting bulky samples so that the stage clip does not interfere with them Gold mirror assembly Reflection measurements KBr windows 2 Supporting samples The following tools are provided in the Microsampling toolkit Tool Use Steel tweezers Picking up extremely small objects R...

Page 48: ...l Part Number Microprobe with right angle bend N9302606 Forceps round tips N9302607 Forceps narrow needle points N9302608 Windows All 13 mm diameter BaF2 1 mm thick N9302611 BaF2 2 mm thick N9302612 ZnSe 1 mm thick N9302613 NaCl 2 mm thick N9302614 KBr 2 mm thick N9302615 Wide tipped forceps hooked 09908138 Wide tipped forceps flat 09908400 1 5 mm microdisk fits in 13 mm disk holder to support ver...

Page 49: ...age 51 Miniature Diamond Anvil Cell part number N9302618 Fiber Optic Illuminator part number N9302602 Microtome Items to Have Available In addition to the items provided with the Spotlight 150 we recommend that you have the following available Tape with adhesive on both sides double sided tape for holding long or large samples on the sample stage Single edge razor blades for cutting samples ...

Page 50: ...1 The major disadvantage of this material is that it is hygroscopic so that the windows fog easily BaF2 Barium fluoride is not hygroscopic Its transmittance cut off is 750 cm 1 It can break or crack easily NaCl Sodium chloride transmits infrared down to 600 cm 1 Otherwise its properties are similar to KBr ZnSe Zinc selenide is not hygroscopic Its transmittance cut off is 650 cm 1 ZnSe is more dura...

Page 51: ...lass or metal A flat black cap from a jar makes a good surface for rolling a light colored sample If you roll the sample on a small flat piece of metal you can view it and collect spectra in reflectance mode Samples rolled on windows transparent to infrared can be examined in transmittance If you flatten fibers on a glass microscope slide they can then be peeled off and mounted either on a window ...

Page 52: ...area because the area of contact is small Rolling a hard sample with the side of a sewing needle held in a pin vise presses it into a flake Slicing Samples from Solids Cutting a wedge of sample Cutting a wedge shaped piece from its edge enables you to produce a thin sample while destroying very little of the original This technique can be used with laminates plastics films paint chips and paper To...

Page 53: ...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 embedding materials These can be used depending on the size and porosity of the sample Acrylic and epoxy resins Although these are commonly used in lig...

Page 54: ...the three screws and tighten them finger tight NOTE If the spectrum collected with the diamond anvil cell shows interference fringes place some KBr in the cell and collect a background spectrum through it Figure 20 The miniature diamond anvil cell Pressing elastomers between windows If your sample is elastic and you are compressing it between windows you must apply pressure continuously Use the fo...

Page 55: ...s left behind as ash 3 Score and break the pipette between the ash and the pyrolysate 4 Add a drop of solvent to the pyrolysate to wash it on to a salt plate If the amount of sample is small use a capillary tube instead of a disposable pipette Using a microbrush to pyrolyze micro amounts 1 Seal the end that is away from the brush fibers and tap the sample particle into this end then heat it gently...

Page 56: ...map to help you positively identify the particles under the microscope Transferring with a tungsten needle When necessary sharpen the tungsten needle 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 reflection or s...

Page 57: ...an use a micropipette to apply liquid to the surface of a salt plate or to the edge of the junction between two 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 t...

Page 58: ...58 Spotlight 150 User s Guide ...

Page 59: ...Techniques for Collecting Spectra ...

Page 60: ... to apply pressure across the windows The sample is held between the two windows The compression cell fits into the sample slide holder on the stage of the microscope Windows with thicknesses equal to 1 mm and 2 mm and outer diameter equal to 13 mm can be used with the cell Two KBr windows 2 mm thickness are included with the system The cell can apply pressure without rotating the windows and ther...

Page 61: ...m is focused if no sample is on the stage 3 Move the sample stage to its highest possible position 4 Release the locking lever located on the right side on the back of the lower cassegrain assembly Figure 22 Figure 22 The lower cassegrain 5 Gently slide the cassegrain assembly forward and out of the dovetail connector NOTE To make withdrawal easier pull the locking lever gently 6 Click Park in the...

Page 62: ... where the infrared beam is focused if no sample is on the stage 3 Make sure that the cassegrain is correctly seated 4 Place the gaiter over the cassegrain if the purge facility is required 5 Slide the cassegrain assembly back into the dovetail connector as far as it goes NOTE To make replacement easier pull the locking lever gently 6 Tighten the locking lever Collecting a Spectrum in an Inert Atm...

Page 63: ...the gas entering through the inlet displaces air from the path of the infrared beam Purging the system 1 Make sure that all parts of the purge system as listed above are in place 2 Set up the microscope See Getting Ready to Use the Spotlight 150 starting on page 33 3 Place the sample in position 4 Purge the microscope and spectrometer for 15 to 20 minutes at a rate of 10 l min 1 5 Collect the back...

Page 64: ...e passage of only those waves that have their plane of vibration in one particular direction The light that emerges is said to be polarized and is represented on the right side of Figure 24 Figure 24 Representation of unpolarized light left and polarized light right Because all components of the wave in the plane of polarization are transmitted the ideal polarizer allows 50 of the light through If...

Page 65: ...nge in polarization is dependent on the wavelength the color of the light emerging changes with the distance traveled through the sample and the amount of birefringence encountered Applications 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 in...

Page 66: ...k and their cylindrical shape can cause lensing effects For these reasons fibers are usually flattened in preparation for infrared microspectroscopy This flattening affects the birefringence of the structure and may degrade the usefulness of this technique Biological substances Birefringence can occur in some biological substances You can collect infrared spectra of thin sections of these material...

Page 67: ...r in with the wheel facing towards you It has two positions The first position allows the full beam to pass through When the analyzer is inserted fully the polarizing element is in the beam Figure 27 Analyzer position 2 When the polarizing element is in the beam rotate the wheel while viewing the sample image on the Setup microscope tab Visible Analyzer Slot ...

Page 68: ...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 the nitrile absorption peak is much stronger th...

Page 69: ...cope and the wheel facing outwards Figure 29 Infrared polarizer position 3 Push the analyzer into the slot until it stops 4 Turn the wheel to orient the polarizing element CAUTION 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 When it is not in use protect it in the case supplied NOTE Both th...

Page 70: ... µm The penetration depth also varies with the wavenumber of the infrared radiation 2 1 2 21 2 1 sin 2 n n d p θ p λ Where 1 n is the refractive index of the ATR crystal for germanium 4 0 λ is the wavelength of the radiation θ is the angle of incidence of the beam 21 n is the ratio of the refractive indices of the sample and the ATR crystal ATR objective The ATR objective enables the microscopic e...

Page 71: ...cassegrain and is focused at the sample position It is reflected once within the crystal then the totally internally reflected beam is collected by the rear portion of the upper cassegrain which focuses it on the remote aperture The radiation is directed onto the detector in the microscope Figure 30 Infrared radiation optical path ...

Page 72: ...surement Ge 5500 cm 1 to 600 cm 1 Ge Di 5500 cm 1 to 600 cm 1 Si 7800 cm 1 to 800 cm 1 Area of contact with sample Nominally 100 µm diameter flat surface Single internal reflection from surface Maintenance The ATR assembly may be removed see Removing the ATR Crystal Holder on page 79 cleaned see Cleaning the ATR Objective Crystal on page 82 and replaced and aligned by the user see Fitting the ATR ...

Page 73: ...ly under the upper cassegrain Be careful not to change the alignment of the two adjusting levers 4 Fit the two adjustment thumb nuts see Figure 31 The assembly is aligned if the adjusting levers have not been moved 5 If fitting the automated ATR objective insert the jack plug into the socket at the rear of the cassegrain Figure 32 Lower the stage if necessary to improve the access to the socket 6 ...

Page 74: ...otlight 150 User s Guide Figure 32 The Automated ATR Crystal Holder and Cassegrain Jack plug socket plug not shown ATR crystal assembly Crystal holder Motor lowers and retracts the crystal Knurled thumb nut ...

Page 75: ...n the Setup Instrument BeamPath tab 4 Place the slide holding the reference mirror L1860409 supplied with the microscope on the sample stage 5 Make sure that the microscope is in reflectance mode by selecting Reflectance in the Sampling Mode section of the Setup Microscope tab 6 Look at the live image and focus the beam on the surface of the mirror There are often dust particles or scratches on th...

Page 76: ...clockwise and slowly lowering the toggle bar You must always support both ends of the toggle bar when lowering or raising the crystal OR Click the button to lower the automated ATR crystal onto the reference mirror 2 Using the knurled height adjustment nut adjust the height of the crystal so that it just rests on the mirror under positive pressure Figure 34 Figure 34 Adjusting the Crystal Height M...

Page 77: ... If there is a deep impression on the tape which does not disappear within a few seconds the crystal height should be raised slightly by turning the knurled height adjustment nut clockwise a quarter of a turn 6 If appropriate repeat steps 4 and 5 until the crystal just touches the tape 7 Once the crystal height has been corrected look at the impression of the crystal on the tape Decide whether the...

Page 78: ... least 20 of the maximum energy measured in reflectance mode see Measuring the Energy in Reflectance Mode on page 75 for details 1 Place the slide holding the reference mirror supplied with the microscope on the Sample Stage 2 Look at the video image on the Setup Microscope tab and focus the microscope on the surface of the mirror There are usually dust particles or scratches on the surface that y...

Page 79: ...um on screen Help for further information 3 Make sure that the ATR crystal is in the raised position 4 Screw the plastic protective cover in place over the crystal 5 For the automated ATR objective remove the jack plug from its socket 6 While holding the crystal assembly unscrew the two adjustment thumb nuts completely Allow the assembly to drop vertically from the cassegrain Be careful not to dis...

Page 80: ...holder 5 Place the new crystal assembly into the ATR crystal holder and refit the height adjusting nut Take care not to damage the crystal 6 Refit the ATR crystal holder to the microscope as described on page 73 7 Align and adjust the ATR crystal holder as described on page 77 Figure 37 The Manual ATR Crystal Assembly Automated ATR Objective 1 Remove the ATR crystal holder as described on page 79 ...

Page 81: ...line with the sprung loaded ball bearing in the wall of the holder Figure 39 You will feel the ball bearing slide into the alignment groove and lock the crystal assembly in position Figure 39 Crystal Assembly aligned in holder 8 Refit the height adjustment nut Take care not to damage the crystal 9 Refit the ATR crystal holder to the microscope as described on page 73 10 Align and adjust the ATR cr...

Page 82: ...l or n hexane may be used to clean the crystal NOTE Do not use acetone or xylene to clean the crystal 1 Pour a small volume of a solvent into a shallow dish 2 Lower the sample stage to allow the dish to be placed on the stage under the crystal 3 Raise the stage so that the tip of the crystal is just immersed in the solvent NOTE Do not immerse the whole of the ATR crystal in the solvent 4 Leave the...

Page 83: ...es per year Every 4 5 months Medium User 15 000 cycles per year Every 8 months Light User 5 000 cycles per year Every 12 Months Materials Needed Methanol in a squirt bottle Small Foam Head Swab Recommend VWR P N 89022 992 Kimwipes or similar low lint cleaning wipes Cleaning Procedure 1 If not already done use Spectrum 10 to raise the crystal into the assembly 2 Disconnect the motor wire from the l...

Page 84: ...lder 5 Carefully grab the crystal holder and remove it from the ATR assembly Set the crystal holder aside and be careful not to damage the crystal 6 Look down into the center of the crystal bearing notice the compression spring and the plunger retracted and off to one side Spray methanol into the bore and allow it to drain from the assembly ...

Page 85: ...t all the way around the bore of the bearing 9 Use a methanol moistened Kimwipe to clean the outside bearing surface alignment groove and contact flat opposite the groove on the crystal holder It may be necessary to use a non marring implement to clean any debris on the sliding surfaces I use a finger nail Take care not to damage the crystal This is a good time to clean the crystal itself refer to...

Page 86: ... down on the crystal holder until it stops You may need to twist the holder a small amount from side to side to seat it on the retracted plunger Do not force it you may damage the stop contact 12 Using another swab clean any debris from the knurled stop collar Notice the black spots in the image below 13 Screw the knurled collar on all the way then back off one and a half 1 5 full revolutions This...

Page 87: ... accessory in your Spotlight system and perform the crystal alignment and focusing procedure to maximize IR energy 15 Reset the counter in the Spectrum software on the Setup Microscope Basic tab click the Reset button to reset the Auto ATR Crystal Up Down counter ...

Page 88: ...rom the Measurement menu The software will prompt you to lower the stage to prevent a collision 5 Lower the stage and click OK The software will prompt you to lower the ATR crystal 6 Use the toggle bar to lower the crystal when prompted and click OK The spectrometer starts to scan and the spectrum is displayed as it is collected 7 Retract the ATR crystal when the scan is completed Collecting a Sam...

Page 89: ...rum is satisfactory click Scan The software will again prompt you to lower the crystal and raise the stage but these messages can be cleared by clicking OK The spectrometer starts to scan and the spectrum is displayed as it is collected CAUTION Always retract the ATR crystal immediately after data collection has been completed in order to avoid accidental damage Automated ATR Objective Collecting ...

Page 90: ...isplayed The software will prompt you to lower the stage to prevent a collision when the ATR crystal is lowered 6 Lower the stage and click OK The automated ATR crystal will be lowered automatically NOTE Before you collect the sample spectrum you should monitor the spectrum to make sure that there is good contact between the crystal and the sample 7 Raise the stage carefully until the sample touch...

Page 91: ...e of reflectance is seen in samples with matt surfaces such as paper and powders The broad collection 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 41 shows three di...

Page 92: ...tion in one direction Figure 40 This is the type of reflection that occurs from a smooth polished surface Absorption information cannot be obtained directly from a specular reflectance spectrum of a dielectric material because the reflectance spectrum is governed by dispersion in the refractive index However you can use the Kramers Kronig integration to calculate the absorbance spectrum from the s...

Page 93: ...ples Reflection Absorption Reflection absorption occurs when the incident radiation passes through a thin absorbent film that is on a reflective surface typically a metal and is then reflected back through the film see Figure 40 The absorbance spectrum of the film can be collected directly Figure 43 shows the spectrum of residual oil on an electronic contact The sample diameter was 100 µm Figure 4...

Page 94: ...Maintenance ...

Page 95: ...chapter contains a list of the available spare parts and optional equipment for the microscope If you need to replace a part use only PerkinElmer approved spare parts CAUTION The covers of the microscope must only be removed by a PerkinElmer Service Representative Inspecting the Microscope At least once a year or whenever the microscope has been subjected to adverse environmental conditions visual...

Page 96: ...apart CAUTION Avoid the excessive use of solvents Flowing solvents dissolve the cement on cemented optics dissolved cement can damage mirror surfaces Cleaning the Cover CAUTION Ensure the power is switched off and the supply lead is disconnected before cleaning the cover You can clean the outside of the microscope using a damp cloth Mild detergent may be used if necessary Always perform a patch te...

Page 97: ... 1 Switch off the microscope and disconnect it from the power supply 2 Insert a screwdriver into the slot at the side of the fuse drawer pull out and flip to one side over the mains inlet The fuse may now be removed 3 Fit the replacement fuse into the fuse drawer You require a 2 0 A time lag 250 V fuse part number 04970839 4 Refit the fuse drawer ...

Page 98: ...to keep it performing properly and to compensate for wear We recommend that the Spotlight 150 is cleaned examined and adjusted periodically by a PerkinElmer Service Representative NOTE If you experience unexpected problems with the microscope contact your PerkinElmer office or representative immediately ...

Page 99: ...1870185 Rotatable Sample Disk Holder N1873039 Holder for Reflection Transmission Measurements N1873124 BaF2 Window 1 mm thick N9302611 BaF2 Window 2 mm thick N9302612 ZnSe Window N9302613 NaCl Window N9302614 KBr Window N9302615 Miniature Diamond Anvil Cell N9302618 Spare Germanium Crystal Manual L1860268 Spare Silicon Crystal Manual L1860269 Spare Diamond Coated Germanium Crystal Manual L1862054 ...

Page 100: ...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 instrument 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 equivalent...

Page 101: ...ure 44 The location of the electrical supply inlet Connecting the Microscope to the Spectrometer The cable from the microscope to the spectrometer comes from the preamp inside the microscope to a connector marked on the rear of the spectrometer The connections from the pre amp in the microscope to the spectrometer are described below Pl 1 PCB D type Connector Line Power Requirement 1 11 Output Sig...

Page 102: ...Appendices ...

Page 103: ...ipment Decontamination Procedure and complete the Certificate of Decontamination These documents are available on the PerkinElmer public website http las perkinelmer com OneSource decontamination htm Alternatively if you do not have access to the internet contact Customer Care Customer Care USA 1 800 762 4000 inside the USA 8 30 a m 7 p m EST 1 203 925 4602 outside the USA Customer Care Canada 800...

Page 104: ... 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 for infor...

Page 105: ...03 Compliance EC directive 20 EMC 20 FCC 20 Connections microscope 25 101 power 100 Conventions 7 Cooling MCT detector 35 Counter reset 87 D Definitions 10 F Fibers 66 Fuse microscope 21 97 I Illuminator 24 Image collecting 30 focusing 40 41 in reflectance 31 in transmittance 30 IR polarizer 68 Inert atmosphere 62 Inspection microscope 95 IR polarizer equipment 68 operation 69 L Liquids small quan...

Page 106: ... focusing 39 lifting 19 operation 26 scan parameters 42 setting up 38 T Techniques compressing 51 crushing 55 diamond anvil cell using 53 flattening solids 51 for biological substances 66 for fibers 66 for laminates 65 for minerals crystals 66 for polymer films 66 for soft materials 60 for thick samples 61 microbrush using 55 microtoming 53 mulls using 56 needle pressing sample with 52 needle tran...

Page 107: ... 16 Viewing in reflectance 29 in transmittance 28 sample 27 Visible polarizer biological substances 66 equipment 66 fibers 66 laminate structures 65 minerals crystals 66 operation 67 polymer films 66 theory 64 W Warning labels 17 microscope 18 WEEE Directive 104 Windows compressing between 52 types 50 Windows Start Menu 38 ...

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PerkinElmer Spotlight 150, User Manual

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