2423_DXR_Raman_UG.pdf

FT-IR Spectrometers

Using Your DXR Raman Instrument part-number 269-242301 Revision A August 2012

© 2012 Thermo Fisher Scientific Inc. All rights reserved.

Thermo Fisher Scientific Inc. provides this document to its customers with a product purchase to use in the product operation. This document is copyright protected and any reproduction of the whole or any part of this document is strictly prohibited, except with the written authorization of Thermo Fisher Scientific Inc. The contents of this document are subject to change without notice. All technical information in this document is for reference purposes only. System configurations and specifications in this document supersede all previous information received by the purchaser. Thermo Fisher Scientific Inc. makes no representations that this document is complete, accurate or errorfree and assumes no responsibility and will not be liable for any errors, omissions, damage or loss that might result from any use of this document, even if the information in the document is followed properly. This document is not part of any sales contract between Thermo Fisher Scientific Inc. and a purchaser. This document shall in no way govern or modify any Terms and Conditions of Sale, which Terms and Conditions of Sale shall govern all conflicting information between the two documents.

For Research Use Only. Not for use in diagnostic procedures.

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Chapter 1

Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1 Questions or Concerns . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1 Conventions Used . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1 Safety Precautions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2 Warranty . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2 Warranty Period . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3 Limits of Warranty . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3 Items not Covered by Warranty . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3 Finding PDF Documents . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3 Ordering Parts. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3

Chapter 2

Using a DXR SmartRaman . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5 Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5 Changing the Laser, Filter, and Grating. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5 Installing an Accessory. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6 Installing an Accessory Tool Head. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6 Enabling the laser . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6 Using a Class IIIb Fiber Optic Accessory . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7 Installing the Spectrometer Alignment Tool . . . . . . . . . . . . . . . . . . . . . . . . . . 9 Installing a 455 nm Laser . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10 Installing a 633 nm Laser . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10 Service . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13 Cleaning Your Instrument. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13 Replacing Fuses . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14 Alignment at Installation for a 633 nm Laser on a DXR SmartRaman . . . . . 14 Safety . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17 Safety Precautions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17 Safety Goggle Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18 Setting up a Laser Safety Area . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18 Safety and Electrical Symbols . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20 Indicators . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21 WEEE Compliance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21 Biohazards or Radioactive Materials and Infectious Agents . . . . . . . . . . . . . . 22 Cooling Fans . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22 Using Corrosives and Solvents. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22 Spectrometer Safety Labels . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23

Using Your DXR Raman Instrument

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Contents

Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25 Sample Bands are too Small. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25 Sample Bands Are too Large . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25 No Raman Signal Appears in the Live Display. . . . . . . . . . . . . . . . . . . . . . . . 26 CCD Overflow Occurred . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26 The Spectrum Has No Sample Bands . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26 The Spectrum Has Large Noise Spikes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26 The Spectrum Has a Sloping Background . . . . . . . . . . . . . . . . . . . . . . . . . . . 27 The Spectrum Baseline Is Severely Tilted or Curved . . . . . . . . . . . . . . . . . . . 27 The Spectrum Baseline Has a Severe Positive Offset . . . . . . . . . . . . . . . . . . . 27 The Spectrum Baseline Is Severely Shifted. . . . . . . . . . . . . . . . . . . . . . . . . . . 28 A Grating Does Not Appear to Be Installed or the Grating Cover Is Open . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28 A Laser Does Not Appear to Be Installed. . . . . . . . . . . . . . . . . . . . . . . . . . . . 28 A Filter or Fiber Optic Accessory Does Not Appear to Be Installed . . . . . . . . 28 The Computer Cannot Communicate with the Instrument . . . . . . . . . . . . . 29 Chapter 3

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Using a DXR Raman Microscope . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .31 Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31 Adjusting the Illuminator Intensity . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31 Positioning a Manual Stage . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32 Positioning a Motorized Stage . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32 Using Darkfield Illumination . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 33 Using Confocal Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 33 Changing the Laser, Filter, and Grating. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 33 Enabling the Laser . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34 Using a Class IIIb Microscope . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35 Using a Class IIIb Fiber Optic Accessory . . . . . . . . . . . . . . . . . . . . . . . . . . . . 36 Installing the Microscope Alignment Tool. . . . . . . . . . . . . . . . . . . . . . . . . . . 38 Installing a 455 nm Laser . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 38 Installing a 633 nm Laser . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 38 Service . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42 Cleaning Your Instrument. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42 Replacing the Nosepiece . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 43 Removing the Stage . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 44 Installing a New Stage . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 44 Replacing Fuses . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 45 Replacing an Illuminator Bulb. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 45 Alignment at Installation for a 633 nm Laser on a DXR Raman Microscope. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 48

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Safety . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 52 Safety Precautions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 52 Safety Goggle Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 53 Setting up a Laser Safety Area . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 53 Safety and Electrical Symbols . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 55 Indicators . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 56 WEEE Compliance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 56 Biohazards or Radioactive Materials and Infectious Agents . . . . . . . . . . . . . . 57 Cooling Fans . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 57 Using Corrosives and Solvents. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 57 Microscope Safety Labels. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 58 Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 60 Sample Bands are too Small. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 60 Sample Bands Are too Large . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 60 No Raman Signal Appears in the Live Display. . . . . . . . . . . . . . . . . . . . . . . . 60 No Visible Image Appears in the Video Pane or Viewer . . . . . . . . . . . . . . . . 61 CCD Overflow Occurred . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 61 The Spectrum Has No Sample Bands . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 61 The Spectrum Has Large Noise Spikes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 61 The Spectrum Has a Sloping Background . . . . . . . . . . . . . . . . . . . . . . . . . . . 62 The Spectrum Baseline Is Severely Tilted or Curved . . . . . . . . . . . . . . . . . . . 62 The Spectrum Baseline Has a Severe Positive Offset . . . . . . . . . . . . . . . . . . . 62 The Spectrum Baseline Is Severely Shifted. . . . . . . . . . . . . . . . . . . . . . . . . . . 63 A Grating Does Not Appear to Be Installed or the Grating Cover Is Open . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 63 A Laser Does Not Appear to Be Installed. . . . . . . . . . . . . . . . . . . . . . . . . . . . 63 A Filter or Fiber Optic Accessory Does Not Appear to Be Installed . . . . . . . . 63 The Nosepiece Does not Appear to be Installed. . . . . . . . . . . . . . . . . . . . . . . 64 The Image is Obscured or Distorted . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 64 The Computer Cannot Communicate with the Instrument . . . . . . . . . . . . . 64

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Contents

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Introduction Questions or Concerns In case of emergency, follow the procedures established by your facility. If you have questions or concerns about safety or need assistance with operation, repairs or replacement parts, you can contact our sales or service representative in your area or visit our web site at www.thermo.com/spectroscopy.

Conventions Used This help system includes safety precautions and other important information presented in the following format: WARNING Indicates a hazardous situation which, if not avoided, could result in death or serious injury.

CAUTION Indicates a hazardous situation which, if not avoided, could result in minor or moderate injury. NOTICE Follow instructions with this label to avoid damaging the system hardware or losing data. Note Contains helpful supplementary information.

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Introduction Safety Precautions

Safety Precautions WARNING Class IIIb instruments should always be operated in a laser safety area. All persons using or in the vicinity of a Class IIIb instruments should wear appropriate laser safety goggles and should be aware of the potential hazards. Use of controls or adjustments or performance of procedures other than those specified in your printed and on-line documentation may result in hazardous radiation exposure. Do not alter or attempt to remove the laser head from its protective housing or attempt to remove the shields that surround the laser head. Exposure to laser energy and high voltage may result. The laser energy from the excitation lasers may be visible or invisible. Never stare directly into the laser beam or at its bright reflection. Never tamper with the laser head. Exposure to laser light or high voltage may result. Avoid skin and eye contact with the invisible laser radiation produced by the excitation laser beam and any reflections of that beam. If you wish to observe trained service personnel, wear properly rated laser safety goggles whenever the instrument power is on and the protective covers are open or removed. When operating our Raman instruments, use only accessories and equipment (such as power supplies and lasers) supplied by us. Use of equipment and accessories not supplied by us can result in permanent damage to the instrument and may create a safety hazard. Do not attempt to service a laser that is not functioning properly. If a laser is malfunctioning, contact our sales or service representative in your area or visit our web site at www.thermo.com/spectroscopy for assistance or to order a replacement laser. NOTICE The power connector and the USB stage and computer connectors are located on the panel on the bottom left side of the instrument (as you face the instrument). The connections to these connectors are made by our service representative during the instrument installation. Do not attempt to alter or modify the connections to these connectors. Note See the “Manufacturer’s laser information” section in the safety notice that was included with your instrument for information about individual excitation lasers.

Warranty Thermo Fisher Scientific warrants that each product we sell you is free from defects in labor and materials and shall conform to its product specifications as defined in the product user documentation. If the product does not function as warranted during the warranty period, we will repair or replace it without charge. If in our judgment we are unable to do so, you may return it to us and we will refund your money.

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1 Introduction Finding PDF Documents

This warranty replaces all other warranties, expressed or implied, including the implied warranties of merchantability and fitness for a particular purpose and any other obligations or liabilities on the part of Thermo Fisher Scientific whether in contract, warranty, negligence or otherwise. Thermo Fisher Scientific shall not be liable for and disclaims all consequential, incidental and contingent damages.

Warranty Period The warranty period is 12 months. If you install the product, the warranty begins on date of invoice. If we install the product, the warranty period begins on the date of installation but will begin no later than 30 days from the date of the invoice. The warranty period for products sold outside the U.S.A. and Canada is 12 months from the date of installation or 14 months from the date of shipment, whichever is less.

Limits of Warranty Misuse, accident, modification, unsuitable physical or operating environment, improper maintenance, or damage caused by a product for which we are not responsible will void the warranty. Certain components may have separate warranty periods as stated in the product user documentation. Consumables are not covered under warranty.

Items not Covered by Warranty We do not warrant uninterrupted or error-free operation of a product. We provide certain non-Thermo Fisher Scientific products on an "as is" basis. Non-Thermo Fisher Scientific manufacturers or suppliers may provide their own warranties to you. Separate software warranty is provided with the software user documentation.

Finding PDF Documents PDF files of the documentation for your instrument are installed on the hard drive of the system computer when the software is installed and a shortcut is available from the Start menu: Start > All Programs > Thermo Scientific OMNIC > Documentation.

Ordering Parts To order parts, contact our sales or service representative in your area or visit our web site at www.thermo.com/spectroscopy.

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Introduction Ordering Parts

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Using a DXR SmartRaman Operation Changing the Laser, Filter, and Grating WARNING Avoid shock hazard. Make sure you turn off the spectrometer power before you replace a laser, filter, or grating.

NOTICE Handle lasers, filters, and gratings gently. Do not touch any optical surfaces or the interior of a laser, filter, or grating. When a laser, filter, or grating is not in use, store it in the case that it was shipped in.

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Using a DXR SmartRaman Operation

Installing an Accessory

Installing an Accessory Tool Head

Enabling the laser You must enable the laser before you can turn it on. To enable the laser, rotate the laser key to the locked (vertical) position as shown below. (For more information about turning on the laser, see the software help available through the Help menu in OMNIC.)

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Note You can insert or remove the laser key only when the laser keyswitch is in the unlocked (horizontal) position. When the laser keyswitch is in the unlocked position, the laser is disabled.

Using a Class IIIb Fiber Optic Accessory WARNING The fiber optic accessory is a class IIIb laser product. Making adjustments, using controls, or performing procedures that are not specified in the printed or on-line documentation may result in exposure to hazardous visible or invisible laser radiation. Make sure you follow all safety precautions listed in the Safety section of this help system before you install the fiber optic accessory. To avoid severe burns from exposure to laser radiation or permanent damage to your eyes, never put anything except samples against the tip of the fiber optic probe, and always wear laser safety goggles that meet the specifications for the laser your fiber optic launcher uses. Also, you should never look directly into the tip of a fiber optic probe or the fiber optic probe connectors, even if you are wearing laser safety goggles. The goggles will protect you for diffuse viewing only. Always set up laser safety area in the location where you are using a fiber optic accessory.

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 To Install a Fiber Optic Accessory

1. Slide the accessory into the instrument and connect the fiber optic cables from the probe.

2. Connect the power cable for the probe LED.

The maximum permissible exposure (MPE) is the level of laser radiation that a person may be exposed to, under normal circumstances, without suffering adverse effects. (These levels are based on the assumption that a person is exposed to the laser beam for an infinite length of time.) The nominal ocular hazard distance (NOHD) is the distance from the laser output aperture within which the level of laser radiation exceeds the MPE.

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This table shows the MPE and NOHD values for fiber optic probes with an aperture of 0.22.

Laser

MPE (Watts/ square meter)

NOHD Fiber Optic Accessory (m)

NOHD Macro System, Universal Platform (m)

455 nm

10.0

0.34

0.50

532 nm

10.0

0.28

0.41

633 nm

10.0

0.26

0.38

780 nm

14.4

0.38

0.56

780 nm (high power) 14.4

0.93

1.37

Installing the Spectrometer Alignment Tool

Note For alignment and calibration instructions, please see the alignment and calibration topics in the on-line software help system. The power connection for the spectrometer alignment tool is automatically made when you install the tool.

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Installing a 455 nm Laser Under most circumstances, your instrument has come equipped to permit user installation of a 455 nm laser. If you specifically ordered this laser wavelength with your DXR, see Changing the Laser, Filter, and Grating. If you need to add this capability in the future, a service visit may be required. Contact our sales or service representative in your area or contact us.

Installing a 633 nm Laser This procedure shows how to install a 633 nm laser. If you have any questions or concerns, please contact us. Time needed: Approximately 1 hour Tools needed: 5/32 inch hex wrench, Philips screwdriver Parts needed: 633 nm HeNe laser assembly (Contact us for ordering information.) 1. Turn off the instrument power, unplug the power cable from the power source, and remove any currently installed lasers. 2. Use a Philips screwdriver to remove the laser connector cover from the back of the instrument.

Attach and balance the laser assembly. 3. Position the laser assembly on the back of the instrument, and then insert and loosely tighten two 5/32 hex screws below the laser tube and one screw above. Lift the left side of the laser assembly so that the weight is resting evenly on the bottom screws. Tighten the bottom screws then the top screw.

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NOTICE Do not touch the mirror optics when you install the mirror cover. 4. Place the mirror cover over the mirror optics. Insert and tighten the three 5/32 hex screws.

5. Connect the power and data cables to their connectors on the rear panel.

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NOTICE Make sure no cables are pinched when you install the laser and power supply covers. 6. Use six Phillips screws to install the laser cover and the power supply cover.

7. Install the 633 nm laser sled, filter, and grating, and position the foam gasket. The gasket goes between the laser sled and the 633 nm laser assembly. Make sure the laser path is not blocked.

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Using a DXR SmartRaman Service

8. Turn on the power. Plug the power cable into the power source, turn off the instrument power, and then go to the Bench tab in the Experiment Setup dialog box and turn on the 633 laser. 9. Align and calibrate the instrument. For instructions, please see the alignment and calibration topics in the on-line software help. If the alignment is successful, you can begin collecting samples. If it fails, proceed to the next step. 10. Align the 633 nm laser: See Alignment at Installation for a 633 nm Laser on a DXR SmartRaman for instructions on aligning the laser on a DXR SmartRaman. See Alignment at Installation for a 633 nm Laser on a DXR Raman Microscope for instructions on aligning the laser on a DXR Raman Microscope.

Service Cleaning Your Instrument If the outside of the instrument needs cleaning, turn off the power, unplug the power cable from the wall outlet, or power strip, and wipe the outside of the instrument with a damp (not wet), soft cloth and a mild soap. (Do not use harsh detergents, solvents, chemicals or abrasives.)

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WARNING Avoid shock hazard. Do not allow liquid or any moist material to come in contact with the power supply or the inside of the instrument.

Replacing Fuses You cannot replace the fuses in your instrument. If you suspect a fuse needs to be replaced, contact our sales or service representative in your area or visit our web site at www.thermo.com/spectroscopy for assistance.

Alignment at Installation for a 633 nm Laser on a DXR SmartRaman This service procedure shows how to align a 633 nm laser on a DXR SmartRaman at installation. This alignment should be performed if the instrument auto alignment fails after the laser is installed. Once you have successfully aligned a 633 nm laser on a system, you do not have to align it again. If you have any questions or concerns, please contact us. WARNING This procedure requires you to defeat a laser safety interlock on your system, which makes the instrument a class IIIb laser product. Making adjustments, using controls, or performing procedures that are not specified in the printed or on-line documentation may result in exposure to hazardous visible or invisible laser radiation. Make sure you follow all safety precautions listed in the Safety section of this help system before you operate a class IIIb laser product. To avoid severe burns from exposure to laser radiation or permanent damage to your eyes, always wear laser safety goggles that meet the specifications for the laser your system uses. Also, you should never look directly into a laser, even if you are wearing laser safety goggles. The goggles will protect you for diffuse viewing only. Always set up laser safety area in the location where you are using a class IIIb system configuration. Time needed: Approximately 15 minutes Tools needed: 3/32 and 5/64 inch hex wrenches, 633 nm laser safety goggles Parts needed: A sheet of light colored paper Note After you turn on the 633 nm laser, you must wait 30 minutes for the laser to stabilize before you perform this procedure. 1. Align and calibrate the instrument.

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For instructions, please see the alignment and calibration topics in the on-line software help. If the alignment is successful, no further alignment is needed and you can begin collecting samples. If not, proceed to the next step. 2. Install the SmartRaman alignment tool, and then use a 3/32 hex wrench to remove the alignment tool cover.

3. Open the Alignment tab in the Experiment Setup dialog box in OMNIC. Choose Align Laser Using Raman Signal and set both Side to Side and Up/Down to 332. 4. Open the Bench tab. Set Laser Power to 1 mW and the Accessory Position to Polystyrene. 5. Place a piece of light colored paper behind the alignment tool pinhole. A halo will appear on the paper. If the red laser dot is centered vertically in the halo, no further adjustment is needed. If not, proceed to the next step.

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6. Place a 5/64 hex wrench in the alignment screw. The alignment screw is accessed through the hole in the bottom of the 633 nm laser mirror cover.

7. Rotate the alignment screw about 1/8 turn (clockwise or counter-clockwise) to make an adjustment. Continue turning the screw in 1/8 turn increments until the red laser dot is centered vertically in the halo.

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Using a DXR SmartRaman Safety

WARNING Your instrument is a class IIIb laser product until you have replaced the alignment tool cover.

8. Reinstall the alignment tool cover, and then align and calibrate the instrument. For instructions, please see the alignment and calibration topics in the on-line software help. If the alignment is successful, you can begin collecting samples. If it fails, contact us for assistance.

Safety Safety Precautions The United States Department of Health and Human Services warns against improper laser use, as follows: WARNING Class IIIb instruments should always be operated in a laser safety area. All persons using or in the vicinity of a Class IIIb instruments should wear appropriate laser safety goggles and should be aware of the potential hazards. Use of controls or adjustments or performance of procedures other than those specified in your printed and on-line documentation may result in hazardous radiation exposure. Do not alter or attempt to remove the laser head from its protective housing or attempt to remove the shields that surround the laser head. Exposure to laser energy and high voltage may result. The laser energy from the excitation lasers may be visible or invisible. Never stare directly into the laser beam or at its bright reflection. Never tamper with the laser head. Exposure to laser light or high voltage may result. Avoid skin and eye contact with the invisible laser radiation produced by the excitation laser beam and any reflections of that beam. If you wish to observe trained service personnel, wear properly rated laser safety goggles whenever the instrument power is on and the protective covers are open or removed. When operating our Raman instruments, use only accessories and equipment (such as power supplies and lasers) supplied by us. Use of equipment and accessories not supplied by us can result in permanent damage to the instrument and may create a safety hazard. Do not attempt to service a laser that is not functioning properly. If a laser is malfunctioning, contact our sales or service representative in your area or visit our web site at www.thermo.com/spectroscopy for assistance or to order a replacement laser.

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NOTICE The power connector and the USB stage and computer connectors are located on the panel on the bottom left side of the instrument (as you face the instrument). The connections to these connectors are made by our service representative during the instrument installation. Do not attempt to alter or modify the connections to these connectors. Note See the "Manufacturer’s laser information" section in the safety notice that was included with your instrument for information about individual excitation lasers.

Safety Goggle Specifications WARNING Always wear safety goggles that meet the specifications listed below for your laser(s) whenever the instrument power is on and the protective covers are open or removed. Also, you should never stare directly into a laser beam or its reflection, even if you are wearing laser safety goggles. The goggles will protect you for diffuse viewing only. 780 nm NIR diode laser: Wear goggles that have an optical density of at least 3 and are rated for wavelengths of 780 nm. 633 nm red laser: Wear goggles that have an optical density of at least 2.5 and are rated for wavelengths of 633 nm. 532 nm green laser: Wear goggles that have an optical density of at least 3 and are rated for wavelengths of 532 nm. 455 nm blue laser: Wear goggles that have an optical density of at least 3 and are rated for wavelengths of 455 nm.

Setting up a Laser Safety Area If you are going to use a class IIIb laser product (such as the fiber optic accessory or the class IIIb configuration of the microscope), the instrument must be connected to an external remote interlock system that blocks the laser beam whenever a safety perimeter around the instrument is breached (when an unauthorized person opens the door, for example). The maximum permissible exposure (MPE) is the level of laser radiation that a person may be exposed to, under normal circumstances, without suffering adverse effects. (These levels are based on the assumption that a person is exposed to the laser beam for an infinite length of time.) The nominal ocular hazard distance (NOHD) is the distance from the laser output aperture within which the level of laser radiation exceeds the MPE. This table shows the MPE and NOHD values for fiber optic probes with an aperture of 0.22.

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Laser




455 nm

10.0

0.34

0.50

532 nm

10.0

0.28

0.41

633 nm

10.0

0.26

0.38

780 nm

14.4

0.38

0.56


0.93

1.37

WARNING To avoid injury, the connectors and the laser safety circuit must be designed and built by someone who is properly trained. One of our representatives will help you install and test your connector. Please have the connector ready before the system arrives. All persons using or in the vicinity of a Class IIIb instrument must wear appropriate laser safety goggles and must be aware of the safety precautions. The remote interlock system protects all people in the vicinity of the class IIIb laser system. Do not attempt to defeat the interlocks on the system. Time needed: Approximately 5 minutes Parts needed: 2 BNC cables 1. Install a switch across the pins of the connectors on each of the BNC cables. (The switch must accommodate +5 VDC at 10 mA while it is closed.)

Note Opening the switch blocks the laser beam, and closing the switch unblocks the beam. 2. Connect the BNC cables to the BNC connectors on the instrument power panel.

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3. Connect the BNC cables to the laser safety circuit you have designed.

Safety and Electrical Symbols The following safety and electrical symbols may be used on this product: Symbol

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Description

Indication

Black graphical symbol inside a yellow triangle with a black triangular band.

This is a warning symbol. The graphic in this symbol is used to alert the user to potential hazards.

Black graphical symbol inside a red circular band with a red diagonal bar.

This is a prohibition symbol. The graphic in this symbol is used to alert the user to actions that shall not be taken or shall be stopped.

White graphical symbol inside a blue circle.

This is a mandatory action symbol. It is used to indicate that an action shall be taken to avoid a hazard.

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Symbol


Description

Indication


This is the general warning sign. Failure to heed the safety precautions could result in personal injury.


This is the general data loss or property damage symbol and is not related to personal injury. Failure to heed these precautions can result in irreparable damage to property or permanent data loss.

Indicators

Note Press the OK button to respond affirmatively (for example, to a software prompt) during data collection. Press the Go button to start a macro you have specified.

WEEE Compliance Many instruments are required to comply with the European Union’s Waste Electrical & Electronic Equipment (WEEE) Directive 2002/96/EC. If compliance is required, the instrument is marked with the following symbol:

We have contracted with one or more recycling/disposal companies in each EU Member State, and this product should be disposed of or recycled through them. Further information on our compliance with these directives, the recyclers in your country, and information on our products which may assist the detection of substances subject to the RoHS Directive are available at:

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www.thermo.com/WEEERoHS

Biohazards or Radioactive Materials and Infectious Agents Instruments, accessories, components or other associated materials may not be returned to us or other accessory manufacturers if they are contaminated with biohazard or radioactive materials, infectious agents, or any other materials and/or conditions that could constitute a health or injury hazard to employees. If you have questions about decontamination requirements, contact our sales or service representative in your area or visit our web site at www.thermo.com/spectroscopy.

Cooling Fans NOTICE Cooling fans are located on the back of the instrument. To avoid overheating, do not block the free flow of air around the instrument. There should be at least 2 cm (about 1 in) of clearance behind the instrument and at least 30 cm (about 12 in) of clearance on each side.

Using Corrosives and Solvents Many standard spectroscopy methods are based on the use of solvents. Sample materials dissolved in solvents can be measured using your spectrometer, but special precautions must be taken.

Caustic or Corrosive Agents Instrument components may be degraded by exposure to caustic or corrosive agents or their vapors. To maintain the instrument in safe working condition, do not use caustic agents. Damage to the instrument caused by the use of caustic agents is not covered by the warranty.

Volatile Solvents If you use volatile solvents regularly, follow the guidelines listed below. These measures will help prolong the life of your instrument and will eliminate the possibility of spectral interference caused by volatile solvent vapors. • Use sealed sample holders. • Do not leave exposed solvent in the sample compartment for longer than necessary. • Do not leave the solvents near the instrument. • Be sure that your work space is properly ventilated.

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Solvents Containing Halogenated Hydrocarbons Chlorinated solvents, perfluorochlorinated solvents, and other solvents containing halogenated hydrocarbons are often used as sample solvents. The pyrolysis of these solvents by an infrared source or by excessive heating caused by laser absorption may produce hydrochloric acid (HCl), hydrofluoric acid (HF), phosgene (COCl2), or other hazardous compounds. Materials such as hydrochloric acid and hydrofluoric acid are highly corrosive and may cause accelerated corrosion of the metallic components in the spectrometer. Damage may be caused in any spectrometer, if the concentration level of corrosive gasses in the air is excessively high due to improper sampling techniques. WARNING Materials such as hydrochloric acid, hydrofluoric acid and phosgene are highly toxic. If you regularly use solvents containing halogenated hydrocarbons, be sure your work area is properly ventilated. Solvents containing halogenated hydrocarbons should not be left in the sample compartment for an extended time.

Spectrometer Safety Labels

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Using a DXR SmartRaman Troubleshooting

Troubleshooting Sample Bands are too Small The Raman signal is too small. You can increase it by doing one or more of the following: • Increase the setting of Exposure Time on the Collect tab. • Increase the setting of Exposures on the Collect tab. • Increase the aperture size by setting Aperture on the Bench tab. • Select a slit aperture instead of a pinhole by setting Aperture on the Bench tab. • Increase the setting of Laser Power on the Bench tab .

Note All of the tabs mentioned here are in the Experiment Setup dialog box. If this problem persists, contact our sales or service representative in your area, or visit our web site at www.thermo.com/spectroscopy.

Sample Bands Are too Large The Raman signal is too large, which saturates the CCD. You can decrease the signal by doing one or more of the following: • Decrease the setting of Exposure Time on the Collect tab. • Decrease the aperture size by setting Aperture on the Bench tab. • Select a pinhole aperture instead of a slit by setting Aperture on the Bench tab. • Decrease the setting of Laser Power on the Bench tab. Note All of the tabs mentioned here are in the Experiment Setup dialog box.

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If this problem persists, contact our sales or service representative in your area, or visit our web site at www.thermo.com/spectroscopy.

No Raman Signal Appears in the Live Display 1. If you have a spectrometer and an accessory sample compartment door is open, close it. 2. If you have a microscope and the microscope compartment is open, close it. 3. If the instrument is turned off, turn it on. 4. If the laser power is off, turn on the laser. 5. If the laser is disabled, enable it in the Bench tab of the Experiment Setup dialog box. If this problem persists, contact our sales or service representative in your area, or visit our web site at www.thermo.com/spectroscopy.

CCD Overflow Occurred Too much light hit the CCD. To correct this problem, try either of the following: • Use a shorter exposure time or smaller aperture. • Reduce the laser power. If this problem persists, contact our sales or service representative in your area, or visit our web site at www.thermo.com/spectroscopy.

The Spectrum Has No Sample Bands 1. If the sample is not at the focal point, focus the sample on the microscope stage. 2. If you have a spectrometer and an accessory sample compartment door is open, close it. 3. If you have a microscope and the microscope compartment is open, close it. 4. If the laser power is off, turn on the laser. 5. If the laser is disabled, enable it in the Bench tab of the Experiment Setup dialog box. If this problem persists, contact our sales or service representative in your area, or visit our web site at www.thermo.com/spectroscopy.

The Spectrum Has Large Noise Spikes Cosmic ray events occurred during data collection. Turn on Cosmic Ray Rejection and set it to Medium. (Cosmic Ray Rejection is on the Collect tab of the Experiment Setup dialog box.)

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If this problem persists, contact our sales or service representative in your area, or visit our web site at www.thermo.com/spectroscopy.

The Spectrum Has a Sloping Background The sample may be fluorescing or heating. To account for this condition try one or more of the following: • Correct the baseline to subtract the broad background. • Use a different laser. Shorter wavelengths heat samples less. • If the sample looks burned, replace it or move it so the laser will strike a fresh area. • Reduce the laser power and collect the sample again. Watch the live display to see if the sample is still heating. (Reducing the laser power reduces the Raman signal generated at the sample and therefore the quality of the data. To compensate, try increasing the number of exposures or the exposure time.) If this problem persists, contact our sales or service representative in your area, or visit our web site at www.thermo.com/spectroscopy.

The Spectrum Baseline Is Severely Tilted or Curved The sample fluoresced during data collection. To correct this problem, try one or more of the following: • Purify the sample. • Make sure the sample container is not responsible for the fluorescence. • If fluorescence is an inherent property of the sample, correct the baseline to subtract the broad background. • Use a longer wavelength laser or expose the sample to the laser beam for a period of time before beginning the collection of the sample spectrum (this is known as “photobleaching”). On the Collect tab of the Experiment Setup dialog box, turn on Preview Data Collection and type the desired exposure time in the Preview Time text box. If this problem persists, contact our sales or service representative in your area, or visit our web site at www.thermo.com/spectroscopy.

The Spectrum Baseline Has a Severe Positive Offset The sample is heating. To account for this condition try one or more of the following: • Correct the baseline to subtract the broad background. • Use a different laser. Shorter wavelengths heat samples less.

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• If the sample looks burned, replace it or move it so the laser will strike a fresh area. • Reduce the laser power and collect the sample again. Watch the live display to see if the sample is still heating. (Reducing the laser power reduces the Raman signal generated at the sample and therefore the quality of the data. To compensate, try increasing the number of exposures or the exposure time.) If this problem persists, contact our sales or service representative in your area, or visit our web site at If this problem persists, contact our sales or service representative in your area, or visit our web site at www.thermo.com/spectroscopy.

The Spectrum Baseline Is Severely Shifted No background was subtracted from the sample data (the number of background exposures is set to zero or the Smart Background feature is disabled). The offset is the detector bias and dark signal. Set Background Exposures on the Collect tab of the Experiment Setup dialog box to an integer greater than 0. If this problem persists, contact our sales or service representative in your area, or visit our web site at If this problem persists, contact our sales or service representative in your area, or visit our web site at www.thermo.com/spectroscopy.

A Grating Does Not Appear to Be Installed or the Grating Cover Is Open 1. Make sure a grating is installed. 2. Make sure the grating cover is closed. 3. Exit OMNIC™, shut down the computer, turn off the instrument, wait 30 seconds, and then turn on the instrument. If this problem persists, contact our sales or service representative in your area, or visit our web site at www.thermo.com/spectroscopy.

A Laser Does Not Appear to Be Installed 1. Make sure a laser is installed and the keyswitch is turned on. 2. Exit OMNIC™, shut down the computer, turn off the instrument, wait 30 seconds, and then turn on the instrument. If this problem persists, contact our sales or service representative in your area, or visit our web site at www.thermo.com/spectroscopy.

A Filter or Fiber Optic Accessory Does Not Appear to Be Installed 1. Make sure a filter or fiber optic accessory is installed.

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2. Exit OMNIC™, shut down the computer, turn off the instrument, wait 30 seconds, and then turn on the instrument. If this problem persists, contact our sales or service representative in your area, or visit our web site at www.thermo.com/spectroscopy.

The Computer Cannot Communicate with the Instrument 1. If the instrument is turned off, turn it on. 2. Check the cable between the computer and the instrument. If it is disconnected, connect it. 3. If the front panel indicators are not on, make sure the instrument is plugged in. If this problem persists, contact our sales or service representative in your area, or visit our web site at www.thermo.com/spectroscopy.

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Using a DXR Raman Microscope Operation Adjusting the Illuminator Intensity

Note If you have a darkfield illuminator or a transmission illuminator, the intensity adjustment control is located on the front of the illuminator power supply.

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Using a DXR Raman Microscope Operation

Positioning a Manual Stage

Positioning a Motorized Stage The joystick moves the motorized stage left and right along the X-axis or forward and back along the Y-axis. The focus knob allows you to adjust the height of the stage along the Z-axis.

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Using Darkfield Illumination Darkfield illumination switches the illumination from the top of a sample to the sides. This increases the contrast and makes it easier to view low contrast samples. To use darkfield illumination, a different illuminator, nosepiece, and objective must be installed. In addition, you must set the Objective parameter on the Bench tab of the Experiment Setup dialog box to the objective you have installed. For assistance or ordering information, contact our sales or service representative in your area or visit our web site at www.thermo.com/spectroscopy for more information.

Using Confocal Operation Confocal operation provides a well defined focus that is useful when examining layered materials or very small samples. To make maximum use of your microscope’s confocal capability, open the Experiment Setup dialog box in OMNIC™, click the Bench tab, and set Aperture to 25 micrometer pinhole.

Changing the Laser, Filter, and Grating WARNING Avoid shock hazard. Make sure you turn off the spectrometer power before you replace a laser, filter, or grating.

NOTICE Handle lasers, filters, and gratings gently. Do not touch any optical surfaces or the interior of a laser, filter, or grating. When a laser, filter, or grating is not in use, store it in the case that it was shipped in.

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Enabling the Laser You must enable the laser before you can turn it on. To enable the laser, rotate the laser key to the locked (vertical) position as shown below. (For more information about turning on the laser, see the software help available through the Help menu in OMNIC.) Note You can insert or remove the laser key only when the laser keyswitch is in the unlocked (horizontal) position. When the laser keyswitch is in the unlocked position, the laser is disabled.

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Using a Class IIIb Microscope WARNING If your microscope has a fiber optic accessory installed and/or it does not have covers, it is a class IIIb laser product. Making adjustments, using controls, or performing procedures that are not specified in the printed or on-line documentation may result in exposure to hazardous visible or invisible laser radiation. Make sure you follow all safety precautions listed in the Safety section of this help system before you operate a class IIIb laser product. To avoid severe burns from exposure to laser radiation or permanent damage to your eyes, always wear laser safety goggles that meet the specifications for the laser your microscope uses. Also, you should never look directly into a laser, even if you are wearing laser safety goggles. The goggles will protect you for diffuse viewing only. Always set up laser safety area in the location where you are using a class IIIb microscope configuration.

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Using a Class IIIb Fiber Optic Accessory WARNING The fiber optic accessory is a class IIIb laser product. Making adjustments, using controls, or performing procedures that are not specified in the printed or on-line documentation may result in exposure to hazardous visible or invisible laser radiation. Make sure you follow all safety precautions listed in the Safety section of this help system before you install the fiber optic accessory. To avoid severe burns from exposure to laser radiation or permanent damage to your eyes, never put anything except samples against the tip of the fiber optic probe, and always wear laser safety goggles that meet the specifications for the laser your fiber optic launcher uses. Also, you should never look directly into the tip of a fiber optic probe or the fiber optic probe connectors, even if you are wearing laser safety goggles. The goggles will protect you for diffuse viewing only. Always set up laser safety area in the location where you are using a fiber optic accessory.  To install a fiber optic accessory

1. Slide the accessory into the instrument and connect the fiber optic cables from the probe.

2. Connect the power cable for the probe LED.

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The maximum permissible exposure (MPE) is the level of laser radiation that a person may be exposed to, under normal circumstances, without suffering adverse effects. (These levels are based on the assumption that a person is exposed to the laser beam for an infinite length of time.) The nominal ocular hazard distance (NOHD) is the distance from the laser output aperture within which the level of laser radiation exceeds the MPE. This table shows the MPE and NOHD values for fiber optic probes with an aperture of 0.22.

Laser



NOHD Microscope 10x Objective* (m)

NOHD Microscope no objective* (m)


455 nm

10.0

0.34

0.30

55.45

0.50

532 nm

10.0

0.28

0.25

59.92

0.41

633 nm

10.0

0.26

0.23

85.92

0.38

780 nm

14.4

0.38

0.34

73.92

0.56


0.93

0.82

22.77

1.37

* These values are for a microscope that is operated without the Class I laser safety enclosure.

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Installing the Microscope Alignment Tool

Note For alignment and calibration instructions, please see the alignment and calibration topics in the on-line software help system.

Installing a 455 nm Laser Under most circumstances, your instrument has come equipped to permit user installation of a 455 nm laser. If you specifically ordered this laser wavelength with your DXR, see Changing the Laser, Filter, and Grating. If you need to add this capability in the future, a service visit may be required. Contact our sales or service representative in your area or contact us.

Installing a 633 nm Laser This procedure shows how to install a 633 nm laser. If you have any questions or concerns, please contact us. Time needed: Approximately 1 hour Tools needed: 5/32 inch hex wrench, Philips screwdriver Parts needed: 633 nm HeNe laser assembly (Contact us for ordering information.) 1. Turn off the instrument power, unplug the power cable from the power source, and remove any currently installed lasers.

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2. Use a Philips screwdriver to remove the laser connector cover from the back of the instrument.

3. Attach and balance the laser assembly. Position the laser assembly on the back of the instrument, and then insert and loosely tighten two 5/32 hex screws below the laser tube and one screw above. Lift the left side of the laser assembly so that the weight is resting evenly on the bottom screws. Tighten the bottom screws then the top screw.

NOTICE Do not touch the mirror optics when you install the mirror cover. 4. Place the mirror cover over the mirror optics. Insert and tighten the three 5/32 hex screws.

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5. Connect the power and data cables to their connectors on the rear panel.

NOTICE Make sure no cables are pinched when you install the laser and power supply covers. 6. Use six Phillips screws to install the laser cover and the power supply cover.

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7. Install the 633 nm laser sled, filter, and grating, and position the foam gasket. The gasket goes between the laser sled and the 633 nm laser assembly. Make sure the laser path is not blocked.

8. Turn on the power. Plug the power cable into the power source, turn off the instrument power, and then go to the Bench tab in the Experiment Setup dialog box and turn on the 633 laser. 9. Align and calibrate the instrument. For instructions, please see the alignment and calibration topics in the on-line software help. If the alignment is successful, you can begin collecting samples. If it fails, proceed to the next step.

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Using a DXR Raman Microscope Service

10. Align the 633 nm laser: See Alignment at Installation for a 633 nm Laser on a DXR SmartRaman for instructions on aligning the laser on a DXR SmartRaman. See Alignment at Installation for a 633 nm Laser on a DXR Raman Microscope for instructions on aligning the laser on a DXR Raman Microscope.

Service Cleaning Your Instrument If the outside of the instrument needs cleaning, turn off the power, unplug the power cable from the wall outlet, or power strip, and wipe the outside of the instrument with a damp (not wet), soft cloth and a mild soap. (Do not use harsh detergents, solvents, chemicals or abrasives.)

WARNING Avoid shock hazard. Do not allow liquid or any moist material to come in contact with the power supply or the inside of the instrument.

NOTICE Be extremely careful when cleaning the microscope objectives. They are delicate optical components. If an objective needs to be cleaned, use pressurized, filtered nitrogen or air to blow off dust and other particles. (Commercially prepared cleaning air like the kind used to clean electronic equipment also may be used.) If this is not sufficient, use commercial cleaning solution and lens paper that is specifically for cleaning delicate glass lenses. To help avoid permanent damage, do not attempt to clean or touch any optical surface inside the instrument (except the microscope objectives as described above), and do not attempt to clean a filter or grating.

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Replacing the Nosepiece

Note When you install a nosepiece, make sure you slide it in until it stops, and then tighten the screw until it is just tight. Do not over tighten. When you install a new nosepiece, you must set the Objective parameter on the Bench tab of the Experiment Setup dialog box to the new objective you will be using. For assistance or ordering information, contact our sales or service representative in your area or visit our web site at www.thermo.com/spectroscopy for more information.

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Removing the Stage

Installing a New Stage If you want to install a new stage on your microscope, please contact our sales or service representative in your area or visit our web site at www.thermo.com/spectroscopy for assistance.

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Replacing Fuses You cannot replace the fuses in your instrument. If you suspect a fuse needs to be replaced, contact our sales or service representative in your area or visit our web site at www.thermo.com/spectroscopy for assistance.

Replacing an Illuminator Bulb The following procedure shows how to replace a darkfield illuminator bulb. If you have a brightfield illuminator or transmission illuminator, the bulb is an LED and should not fail during the lifetime of the instrument. If you suspect a brightfield or transmission illuminator needs to be replaced, or if there is a problem with the illuminator, contact us. Time needed: Approximately 10 minutes Tools needed: A 3.0 mm hex wrench Parts needed: Replacement illuminator bulbs (Contact us for ordering information.) WARNING To avoid fire hazard, make sure your replacement illuminator bulbs are supplied by us and are appropriate for your instrument and illuminator. Always turn off the instrument power and unplug the power cable from the power source before replacing an illuminator bulb. 1. Turn off the instrument power and unplug the power cable from the power source. Caution To avoid being burned, let the illuminator cool for at least five minutes before replacing the bulb. 2. Use a 3.0 mm hex wrench to loosen, but not remove, the screw.

3. Lift the cover off.

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CAUTION Avoid burn hazard. Make sure the bulb is cool before removing it.

4. Squeeze the levers to release the bulb.

WARNING To avoid fire hazard, make sure your replacement illuminator bulbs are supplied by us and are appropriate for your instrument and illuminator.

5. Squeeze the levers, insert the bulb all the way, and release the levers. (To extend bulb life, always handle a new bulb with a clean tissue or cloth.)

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6. Replace the cover.

7. Use a 3.0 mm hex wrench to tighten the screw. (Do not over tighten.)

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8. Connect the instrument power cable to a power source (an electrical outlet or power strip, for example), and then turn on the instrument power.

Alignment at Installation for a 633 nm Laser on a DXR Raman Microscope This service procedure shows how to align a 633 nm laser on a DXR Raman Microscope at installation. This alignment should be performed if the instrument auto alignment fails after the laser is installed. Once you have successfully aligned a 633 nm laser on a system, you do not have to align it again. If you have any questions or concerns, please contact us. WARNING This procedure requires you to defeat a laser safety interlock on your microscope, which makes the instrument a class IIIb laser product. Making adjustments, using controls, or performing procedures that are not specified in the printed or on-line documentation may result in exposure to hazardous visible or invisible laser radiation. Make sure you follow all safety precautions listed in the Safety section of this help system before you operate a class IIIb laser product. To avoid severe burns from exposure to laser radiation or permanent damage to your eyes, always wear laser safety goggles that meet the specifications for the laser your microscope uses. Also, you should never look directly into a laser, even if you are wearing laser safety goggles. The goggles will protect you for diffuse viewing only. Always set up laser safety area in the location where you are using a class IIIb microscope configuration Time needed: Approximately 15 minutes Tools needed: 5/32 hex wrench, 5/64 inch hex wrench, Philips screwdriver, 633 nm laser safety goggles Parts needed: A sheet of white paper

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Note After you turn on the 633 nm laser, you must wait 30 minutes for the laser to stabilize before you perform this procedure. 1. Align and calibrate the instrument. For instructions, please see the alignment and calibration topics in the on-line software help. If the alignment is successful, no further alignment is needed and you can begin collecting samples. If not, proceed to the next step. 2. Plug in the DXR Raman Microscope alignment tool, but do not place it on the microscope stage. Note If you have a magnet or a spare grating, you can use that instead of the magnet from the microscope compartment cover, and you can skip the following step. 3. Open one side of the microscope compartment and use a Philips screwdriver to remove the magnet from the compartment cover. Save the magnet screws—you will need them when you reinstall the magnet.

Front side of magnet

Back side of magnet

4. Place the magnet (or a spare grating) on a safety interlock in the microscope compartment.

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5. Install a 10X objective in the microscope nosepiece and place a sheet of paper on the stage. 6. Open the Alignment tab in the Experiment Setup dialog box in OMNIC. Choose Align Laser Using Raman Signal and set both Side to Side and Up/Down to 332. 7. Look at the objective halo on the paper. Do not look through the eyepiece. If the red laser dot is centered vertically in the halo, no further adjustment is needed. If not, proceed to the next step. 8. Place a 5/64 hex wrench in the alignment screw. The alignment screw is accessed through the hole in the bottom of the 633 nm laser mirror cover.

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9. Rotate the alignment screw about 1/8 turn (clockwise or counter-clockwise) to make an adjustment. Continue turning the screw in 1/8 turn increments until the red laser dot is centered vertically in the objective halo.

WARNING Your instrument is a class IIIb laser product until you have enabled the laser safety interlocks and checked to make sure they operate properly.

10. Enable and test the microscope compartment laser safety interlocks. Reinstall the magnet you removed from the microscope compartment cover in step 2. When this is done, test the interlocks by checking the Laser At Sample indicator —it should turn on when you close the microscope compartment cover and turn off when you open the cover. If it does not, turn off the instrument power and contact us for assistance. Do not attempt to use the instrument. 11. Align and calibrate the instrument. For instructions, please see the alignment and calibration topics in the on-line software help. If the alignment is successful, you can begin collecting samples. If it fails, contact us for assistance.

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Using a DXR Raman Microscope Safety

Safety Safety Precautions The United States Department of Health and Human Services warns against improper laser use, as follows: WARNING Class IIIb instruments should always be operated in a laser safety area. All persons using or in the vicinity of a Class IIIb instruments should wear appropriate laser safety goggles and should be aware of the potential hazards. Use of controls or adjustments or performance of procedures other than those specified in your printed and on-line documentation may result in hazardous radiation exposure. Do not alter or attempt to remove the laser head from its protective housing or attempt to remove the shields that surround the laser head. Exposure to laser energy and high voltage may result. The laser energy from the excitation lasers may be visible or invisible. Never stare directly into the laser beam or at its bright reflection. Never tamper with the laser head. Exposure to laser light or high voltage may result. Avoid skin and eye contact with the invisible laser radiation produced by the excitation laser beam and any reflections of that beam. If you wish to observe trained service personnel, wear properly rated laser safety goggles whenever the instrument power is on and the protective covers are open or removed. When operating our Raman instruments, use only accessories and equipment (such as power supplies and lasers) supplied by us. Use of equipment and accessories not supplied by us can result in permanent damage to the instrument and may create a safety hazard. Do not attempt to service a laser that is not functioning properly. If a laser is malfunctioning, contact our sales or service representative in your area or visit our web site at www.thermo.com/spectroscopy for assistance or to order a replacement laser. NOTICE The power connector and the USB stage and computer connectors are located on the panel on the bottom left side of the instrument (as you face the instrument). The connections to these connectors are made by our service representative during the instrument installation. Do not attempt to alter or modify the connections to these connectors. Note See the “Manufacturer’s laser information” section in the safety notice that was included with your instrument for information about individual excitation lasers.

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Safety Goggle Specifications WARNING Always wear safety goggles that meet the specifications listed below for your laser(s) whenever the instrument power is on and the protective covers are open or removed. Also, you should never stare directly into a laser beam or its reflection, even if you are wearing laser safety goggles. The goggles will protect you for diffuse viewing only. 780 nm NIR diode laser: Wear goggles that have an optical density of at least 3 and are rated for wavelengths of 780 nm. 633 nm red laser: Wear goggles that have an optical density of at least 2.5 and are rated for wavelengths of 633 nm. 532 nm green laser: Wear goggles that have an optical density of at least 3 and are rated for wavelengths of 532 nm. 455 nm blue laser: Wear goggles that have an optical density of at least 3 and are rated for wavelengths of 455 nm.

Setting up a Laser Safety Area If you are going to use a class IIIb laser product (such as the fiber optic accessory or the class IIIb configuration of the microscope), the instrument must be connected to an external remote interlock system that blocks the laser beam whenever a safety perimeter around the instrument is breached (when an unauthorized person opens the door, for example). The maximum permissible exposure (MPE) is the level of laser radiation that a person may be exposed to, under normal circumstances, without suffering adverse effects. (These levels are based on the assumption that a person is exposed to the laser beam for an infinite length of time.) The nominal ocular hazard distance (NOHD) is the distance from the laser output aperture within which the level of laser radiation exceeds the MPE. This table shows the MPE and NOHD values for fiber optic probes with an aperture of 0.22.

Laser



NOHD Microscope 10x Objective* (m)

NOHD Microscope no objective* (m)


455 nm

10.0

0.34

0.30

55.45

0.50

532 nm

10.0

0.28

0.25

59.92

0.41

633 nm

10.0

0.26

0.23

85.92

0.38

780 nm

14.4

0.38

0.34

73.92

0.56


0.93

0.82

22.77

1.37

* These values are for a microscope that is operated without the Class I laser safety enclosure

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WARNING To avoid injury, the connectors and the laser safety circuit must be designed and built by someone who is properly trained. One of our representatives will help you install and test your connector. Please have the connector ready before the system arrives. All persons using or in the vicinity of a Class IIIb instrument must wear appropriate laser safety goggles and must be aware of the safety precautions. The remote interlock system protects all people in the vicinity of the class IIIb laser system. Do not attempt to defeat the interlocks on the system. Time needed: Approximately 5 minutes Parts needed: 2 BNC cables 1. Install a switch across the pins of the connectors on each of the BNC cables. (The switch must accommodate +5 VDC at 10 mA while it is closed.)

Note Opening the switch blocks the laser beam, and closing the switch unblocks the beam. 2. Connect the BNC cables to the BNC connectors on the instrument power panel.

3. Connect the BNC cables to the laser safety circuit you have designed.

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Safety and Electrical Symbols The following safety and electrical symbols may be used on this product: Symbol

Description

Indication


This is a warning symbol. The graphic in this symbol is used to alert the user to potential hazards.

Black graphical symbol inside a red circular band with a red diagonal bar.

This is a prohibition symbol. The graphic in this symbol is used to alert the user to actions that shall not be taken or shall be stopped.


This is a mandatory action symbol. It is used to indicate that an action shall be taken to avoid a hazard.


This is the general warning sign. Failure to heed the safety precautions could result in personal injury.


This is the general data loss or property damage symbol and is not related to personal injury. Failure to heed these precautions can result in irreparable damage to property or permanent data loss.

Indicators

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Note Press the OK button to respond affirmatively (for example, to a software prompt) during data collection. Press the Go button to start a macro you have specified.

WEEE Compliance Many instruments are required to comply with the European Union’s Waste Electrical & Electronic Equipment (WEEE) Directive 2002/96/EC. If compliance is required, the instrument is marked with the following symbol:

We have contracted with one or more recycling/disposal companies in each EU Member State, and this product should be disposed of or recycled through them. Further information on our compliance with these directives, the recyclers in your country, and information on our products which may assist the detection of substances subject to the RoHS Directive are available at available at: www.thermo.com/WEEERoHS

Biohazards or Radioactive Materials and Infectious Agents Instruments, accessories, components or other associated materials may not be returned to us or other accessory manufacturers if they are contaminated with biohazard or radioactive materials, infectious agents, or any other materials and/or conditions that could constitute a health or injury hazard to employees. If you have questions about decontamination requirements, contact our sales or service representative in your area or visit our web site at www.thermo.com/spectroscopy.

Cooling Fans NOTICE Cooling fans are located on the back of the instrument. To avoid overheating, do not block the free flow of air around the instrument. There should be at least 2 cm (about 1 in) of clearance behind the instrument and at least 30 cm (about 12 in) of clearance on each side.

Using Corrosives and Solvents Many standard spectroscopy methods are based on the use of solvents. Sample materials dissolved in solvents can be measured using your spectrometer, but special precautions must be taken.

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Caustic or Corrosive Agents Instrument components may be degraded by exposure to caustic or corrosive agents or their vapors. To maintain the instrument in safe working condition, do not use caustic agents. Damage to the instrument caused by the use of caustic agents is not covered by the warranty.

Volatile Solvents If you use volatile solvents regularly, follow the guidelines listed below. These measures will help prolong the life of your instrument and will eliminate the possibility of spectral interference caused by volatile solvent vapors. • Use sealed sample holders. • Do not leave exposed solvent in the sample compartment for longer than necessary. • Do not leave the solvents near the instrument. • Be sure that your work space is properly ventilated.

Solvents Containing Halogenated Hydrocarbons Chlorinated solvents, perfluorochlorinated solvents, and other solvents containing halogenated hydrocarbons are often used as sample solvents. The pyrolysis of these solvents by an infrared source or by excessive heating caused by laser absorption may produce hydrochloric acid (HCl), hydrofluoric acid (HF), phosgene (COCl2), or other hazardous compounds. Materials such as hydrochloric acid and hydrofluoric acid are highly corrosive and may cause accelerated corrosion of the metallic components in the spectrometer. Damage may be caused in any spectrometer, if the concentration level of corrosive gasses in the air is excessively high due to improper sampling techniques. WARNING Materials such as hydrochloric acid, hydrofluoric acid and phosgene are highly toxic. If you regularly use solvents containing halogenated hydrocarbons, be sure your work area is properly ventilated. Solvents containing halogenated hydrocarbons should not be left in the sample compartment for an extended time.

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Microscope Safety Labels

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Using a DXR Raman Microscope Troubleshooting

Troubleshooting Sample Bands are too Small The Raman signal is too small. You can increase it by doing one or more of the following: • Increase the setting of Exposure Time on the Collect tab. • Increase the setting of Exposures on the Collect tab. • Increase the aperture size by setting Aperture on the Bench tab. • Select a slit aperture instead of a pinhole by setting Aperture on the Bench tab. • Increase the setting of Laser Power on the Bench tab. .

Note All of the tabs mentioned here are in the Experiment Setup dialog box. If this problem persists, contact our sales or service representative in your area, or visit our web site at www.thermo.com/spectroscopy.

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Sample Bands Are too Large The Raman signal is too large, which saturates the CCD. You can decrease the signal by doing one or more of the following: • Decrease the setting of Exposure Time on the Collect tab. • Decrease the aperture size by setting Aperture on the Bench tab. • Select a pinhole aperture instead of a slit by setting Aperture on the Bench tab. • Decrease the setting of Laser Power on the Bench tab. Note All of the tabs mentioned here are in the Experiment Setup dialog box. If this problem persists, contact our sales or service representative in your area, or visit our web site at www.thermo.com/spectroscopy.

No Raman Signal Appears in the Live Display 1. If you have a spectrometer and an accessory sample compartment door is open, close it. 2. If you have a microscope and the microscope compartment is open, close it. 3. If the instrument is turned off, turn it on. 4. If the laser power is off, turn on the laser. 5. If the laser is disabled, enable it in the Bench tab of the Experiment Setup dialog box. If this problem persists, contact our sales or service representative in your area, or visit our web site at www.thermo.com/spectroscopy.

No Visible Image Appears in the Video Pane or Viewer 1. If the illuminator is set to low intensity, set it to higher intensity. 2. If you are in the Bench tab of the Experiment Setup dialog box, go to another tab. 3. If the viewer selection rod is all the way out, move it all the way in or to the center position. If this problem persists, contact our sales or service representative in your area, or visit our web site at www.thermo.com/spectroscopy.

CCD Overflow Occurred Too much light hit the CCD. To correct this problem, try either of the following: • Use a shorter exposure time or smaller aperture.

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• Reduce the laser power. If this problem persists, contact our sales or service representative in your area, or visit our web site at www.thermo.com/spectroscopy.

The Spectrum Has No Sample Bands 1. If the sample is not at the focal point, focus the sample on the microscope stage. 2. If you have a spectrometer and an accessory sample compartment door is open, close it. 3. If you have a microscope and the microscope compartment is open, close it. 4. If the laser power is off, turn on the laser. 5. If the laser is disabled, enable it in the Bench tab of the Experiment Setup dialog box. If this problem persists, contact our sales or service representative in your area, or visit our web site at www.thermo.com/spectroscopy.

The Spectrum Has Large Noise Spikes Cosmic ray events occurred during data collection. Turn on Cosmic Ray Rejection and set it to Medium. (Cosmic Ray Rejection is on the Collect tab of the Experiment Setup dialog box.) If this problem persists, contact our sales or service representative in your area, or visit our web site at www.thermo.com/spectroscopy.

The Spectrum Has a Sloping Background The sample may be fluorescing or heating. To account for this condition try one or more of the following: • Correct the baseline to subtract the broad background. • Use a different laser. Shorter wavelengths heat samples less. • If the sample looks burned, replace it or move it so the laser will strike a fresh area. • Reduce the laser power and collect the sample again. Watch the live display to see if the sample is still heating. (Reducing the laser power reduces the Raman signal generated at the sample and therefore the quality of the data. To compensate, try increasing the number of exposures or the exposure time.) If this problem persists, contact our sales or service representative in your area, or visit our web site at www.thermo.com/spectroscopy.

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The Spectrum Baseline Is Severely Tilted or Curved The sample fluoresced during data collection. To correct this problem, try one or more of the following: • Purify the sample. • Make sure the sample container is not responsible for the fluorescence. • If fluorescence is an inherent property of the sample, correct the baseline to subtract the broad background. • Use a longer wavelength laser or expose the sample to the laser beam for a period of time before beginning the collection of the sample spectrum (this is known as “photobleaching”). On the Collect tab of the Experiment Setup dialog box, turn on Preview Data Collection and type the desired exposure time in the Preview Time text box. If this problem persists, contact our sales or service representative in your area, or visit our web site at www.thermo.com/spectroscopy.

The Spectrum Baseline Has a Severe Positive Offset The sample is heating. To account for this condition try one or more of the following: • Correct the baseline to subtract the broad background. • Use a different laser. Shorter wavelengths heat samples less. • If the sample looks burned, replace it or move it so the laser will strike a fresh area. • Reduce the laser power and collect the sample again. Watch the live display to see if the sample is still heating. (Reducing the laser power reduces the Raman signal generated at the sample and therefore the quality of the data. To compensate, try increasing the number of exposures or the exposure time.) If this problem persists, contact our sales or service representative in your area, or visit our web site at www.thermo.com/spectroscopy.

The Spectrum Baseline Is Severely Shifted No background was subtracted from the sample data (the number of background exposures is set to zero or the Smart Background feature is disabled). The offset is the detector bias and dark signal. Set Background Exposures on the Collect tab of the Experiment Setup dialog box to an integer greater than 0. If this problem persists, contact our sales or service representative in your area, or visit our web site at www.thermo.com/spectroscopy.

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A Grating Does Not Appear to Be Installed or the Grating Cover Is Open 1. Make sure a grating is installed. 2. Make sure the grating cover is closed. 3. Exit OMNIC™, shut down the computer, turn off the instrument, wait 30 seconds, and then turn on the instrument. If this problem persists, contact our sales or service representative in your area, or visit our web site at www.thermo.com/spectroscopy.

A Laser Does Not Appear to Be Installed 1. Make sure a laser is installed and the keyswitch is turned on. 2. Exit OMNIC™, shut down the computer, turn off the instrument, wait 30 seconds, and then turn on the instrument. If this problem persists, contact our sales or service representative in your area, or visit our web site at www.thermo.com/spectroscopy.

A Filter or Fiber Optic Accessory Does Not Appear to Be Installed 1. Make sure a filter or fiber optic accessory is installed. 2. Exit OMNIC™, shut down the computer, turn off the instrument, wait 30 seconds, and then turn on the instrument. If this problem persists, contact our sales or service representative in your area, or visit our web site at www.thermo.com/spectroscopy.

The Nosepiece Does not Appear to be Installed 1. Make sure the nosepiece is properly installed. 2. Exit OMNIC™, shut down the computer, turn off the instrument, wait 30 seconds, and then turn on the instrument. If this problem persists, contact our sales or service representative in your area, or visit our web site at www.thermo.com/spectroscopy.

The Image is Obscured or Distorted If the objective is dirty or contaminated, clean it. (See the “Cleaning your instrument” topic.) If this problem persists, contact our sales or service representative in your area, or visit our web site at www.thermo.com/spectroscopy.

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The Computer Cannot Communicate with the Instrument 1. If the instrument is turned off, turn it on. 2. Check the cable between the computer and the instrument. If it is disconnected, connect it. 3. If the front panel indicators are not on, make sure the instrument is plugged in. If this problem persists, contact our sales or service representative in your area, or visit our web site at www.thermo.com/spectroscopy.

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2423_DXR_Raman_UG.pdf

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