Professional Documents
Culture Documents
Operators Manual
(UP 266, UP 266 IV, UP 213, UP 213 IV)
New Wave Research Inc. 47613 Warm Springs Blvd. Fremont, CA 94539 Tel: (800) 566-1743 or (510) 249-1550 Fax: (510) 249-1551 Email: lasers@new-wave.com Website: http://www.new-wave.com
FEBRUARY 2, 2001
Website: http://www.merchantek.com
FEBRUARY 2, 2001
Copyright 2001 by New Wave Research, Inc. All rights reserved. Printed in the U.S.A. Reproduction or translation of any part of this publication, except as permitted by the 1976 United States Copyright Act, without prior written permission of New Wave Research, Inc. is unlawful
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SAFETY SAFETY SUMMARY Optical Safety Laser Safety Electrical Safety Safety Features Laser Covers Interlocks Laser Light Emissions Government Regulations Laser Classification Location of Safety Labels HARDWARE SETUP PROCEDURES SYSTEM OVERVIEW Laser Module Base Module Laser Power Supply Preparation Space Requirements Electrical Requirements Laser Safety Requirements SYSTEM INSTALLATION Unpacking the UP266X Base Module Installation Laser Module Installation Video Train Installation Connecting the Laser Module to the Base Module Laser Power Supply Installation Cooling System External Connections AC Power Connections Computer & System Connections Mass Spectrometer Connections Turning off the system Starting the Software Establishing Coolant Flow Testing the Light Sources Testing the X-Y Stages Testing the Z Axis Testing the Video System Testing the Laser System SIGNAL SPECIFICATIONS Trigger In to the LAS Trigger Out from the LAS Circuit Diagrams Trigger Out Operation Disabled
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Laser Mode Pattern Mode Experiment Mode Trigger In Operation Pattern Mode Experiment Mode INTRODUCTION TO LASERS THE GENERAL LASER P RINCIPLE ND:YAG LASER General Introduction Q-switching P OLARIS / TEMPEST LASER Optical Attenuator Harmonic Generation UP SERIES SYSTEM DESCRIPTION GENERAL OVERVIEW LASER FORMATION CRATER SIZE SELECTION VIEWING THE SAMPLE SAMPLE CHANGEOVER SOFTWARE STEP-BY-STEP GUIDE I. GETTING STARTED STEP 1: Load the software STEP 2: Load NIST612 glass standard STEP 3: Purge the gas lines STEP 4: Select online mode STEP 5: Calibrate the XYZ stage STEP 6: Select the light source STEP 7: Select the lowest magnification STEP 8: Focus on the sample surface via Z-stage STEP 9: Adjust laser energy to full output STEP 10: Adjust repetition rate to 20Hz STEP 11: Select largest crater diameter STEP 12: Selecting Continuous Ablation mode STEP 13: Click on FIRE II. TUNING THE ICP-MS STEP 1: Select sample area STEP 2: Select line pattern STEP 3: Draw line on the sample STEP 4:Choose line properties STEP 5: Monitor masses STEP 6: Run a short term stability test III. SCREEN P ROPERTIES AND CALIBRATION ROUTINE STEP 1: Adjust Video properties STEP 2: Adjust Display properties STEP 3: Calibrate Screen IV. LASER ABLATION P ARAMETERS AND PATTERN SELECTION Influence of laser parameters
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Preablation Internal standards Real Time analyses Laser Pattern V. RUNNING AN EXPERIMENT File Options VI. V IDEO OVERLAY FUNCTION STEP 1: Create the sample map area STEP 2: Make the sample map MAINTENANCE & TROUBLE-SHOOTING MAINTENANCE Safety System Inspection Cooling System Maintenance Light Source Maintenance Laser/Video Alignment TROUBLESHOOTING Interface Problems Safety Interlock Problems Laser Power Supply Interlock Failure Door, Rear Cover Interlock Failure Trinocular Viewer Interlock Failure Laser Problems Laser to Video Misaligned (the spot is not at the center of the crosshairs) Laser Low Energy Laser Doesnt Fire
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Chapter 1
Safety
1 FEBRUARY 2, 2001
2 FEBRUARY 2, 2001
Safety
Safety Summary
Review the following safety precautions to avoid injury and prevent damage to the Laser Ablation System or any products connected to it. To avoid potential hazards, use the system only as specified. WARNING: The UP Series Laser Ablation System contains subsystems that present dangerous voltage, current and radiation hazards. Only qualified personnel should perform service procedures.
Optical Safety
The Standard UP Series is designed to meet Class I laser safety requirements and as such does not require special precautions under normal operation. However, configurations of the UP Series are available for some applications designated as a Class 4 laser product and the system is based on a Nd:YAG laser that generates high-energy radiation that can pose serious risks to eye safety. Infrared and ultraviolet radiation are invisible to the eye so the hazard is not immediately obvious, but the radiation can be focussed onto the retina, corona or lens. For this reason it is very important that, when performing any normal operation of Class 4, and/or maintenance or service which might expose the service personnel to internal laser radiation, service personnel wear safety glasses suitable for protection of high energy ultraviolet radiation and be aware of any possible reflections. Avoid any exposure of skin to the high energy UV radiation since it may cause cancer. This Nd:YAG laser ablation system meets the requirements for Class I laser product when all panels are closed. The interlocks must never be defeated other than for manufacturers service. With any enclosure removed, or sample chamber removed or disassembled, the UP series emits Class 4 laser radiation. The only maintenance required by the customer that will open a safety interlock is during flash lamp replacement. During flashlamp replacement the user will disconnect the AC power, remove the infrared cavity cover to access the flash lamp. The flash lamp replacement is performed without ever turning the laser on. In addition, the tygon tubing that transports the aerosol generated during ablation from the sample chamber to the mass spectrometer is replaced periodically. This involves removing two hex head screws from the rear access cover of the Class 1 enclosure. This procedure requires tools and should be performed without firing the laser.
Cleaning of the sample chamber window will be required periodically. This procedure requires tools and must be performed without firing the laser. Interlocks will ensure the laser does not fire during this procedure. Access to radiation from this product is necessary only under some service conditions when interlocked panels are opened and the interlocks defeated, unless purchased as a Class 4 product. These procedures are undertaken only by staff who have been suitably trained, and approved by the manufacturer. Laser radiation is emitted as a narrow beam of almost parallel rays, the intensity of which will remain high even at some distance from the laser. Although the radiation is non-ionizing, exposure can cause damage to living tissue as a result of heat produced during radiation absorption. The radiation of an Nd:YAG laser lies outside the visible range. In general, the maximum permissible radiation exposure for the skin is several times greater than for eye. Safety measures with regard to radiation hazard are therefore mainly based on dangers for the eye. WARNING: The Nd:YAG laser in the UP series laser ablation system is a Class IV high power laser whose beam is, by definition, a safety and fire hazard. Take all necessary precautions to prevent accidental exposure to both direct and reflected beams. DIFFUSE, AS WELL AS SPECULAR BEAM REFLECTIONS, CAN CAUSE SEVERE EYE AND SKIN DAMAGE.
WARNING: BECAUSE THE RADIATION OF AN Nd:YAG LASER IS INVISIBLE, THEY ARE EXTREMELY DANGEROUS. Possible wavelengths are high intensity ultraviolet, visible, and infrared radiation of 213, 266, 355, 532, and 1064 nm. Radiation passes easily through the cornea and focuses on the retina of the eye where it can cause instantaneous permanent damage including blindness. AVOID EYE AND SKIN EXPOSURE TO DIRECT OR SCATTERED RADIATION.
CAUTION: USE OF CONTROLS, ADJUSTMENTS OR PERFORMANCE OF PROCEDURES OTHER THAN THOSE SPECIFIED HEREIN MAY RESULT IN HAZARDOUS RADIATION EXPOSURE.
Follow the instructions contained in this manual for proper and safe operation and servicing of your laser. Wear protective eyewear; selection depends on the energy and wavelength of the laser beam as well as operating conditions. Consult ANSI, ACGIH or OSHA standards for guidance. At all times during operation, and maintenance, or service of your laser, avoid exposure to the laser or collateral radiation exceeding the accessible emission limits listed in Performance Standards for Laser Products, 21 CFR 1040 10 (d). (Laser Institute of America, 12424 Research Parkway, Suite 125, Orlando, FL 32826 ((407) 380-1553)
Laser Safety
WARNING: Do not power-up the Laser Ablation System before reading and understanding the operating and safety procedures. Use of controls, adjustments, or performing procedures other than those specified may result in hazardous laser radiation exposure and personal injury, laser system damage, and void the warranty. Laser light poses safety hazards that are not associated with conventional light sources. Special precautions must be observed when maintaining or servicing the UP series laser ablation system. The safe use of lasers requires that all personnel working in the lasers area are aware of the dangers involved. Laser beams are intense enough to burn skin, clothing or paint. They can ignite volatile substances such as alcohol or other solvents. The beam may also cause damage if reflected from some other surface. For this reason, it is important to observe the following precautions whenever the Class I protective safety enclosure is removed and/or the safety interlocks defeated.
Avoid eye contact with the output beam; even diffuse reflections are particularly hazardous when the protective cover is removed. Treat back reflections from any optic surface as you would the main laser beam. Even though the energy of such reflections is only a fraction of that contained in the main beam, it is sufficient to cause serious bodily harm, especially to the eye. Use protective eyewear at all times when protective housings are removed, or operation of a Class 4 designated system . Selection depends on the wavelength and the intensity of the radiation, conditions of use and visual function required. Operate the laser at the lowest possible beam intensity. Avoid blocking the output beam or its reflection with any part of the body. Establish a controlled access area during maintenance and service. Limit access to those trained in the principles of laser safety. Maintain a high ambient light level in the laser operation area to constrict the pupil of the eye, reducing the possibility of injury. Post warning signs prominently near the laser operation area. Provide enclosures or barriers for beam paths whenever possible.
To prevent unnecessary reflections and scattering, set up energy absorbing targets to capture the laser beam. If laser service is required, contact New Wave Research / Merchantek Products at Tel 510 249 1550 or Fax 510 249 1551, E-mail: lasers@new-wave.com
Electrical Safety
The UP Series meets CE safety and emission standards. WARNING: The laser head and power supply contain electrical circuits operating at lethal voltage and current levels. Certain procedures, such as changing the water filter or cleaning optical components require removal of the protective systems. It is important that all personnel using the laser observe all safety precautions outlined in this manual. The most important rule when working with the laser is to switch it off completely. There are no user serviceable parts on the electrical side of the Laser Power Supply. New Wave Research must carry out Service procedures on power supply electronics.
Safety Features
The following features are built into the UP series and conform to government regulations to provide safe laser operation.
Laser Covers
The Nd:YAG laser beam is enclosed in a protective housing, which prevents access to radiation in excess of Class I limits, unless purchased as a Class 4 designated product. The cover also protects against stray radiation. Do not remove the cover, except to perform maintenance procedures by trained personnel.
Interlocks
The Nd:YAG laser ablation system has a series of interlocks to prevent accidental exposure to dangerous levels of electricity or radiation. In addition, there are interlocks designed to interrupt laser operation if the laser is damaged. The interlocks are:
Remote interlock interrupted (if utilized). Sample cell open or removed. (if purchased). Transluc ent Class One Enclosure Removed. System Cover Removed. Trinocular head (if purchased).
Government Regulations
New Wave Research suggests that laser users purchase a copy of the American National Standard for the Safe Use of Lasers (ANSI Z136.1-1993). This publication provides recommendations for the safe use of lasers and laser systems that operating at wavelengths between 180 nm and 10 um. The publication is available from:
Laser Institute of America 12424 Research Parkway, Suite 125 Orlando, FL 32826 (407) 380-1553
Laser Classification
The governmental standards and regulations specify the laser must be classified according to the output power or energy, and laser wavelength. The UP series can be supplied as either a Class I or class IV laser system. In either case, when the protective enclosure is removed and/or safety interlocks defeated, the laser is classified as Class IV based on 21 CFR, subchapter J, part II, section 1040-10(d) and Class IV based on EN 60825-1, clause 9 of the European Community Standards.
The following images, Figure 1, Figure 2, Figure 3, and Figure 4, show the location of the labels.
Figure 1
Figure 3
Figure 2
Figure 4
The following images show the safety labels used on the UP Series Ablation Systems.
OR
Figure 6 Class 1 laser label (Quantity 2)
Details referring to CDRH-IR Radiation Control Drawing (RCD) Nd:YAG, UP - 213, UP - 266
9 FEBRUARY 2, 2001
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Chapter 2
Hardware Setup Procedures
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Laser Module
The UP SERIES incorporates a specially designed Nd:YAG laser, frequency quadrupled or quintupler to generate an ultraviolet wavelength and flat beam profile. The laser and beam delivery system provide flat beam focusing that allows sampling to a uniform depth rather than a crater, which is deep in the center and shallow at the edges. The Laser Module also contains the video system, including a high-resolution CCD camera, computer-controlled zoom, high magnification objective, light sources for sample illumination, and specified options.
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Base Module
The Base Module contains the system power supply, the X-Y stepper motor controller, power supply and XY stages, Z axis controller, Z axis stage, the valves for controlling the gas flow, transmitted light source with polarizer, ring and reflected lighting sample chamber, and specified options.
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Start Up
Preparation
WARNING: Do not power-up the Laser Ablation System before reading and understanding the operating and safety procedures. Use of controls, adjustments, or performing procedures other than those specified may result in hazardous laser radiation exposure and personal injury, laser system damage, and void the warranty.
The UP SERIES installation procedure is relatively simple, but does require some preparation. Prior to unpacking the system and installation, evaluate the physical arrangement of the laboratory to choose a suitable location. The following sections discuss space, electrical and laser safety requirements. Proceed with the installation once a suitable location has been selected and prepared.
Space Requirements
The Laser Ablation Base Module and Laser Module require 20 Wide x 26 Deep x 34 High (50 x 66 x 86 centimeters) of countertop space. The system weighs approximately 120lbs. In addition, space must be made for the computer monitor and keyboard if the system is not integrated with the mass spectrometer. The Laser Power Supply usually sits on the floor and occupies a 9 Wide x 15 Deep x 19 High (22 x 38 x 48 centimeters) footprint. For most applications, the sample flow path should be short. Therefore, the Laser Ablation System needs to be placed close to the mass spectrometer.
Electrical Requirements
The Laser Power Supply is shipped configured as either a 110 VAC, 10 A, 50/60 Hz or a 220 VAC, 5A, 50/60 HZ system. The Laser Ablation System is shipped configured as either a 110 VAC, 5 A, 50/60 Hz or a 220 VAC, 3A, 50/60 HZ system.. In either case, the system should be located within 6 feet (2 meters) of four power outlets for the: Base Module, Laser Power Supply, Computer, and Computer Monitor.
DANGER HIGH VOLTAGE: Both the Laser Module and the Laser Power Supply contain electrical circuits operating at lethal voltage and current levels. Always disconnect and wait at least one minute to allow capacitors to bleed down before servicing any part of the laser system.
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A power cord set that meets the requirements of the country in which the system was purchased is provided with every system. If the system is used in another country, a power cord set that meets the requirements of that country must be used. User replacement fuses provide electrical overload protection.
WARNING: This system is designed for connection to a grounded outlet. The grounded type plug is an important part of the safety design. To avoid the risk of electrical shock or damage to the system, do not disable or remove this feature.
DANGER INVISIBLE LASER RADIATION: The UP SERIES uses a Class IV Nd:YAG Laser. The output beam is, by definition, a safety and fire hazard. Precautions must be taken during the use and maintenance to prevent accidental exposure to direct or reflected radiation from the laser beam.
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System Installation
Unpacking the UP266X
The UP SERIES Laser Ablation System has been carefully inspected and packaged for shipment. Inspect the external packaging immediately upon receipt for shipment damage. If damage is evident, immediately file a claim against the carrier and notify New Wave Research / Merchantek Products. Inspect all items during unpacking with a factory-authorized representative, and notify the carrier immediately of any concealed damage. Be sure to save all packing materials in case a future shipment is needed. The UP SERIES laser ablation system will arrive in two (3) crates. One crate will include the top half of the system with attached laser umbilical. The second crate will include the base system platform, with the third crate containing the laser power supply, and accessory box. If a computer was ordered with the system there will be two (2) additional boxes which contain the computer monitor and computer with pre-installed video card and software. If the UP SERIES is shipped or removed from storage during cold weather, allow the system 4 to 8 hours to attain room temperature before opening and exposing to warm, humid air. WARNING: If condensation forms on or inside the UP PLATFORM, allow it to dry thoroughly before connecting to the AC power source and operating. Failure to do so may cause injury or equipment damage.
Figure 10
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Figure 11
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Figure 12 shows the top Laser Module with the covers removed and ready for installation onto the Base Module.
Figure 12
Two people are necessary to place the top Laser Module onto the Base Module. With one person on each end of the Laser Module, carefully lower the Laser Module onto the Base Module. The cabling connected to the z-axis on the Base Module must be guided through the rectangular cutout on the Laser Module. The Base Module has two locating pins used to properly locate the Laser Module onto Base Module. Use the (11) 10-32 x 5/8 screws, supplied in the accessory box, to secure to Laser Module onto the Base Module.
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Figure 13
Figure 14
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Replace the protective sheet metal housing (if included) onto the Laser Optical Deck. Be careful not to bump the optical mounts. Secure this cover in place with the 5 captive straight slot screws. Place the Main Cover onto the Laser Module. To install this cover, place the back end of the cover over the back bulkhead panel. As the front end of the cover is lowered into place, spread the two lower front corners over the base optical plate. As the cover is placed over the optical plate, slide the cover forward until flush with the back panel. Secure into place with the (6) 6-32 screws that were earlier removed. Place the Front Bezel onto the Laser Module. Secure into place with the (2) 6-32 around the front of the base, and the (4) screws on the Video Tower.
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WARNING: Secure all connectors. Operating the Laser Ablation System with cables loose or disconnected may cause equipment damage.
Install the 9-pin to 15-pin power supply interface cable from the Laser Module to the Laser Power Supply. Connect the 15-pin end of the cable to the 15-pin connector labeled Remote on the rear panel of the Laser Power Supply. Connect the two BNCs to the Fire Lamp and Fire Qsw connectors on the rear panel of the Laser Power Supply. Connect the 9-pin end of the cable to the 9-pin connector on the Laser Module labeled Power Supply Interface.
Figure 15 (Back View of Laser Power Supply) shows the cable interconnects to the Laser Power Supply.
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Cooling System
The UP SERIES system includes an integrated liquid to air heat exchanger that removes heat from the laser. A squeeze bottle and distilled water are supplied to aid in filling the system. Removing the Laser Power Supply cover is not necessary to add coolant to the system. To fill the system:
Remove the fill plug located on the front of the Laser Power Supply. Remove the jumper tube located on the rear of the Laser Power Supply. This connects the water in and water out ports. Use the squeeze bottle to force water into the water return connector on the rear of the Laser Power Supply until the reservoir is half full. The level of the reservoir is viewed through the slot on the front of the Laser Power Supply. Again using the squeeze bottle, force water into the water out connector on the rear of the laser Power Supply until the reservoir is from the top of the slot. Again using the squeeze bottle, force water into the tubes coming from the Laser Module until water is forced out the second tube and all air is removed from the laser. Quickly plug both tubes from the Laser Module into the rear of the Laser Power Supply. If the water reservoir is not filled from the top, squeeze water into the front fill plug until the proper level is achieved.
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WARNING: To avoid laser head damage, use only fresh distilled water to fill the cooling system.
Figure 17
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Note: To insure stabile output energy, the system should be allowed to warm-up for a minimum of 20 minutes with the power switch on the back of the power supply turned on. It is recommended that this switch be left on at all times, even when the system is not being used for extended periods. The Laser Power Supply key switch should be turned on only during the period when the system is being used.
As the software loads, a system self-test and subsystem resource verification will be performed. The results of the subsystem resource verification are reported in the Start-up screen (see Software Chapter 5). Any errors detected during the self-tests will be reported in special message windows.
The Start-up screen provides the following status information concerning the results of the resource verification.
Laser Controller Present. X-axis Stage Controller Present. Y-axis Stage Controller Present. Z-axis Stage Controller Present. Coax Light Source Present. Ring Light Source Present. Transmitted Light Source Present. Gas Valve Controller Present.
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If any of these controllers are not located, contact a New Wave Research / Merchantek Products representative as the system may require maintenance. Once the self-tests are complete, the Start-up screen disappears and main program window appears.
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NOTE: A solid blue screen indicates that the video card is not receiving a camera signal. If this occurs, verify the Base Unit power is on, the 25-pin cable is connected between the Base Module and Laser Module, and the S-video cable is connected between the Laser Module and the computer.
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If the auto-focus option is being used, only fire the laser when the auto-focus has locked on to the sample and is not moving. Always flow gas through the sample chamber when firing the laser.
If the above precautions are not followed it may result in damage to the laser objective lens and / or the sample cell.
Connection diagram
The following diagram shows the various cable connections for a typical -UP system.
This document describes the proposed specifications for the synchronization and trigger signals interface between a mass spec (MS) system and the New Wave Research / Merchantek Products UP Laser Ablation System (LAS).
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Signal Specifications
Trigger In to the LAS
An input to the LAS is provided on the LAS back panel. See Figure 18 System Interconnect. This input can be configured via a jumper to accept either a TTL-level trigger signal, or a contact closure. The input is optically isolated from the rest of the LAS by an opto-isolator.
Circuit Diagrams
The diagrams below show the electrical details for the interface signals when configured for either switch closure or TTL interface.
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Disabled
No trigger signal is generated.
Laser Mode
The trigger out signal is active while the laser is firing during a scan. The signal goes active when the laser first starts firing during a scan, remains active while the laser continues to fire, and goes inactive once the laser stops firing. The signal is not active during a pre-ablation pass, even when the laser is firing. If a raster grid or line grid scan pattern is defined, the signal will be inactive during the pause between sites on the grid.
Pattern Mode
The trigger out signal goes active N1 msecs after the scan of an each pattern is initiated, remains active while the scan is being performed, and goes inactive N2 msecs after the scan of each pattern is complete. The values for N1 and N2 are user-selectable, between 0 and 9999 msecs.
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The signal is not active during a pre-ablation pass. If a raster grid or line grid scan pattern is defined, the signal will be active during the pause and movement between sites on the grid.
Experiment Mode
The trigger out signal goes active N1 msecs after an experiment run is started, stays active during the rest of the run, and goes inactive N2 msecs after the last scan pattern in the experiment is complete. The values for N1 and N2 are user-selectable, between 0 and 9999 msecs. The signal remains active during the pause and movements between scan pattern locations, and remains active during the pre-ablation pass.
Trigger In Operation
The MS generates the trigger in signal to trigger the LAS to start a scan. The LAS software defines two modes of operation for the trigger in signal: Pattern Mode, and Experiment Mode.
Pattern Mode
After the user presses the Run Experiment button, the LAS waits for the trigger in signal to go active before performing the scan of the first pattern. The LAS will perform the scan, and then check the trigger in signal again it wont proceed with the next pattern until/unless the trigger signal is active. Thus, the LAS checks the state of the trigger in signal at the start of each pattern scan, and only proceeds with the scan if the signal is active.
Experiment Mode
After the user presses the Run Experiment button, the LAS waits for the trigger in signal to go active before starting the experiment run. The LAS checks the state of the trigger in signal only at the start of the experiment run.
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Chapter 3
Fundamentals
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Introduction to Lasers
The General Laser Principle
The principle of lasers, the Light Amplification by Stimulated Emission of Radiation is best explained when looking at the process of photon emission. This process, from an excited state takes place statically and is described as spontaneous emission. The opposite process, the process of absorption, occurs when light hits an atom a photon can be absorbed if the energy corresponds to the excitation energy of the atom.
E2-E1 + h * v12
After absorption, the atom is in excite state 2, so apart from being excited by electrons, atoms can also be excited by photons. However, in distinction to electron excitation, the photon energy of the absorbed radiation has to correspond to the transition energy. The third interaction process is a process that is essential for the generation of laser light, the stimulated emission. It can occur when photons with energy h v12 collide with an atom in state 2 and the decay energy corresponds to the incident photon energy
The incident photon thus stimulates a radiation process. When the emitted photon has the same direction as the incident photon, the phases of the two emitted wares are also the same. Stimulated emission allows the construction of a light amplifier in the optical region of the spectrum. The following three illustrations demonstrate the formation of this laser.
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First a laser medium must be created which is suitable as an optical amplifier. For this, N2 > N1 is the sole condition, which is necessary in a two-level system. This is indicated by a pump arrow and is independent of its realisation in individual cases. In order to prevent the spontaneous emission from destroying the inversion, these losses have to be compensated for by pumping. On two sides of the laser medium, mirrors are placed to form a resonator. One mirror is partially reflecting. As spontaneous emission always generates photons, a photon field will be created along the resonator as a result of the amplification in the laser medium and the feedback by the resonator. This photon field is emitted through the partially reflecting mirror as laser emission. The laser emission shows a high degree of directionality and can therefore achieve a high energy density. There are many different classification of the various lasers, i.e. solid state lasers such as Nd:YAG lasers, gas lasers such as He-Ne or Excimer lasers as well as liquid lasers and semiconductor lasers.
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Nd:YAG Laser
General Introduction
The Nd:YAG laser uses traditional flash lamp pumping. Distilled water cools the lamp and gain medium, reducing thermal lensing. When electrically pulsed, the lamp emits light that excites the laser gain medium, an Nd:YAG rod. The laser crystal is an yttrium aluminium garnet single crystal, doped with neodymium ions (hence the term Nd:YAG). Similar to a capacitor storing electrical energy, the Nd:YAG rod absorbs the flash lamps optical energy. Neodymium atoms that have been excited to a higher electronic state (the lasing level) store this energy. These atoms remain excited for a fraction of a millisecond before spontaneous emission starts. In the absence of Q-switching, spontaneous emission (lasing, or light amplification through stimulated emission) begins as soon as the cavity gain overcomes its losses. The duration of this spontaneous laser pulse is almost as long as the driving lamp pulse. This non Q-switched pulse has high energy, but its peak power is low, because of its relatively long width. The Q0switch improves performance by both increasing the amount of energy stored in the rod and by preventing or delaying spontaneous emission. Whilst closed, a Q-switch in the laser cavity introduces an additional loss and blocks spontaneous emission, allowing the number of excited atoms in the rod to build further. When instantaneously opened, it releases the cavitys stored energy in a shorter pulse with both higher average and peak power.
Q-switching
The Q-switch consists of a crystal, quarter wave plate and a vertical polarizer, placed in the laser cavity between its end mirrors. The lamp pumps the gain medium while the Q-switch is closed (there is no voltage applied to its crystal, and the crystal does not rotate light). While closed, light exiting the rod cannot return to stimulate spontaneous emission, and the rods energy storage capacity increases. Horizontally polarized light exiting the gain medium never returns; it is always blocked by the vertical polarizer. When the Q-switch is closed, it also blocks vertically polarized light: this light passes unchanged through the vertical polarizer and the crystal, then rotates 450 transiting the quarter wave plate. On its return path, it rotates another 450. Now horizontally polarized, the vertical polarizer prevents it from re-entering the rod. After maximum storage occurs (about 100 microseconds after the lamp begins pumping), the Qswitch opens: a Marx bank suddenly applies a high voltage to the crystal. When so energized, the crystal now rotates the light another 900 (450 in each direction through the Q-switch). Vertically polarized light now rotates a total of 180 0, so it retains its polarization travelling through the Qswitch, and can re-enter the laser rod. This light is now free to oscillate between the cavity end mirrors. During these oscillations, the light increases in energy by extracting the energy stored in the gain medium. The resultant laser pulse is 3-5 nanoseconds long, with high peak and total power.
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Polaris Laser
The POLARIS employs a flash lamp-pumped Nd: YAG rod in a thermally compensated resonator to generate radiation at 1064 nm. The resonator is very compact, mechanically isolated from the laser housing, which makes the system relatively insensitive to vibrations and temperature change. The IR head is housed in a separate sealed area that requires no adjustments in normal operation. The only time the IR head needs to be opened is on the rare occasion that the flash lamp needs to be changed during a maintenance procedure.
Optical Attenuator
The optional optical attenuator serves to control the laser energy without affecting the beam quality. The optical attenuator is designed to work on the 1064 nm beam, so it is placed directly after the IR head, before any harmonic generation crystals.
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The optical attenuator consists of a half wave plate, followed by a polarizer. The half wave plate is secured to a motorized rotating mount. The servo motor controlled angle is set by input from the control panel. The polarizer is permanently aligned to transmit vertically polarized light. This maintains the polarization of the IR light as emitted from the IR head in the standard configuration.
Harmonic Generation
The 1064 nm laser pulse exits the IR head and then different harmonic wavelengths may be generated if these options have been installed. The second harmonic at 532 nm is generated by passing the IR beam through an angle tuned KTP crystal. The Polaris uses Type II phase matching in KTP to generate the second harmonic, so the polarization of the IR beam must be adjusted to maximize SHG intensity. Dichroic mirrors separate the second harmonic from the fundamental light and direct the beam to the output port. The second harmonic light is vertically polarized. The third harmonic at 355 nm may be generated in the Polaris if the option has been purchased and installed. The third harmonic at 355 nm is generated by combining one photon at 532 nm with one photon at 1064 nm. Third harmonic generation is accomplished by Type I phase matching in BBO. The second harmonic must be detuned slightly to achieve the maximum third harmonic conversion efficiency. The third harmonic light is separated from the fundamental and second harmonic using a pair of dichroic mirrors. The third harmonic light is vertically polarized. The fourth harmonic of Nd: YAG at 266 nm can be generated by doubling the 532 nm second harmonic light. This is done by placing the correct BBO crystal in the optical path and combining two photons at 532 nm to give one photon at 266 nm. The light at 266 nm is separated using a pair of dichroic mirrors to select only the fourth harmonic light. The fourth harmonic light is vertically polarized.
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Chapter 4
Laser Description
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Laser Formation
The following figure shows the doubling crystals to quadruple the fundamental wavelength of 1064nm to 266nm. For further details of the laser fundamentals and the generation of harmonic wavelength, please refer to chapter 2, Fundamentals.
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The laser fires with a fixed pulse energy, optimising its efficiency and stability. The energy of the beam is focused onto the sample, then attenuated, in accordance with the energy appropriate to the crater size required and the matrix at the target site. The energy attenuator enables the continuous adjustment of the laser energy without changing the voltage of the flash lamp.
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Samples can either be viewed through transmitted light, reflective light or coaxial light. The type of light source and the brightness is under computer control.
Samples are mounted in a cell on a high precision XY stage. The stage is fully under software control. Automatic operation permits the storage of sampling patterns and coordinates for automated, unattended analysis. The laser cell is flushed with argon and/or helium gas, carrying the ablated material to the plasma for ionization and subsequent analysis in the mass spectrometer.
Sample Changeover
The gas bypasses the cell when loading or unloading samples, then the cell is purged of air before the gas is routed back to the torch. The operation of the different gas lines is under software control. For easy sample changeover, the whole sample cassette can be removed as shown in the following sequence.
Figure 32: Sample changeover step 1: Lift the two cam levers after selecting BYPASS on the main screen.
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Figure 33: Sample changeover step 2: Pull the sample cassette out
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Chapter 5
Software Step-by-Step Guide
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I. Getting Started
STEP 1: Load the software
To install the software insert the floppy disk, the software package is self-extracting and will guide the user through the installation. Once installed, the software is started by clicking on the icon or via PROGRAMS in the Start menu. The first opening screen when for the software looks like below:
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When passing the mouse over each function, the description of this particular function will be displayed. The icons on the upper row of the software screen enable the functions such as the selection of the illumination source and the brightness, the zoom function of the monitor, the mode of ablation, the frequency, the crater spot size and laser on/off function.
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Purge is selected after sample changeover to flush any air out of the chamber for a fixed user defined period before automatically switching back to ONLINE. The PURGE timeout may be edited via a pull down menu, which can be opened by a right hand mouse click on any of the gas control buttons.
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Click on SET PURGE TIMEOUT and enter the amount of time in seconds. Then click on OK. Typically a purge timeout of 30 seconds is sufficient.
Connect the laser to the ICP-MS and purge the gas lines for a few minutes.
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Click once on the POSITION icon on the tool bar, and confirm the calibration of the stage by clicking on YES.
When the calibration routine has completed the stages are at their HOME positions. The stage position window opens as shown below. A previously stored stage position may be selected from a list, or the stage may be driven manually using the scroll bars or the joystick controls. If the CENTRE position has been stored previously, select it and the stage will move to the centre of the stages or any other previous stored position.
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To save a new position, drive to the new position, then click on DEFINE NEW POSITION, enter the new file name and click on SAVE.
In the case that the CENTRE position has not been stored previously, drive the stage manually to 25mm in X and Y direction and 0 in Z direction. It is recommended to always load your sample into the centre of the stage to enable an easy focussing in just adjusting the Z stage.
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Alternatively, click once the magnifying glass icon and this window will be shown to enter the magnification manually.
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For the spot size calibration, click once with the right mouse button on the icon and the following display box will appear.
The preset Crater sizes may be changed by editing the iris and expander settings in the lookup table or by manually editing the current iris and expander settings.
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In Continuous mode the laser will fire continuously or as long as the time specified in an ablation pattern.
In SINGLE SHOT mode, the laser will just fire one single shot.
In BURST MODE, a specified number of bursts will be fired, to select the number of burst, click the burst icon once with the right mouse and the following menu will appear.
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Enter the number of bursts for this mode. For the Getting Started guide, select the continuous mode of ablation.
A large crater should now form in the sample. A signal on La139 should be obtained on the ICPMS. This proves that the laser is functioning and that the laser ablation signal reaches the ICPMS, the gas lines are therefore connected correctly.
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Then use the MEASURE tool, which is the last icon in the row of tools and drag it a known distance on the video window. This may be done using the optical standard supplied by New Wave Research or simply by measuring a distance previously recorded by reading back the stage positions, e.g. use stage read-back positions to measure the distance between the two craters. The image of the optical standard at 0% zoom looks as shown in Figure 5-III.5.
Drag the measuring tool over a distance of e.g. 20mm of the optical standard. It is very important not to move the stage during this process. For best results use two points as far apart on the video image as possible as this will reduce the error in the calculations since the measurement is made over a wider distance. If you are not using the optical standard, ensure that the exact distance between the two points chosen is known accurately.
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The distance is then reported back by the software. If the distance reported is inaccurate the correct value may be entered by the user and applied.
Repeat this process for all different zoom positions e.g. 25%, 50%, 75% and 100%. It is important that the screen will be calibrated at all zoom levels. For example, the optical standard at 100% zoom is shown in Figure 5-III.9. Now the two widest points apart stretch only over an area of 4mm. Drag over this distance with the measuring tool to calibrate the screen at highest magnification.
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Pre-ablation
Prior to the acquisition of data there are several advantages to be gained by adopting a period of preconditioning the sample. Using a pre-ablation time, prior to the bulk analysis can improve the stability of the density and composition of laser ablated aerosols. The direct sampling of solids may be affected by surface contamination, even when surfaces have been milled or ground prior to analysis. A period of pre-ablation before acquisition serves to clean the samples so that such contamination is reduced. Sensitivity is seldom enhanced by pre-ablation of the sample. The greatest effects are found in the reproducibility and precision of repeat analyses. The pre-ablation of sample is of use only in bulk analysis applications. The analysis of small features and surface layers does not generally permit lengthy periods of pre-ablation.
Internal standards
The use of an internal standard for quantitative and semi-quantitative analyses is highly recommended. The use of an internal standard, a minor isotope of the matrix element or a known concentration of a trace or minor element can be selected as an aid to quantitation. In cases where there is no certified element concentration available, a user value for the LA-ICP-MS can be chosen.
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Many laser sampling application areas are not well furnished with certified reference materials, and so semi-quantitative analysis routines are common. The choice of internal standard and the correct use of calibration routines then becomes a key factor in the generation of accurate data.
Laser Pattern
There is a range of different laser patterns available to suit the application requirement. Raster Grid of Spots Line Line of Spots Single Spot Whilst many feature laser sampling application involve ablation from a single site, it is sometimes advantageous to acquire data from a larger areas, as for most bulk analyses applications. Some applications, such as the analysis of fluid inclusions, may require refocusing during the ablation process, particularly if the fluid inclusion is not near the sample surface. Isotope ratio calculations may also require longer than normal acquisition times. For such applications, the software is designed to give incremental control of the Z stage during the acquisition, to keep the laser in focus throughout. The laser pattern are under software control and can describe rectangular raster and lines of shots on a sample surface, covering a much wider surface area than single spot analysis. During raster or line sample, a single acquisition that contains data representative of the entire sampled areas is taken. The sample can also be acquired in Real Time mode. Users can define the size of a raster pattern by entering an appropriate number of points and distance between the points. The raster area can be placed at any position on the sample and therefore repeat analyses can be completed on the same area of the sample or on an entirely new area. The number of shots per raster co-ordinate can be varied, as well as the distance between the shots and the number of passes.
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To select the ablation pattern, click on the downward arrow next to the TOOL icon.
When the required pattern has been selected the ablation conditions may be viewed and edited by right hand mouse clicking in the selected pattern next to the TOOLS button. For each pattern the spacing, the number of passes, scan speed, the Depth per Pass, the repetition Rate and Spot Size can be selected. Raster set-up
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Grid set-up For the GRID SET-UP there is an intersite pause that can be selected by the user.
Line of spots
Line Set-up
For single spot ablation, a single click in the sample image selects the ablation site.
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V. Running an Experiment
An ablation pattern can be applied to the sample by holding down the left mouse button to select the ablation start point and releasing at the required end point. The figure below shows a series of ablation patterns drawn on the sample image. As each pattern is drawn it is added to the list in the DEFINED PATTERN window on the left hand side of the screen. An individual pattern may be selected by clicking on the relevant pattern in the DEFINED PATTERNS LIST. When a pattern is selected, it changes colour from green to yellow on the screen. To start an ablation experiment, click on the START EXPERIMENT button. An experiment window opens. The user can choose to run the whole experiment or just those individually selected pattern in this window. To start ablation, click the ENABLE LASER box and then click RUN.
It is also possible to ablate a sample without the need to define a pattern on the sample surface. By clicking on the FIRE button the laser will ablate the sample at the viewing crosshair using the currently defined ablation settings. Each pattern or single spot may be highlighted and deleted by right-clicking and selecting DELETE in the pull-down menu. The pattern property of each pattern can be viewed by right hand clicking on the selected pattern. All laser parameters such as the energy output; repetition rate, crater size etc. can be edited in this window.
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File Options
There are five utilities in the FILE menu. Experiment details may be saved or opened or a new experiment started. Experiment details may be printed out and the sample image on the PC screen may be saves as a Bitmap (*.bmp), Tagged Image File (*.tiff) or a True vision Targa (*.TGA).
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In this SAMPLE MAP MANAGEMENT AREA it is now possible to define the area of the sample for the map creation. It is also possible to save and recall existing maps to and from files on the computer. The grey area represents the total area of the range of motion on the XY stage. The blue box represents the current size and location of the area to be mapped. This blue box can be dragged with mouse to change the location of the sample map. The green box shows the current position of the stage.
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The MAP CENTER LOCATION offers three choices for the position of the map area: CENTER OF SAMPLE AREA: the map will be centered within the area of the total travel of the XY stages. CURRENT STAGE POSITION: the map will be centered at the current stage position, as long as the map is not outside the travel range of the stages. USER DEFINED LOCATION: the map is centered around the user defined location, which can be either entered manually by typing in the XY values or by dragging the blue box in the map preview to the required location. The MAP SIZE is defined by the number of images. The more images are used the larger the area covered for the sample map. It is recommended to create the sample maps with the zoom set to 0%, as the zoom setting will affect the total size of area sampled. The estimated time for creating the map is displayed in the status line the bottom of the window.
The current position displayed as the green box, can be viewed throughout the complete process of creating the map. At the end of the process, all images overlaid can be viewed, as shown in Figure 5-VI.3.
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Click on OK and the sample map will now be shown in the left lower corner of the main menu. It is now possible to click anywhere on the map and the stages will automatically move to that new position. The actual image of that particular location can then be viewed under high magnification.
A sample map can be saved for reuse. By default, they are saved in the Maps subdirectory of the folder where the program was installed (usually C:\Program Files\Merchantek EO\Laser Ablation\Maps). A sample map is saved as a Windows bitmap file.
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Chapter 6
Maintenance & Trouble shooting
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Maintenance
Safety System Inspection
The Class I laser enclosure includes a number of interlocks that allow user access to areas exposed to the Class IV UV laser. The areas interlocked are the sample chamber access door, rear Base Module cover and trinocular assembly (if installed). The interlocks prevent the laser from firing whenever these areas are exposed. The trinocular assembly prevents the laser from firing whenever the trinocular is set for user viewing. To insure a safe environment, test the interlock functions once a month. Using appropriate safety eyewear, attempt to fire the laser with each of the covers open, verifying that the system does not fire the laser and the interlock warning is displayed. To test the trinocular assembly, attempt to fire the laser in the two user view modes however, do not look into the eyepieces. For Class IV systems, the sample chamber may or may not be supplied, and therefore, an interlock for this devise may not be supplied.
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Laser/Video Alignment
The laser alignment (spot on the sample) to the video crosshairs may drift from shipping or extended use. Two small holes on the right side of the Laser Module provide access to a turning mirror used to bring the laser back into alignment. To align the laser:
Remove the front system covering the access holes. Place an object (coin, etc) into the sample chamber. Set the laser for 4Hz, 35% power and a 40-micron spot.
While firing the laser, adjust the turning mirror until the laser is centered on the crosshair.
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Troubleshooting
Interface Problems
System fails to find the UP SERIES
Check serial cable installation between the computer and Base Module. Check the COM port selection. Check the Base Module power.
Laser Problems Laser to Video Misaligned (the spot is not at the center of the crosshairs)
Use the turning mirror to realign the laser. See Laser/Video Alignment on preceding page.
NOTE: To verify full energy, the iris should be 100% open and the beam expander set for minimum spot size.
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Check both BNCs are attached to the correct points on the rear of the Laser Power Supply. Verify that the switch labeled Fire Q-SW is in the Ext position.
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A AC Power Connections ...................................21 American National Standard for the Safe Use of Lasers ..........................................................6 analytical methodology ...................................71 B Base Module Installation.................................16 Beam size calibration table ..............................60 BURST OF SHOTS........................................61 BYPASS........................................................52 C Calibrate Screen.............................................68 CENTRE position...........................................55 Circuit Diagrams ............................................27 Class I laser......................................................2 Class IV...........................................................2 Connection diagram........................................26 Continuous Ablation mode ..............................61 Coolant Flow..................................................24 Cooling System ..............................................20 Coreco Bandit ................................................21 D DEFINE NEW POSITION..............................56 depth-profile ..................................................72 Display properties...........................................68 E Electrical Requirements ..................................14 Electrical Safety ...............................................4 energy radiation................................................2 excitation .......................................................32 Experiment.....................................................76 External Connections ......................................21 F fifth harmonic .................................................38 File Options ...................................................77 fill plug ..........................................................20 FIRE button ...................................................62 flash lamp ......................................................35 Focus .............................................................57 fourth harmonic ..............................................38 fundamental frequency....................................36
G gas control .....................................................52 Getting Started ...............................................50 Government Regulations ...................................6 Grid set-up.....................................................74 H Harmonic Generation......................................36 HOME positions .............................................55 I installation procedure......................................14 interlocks .........................................................2 Internal standards ...........................................71 IR head..........................................................37 L Laser Ablation Parameters...............................71 Laser Classification ..........................................6 Laser Covers....................................................4 laser energy....................................................58 laser formation ...............................................33 Laser Light Emissions .......................................5 laser medium ..................................................34 Laser Module .................................................12 Laser Module Installation................................17 Laser Power Supply ........................................13 Laser Power Supply Installation ......................19 Laser Principle ...............................................32 Laser Safety .....................................................3 light source ....................................................56 Light Sources .................................................25 Line of spots ..................................................74 Line Set-up ....................................................74 Load the software...........................................50 M magnification .................................................57 Manual spot size control .................................60 Mass Spectrometer Connections ......................22 MEASURE tool .............................................68 Polaris laser....................................................37 Monitor masses ..............................................66 N Nd:YAG laser .......................................... 12, 35
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O ONLINE........................................................52 Optical Attenuator ..........................................37 Optical Safety...................................................2 optical standard ..............................................69 P Pattern Selection.............................................71 photons ..........................................................34 POSITION icon..............................................55 Power Supply Interface.................................19 Preablation.....................................................71 Purge .............................................................52 Q Q-switch........................................................35 Quadrupling ...................................................36 R radiation...........................................................2 Raster set-up ..................................................73 Real Time analyses.........................................72 repetition rate .................................................58 resource verification .......................................23 RS-232 ..........................................................21 S safety hazards...................................................3 Safety Labels....................................................6 sample map....................................................78 Screen Properties...........................................67 sensitivity.......................................................71 SET PURGE ..................................................53 short term stability test....................................66 Signal Specifications.......................................27 SINGLE SHOT..............................................61 Single site setup..............................................75 Software Step-by-Step Guide ..........................50 Space Requirements........................................14
spontaneous emission................................ 32, 34 spot size calibration ........................................59 Startup screen.................................................23 stimulated emission ........................................32 S-Video cable .................................................21 switch closures ...............................................27 system calibration ...........................................55 System Connections........................................21 System Installation .........................................16 system off ......................................................23 system on.......................................................23 System Overview ...........................................12 T TOOL icon.....................................................73 Trigger In.......................................................27 Trigger Out ....................................................27 TTL signals ....................................................27 tuning process ................................................58 U umbilical cable ...............................................19 Unpacking......................................................16 V Video Overlay Function..................................78 Video properties .............................................67 W water reservoir................................................20 X X Y Z POSITION...........................................55 Z zonation studies..............................................72 ZOOM...........................................................57
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