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Preparing Samples . 49

Tools for Sample Preparation

This section lists the tools you need for preparing samples:

•

Tools provided with the imaging system;

•

Tools in the microsampling toolkit;

•

Materials to have available;

•

Specialized accessories you may want to purchase.

Tools Provided with the Imaging System

The following items for use in sampling are provided in the Sampling Accessories Kit that is

supplied:

Item

Use

Holder for 13 mm disks

Supporting 13 mm disks on the sample stage.

Slides, glass (box)

Supporting samples for sample preparation.

Rotating 13 mm disk holder

Supporting samples and allows 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 slide

Background sample for measurements in reflectance

mode.

Gold mirror and white reflector

slide

Background sample for measurements in reflectance and

diffuse reflectance modes (supplied with InGaAs systems).

KBr windows (2)

Supporting samples.

Содержание Spotlight 400 Series

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

Страница 2: ...ot be liable for errors contained herein for incidental consequential damages in connection with furnishing performance or use of this material Copyright Information This document contains proprietary...

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

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

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

Страница 6: ......

Страница 7: ...Introduction...

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

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

Страница 10: ...s En los recuadros como ste se proporciona informaci n sobre este tipo de circunstancias Caution Attention Nous utilisons le terme CAUTION ATTENTION pour signaler les situations susceptibles de provoq...

Страница 11: ...los recuadros como ste se proporciona informaci n sobre este tipo de circunstancias Warning Danger Nous utilisons la formule WARNING DANGER pour avertir des situations pouvant occasionner des dommages...

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

Страница 13: ...Warnings and Safety Information...

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

Страница 47: ...Preparing Samples...

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

Страница 95: ...Maintenance...

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

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

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

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

Страница 100: ...remove the mains cord 2 Insert a screwdriver into the slot at the side of the fuse drawer and pull out and flip to one side over the mains inlet The fuse may now be removed 3 Fit the replacement fuse...

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

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

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

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

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

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

Страница 107: ...Appendices...

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

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

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

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

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

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

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

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

Страница 116: ...rom contamination The customer s responsible body is required to follow the Equipment Decontamination Procedure and complete the Certificate of Decontamination These documents are available on the Per...

Страница 117: ...effective means of protecting the customer s environment The requirements for waste collection reuse recycling and recovery programs are set by the regulatory authority in your location Contact your...

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

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

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

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