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Published on January 4, 2008

Author: george

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CIC Photonics:  CIC Photonics IRGAS Training Schedule - Day 1 :  Schedule - Day 1 FTIR analysis IR spectrum Michelson interferometer Fast Fourier transform and corrections Interferogram, single beam spectrum, absorption spectrum and transmission spectrum Beer’s law Instrument resolution Quantification analysis-Classical Least Squares introduction Hardware description Bomem WorkIR Instrument purge Manual manifold SPGAS software IRGAS 100 IRGAS configuration manager Data retrieval Schedule - Day 2:  Schedule - Day 2 SPGAS software cont. Qmax – quantification manager IRGAS spectra reprocessing software Hardware installation System power Pipe installation Instrument purge Software installation IRGAS software Bomem Ethernet drivers System verification System maintenance Schedule - Day 3:  Schedule - Day 3 IRGAS worksheet IRGAS options IRGAS product array Marketing and selling strategies and techniques Competitors and competing products Service and maintenance FTIR Analysis:  FTIR Analysis Tab 1 Light Spectrum:  Light Spectrum Infrared is invisible light ranging from 1mm to 750nm in wavelength Infrared light can be divided into three parts: Far infrared -1mm to 10µm Mid infrared - 10µm to 2.5µm Near infrared - 2.5µm to 750 nm Infrared (IR) Spectrum:  Infrared (IR) Spectrum IRGAS System mid infrared range 2.5µm – 25µm in wavelength 4000 cm-1 – 400 cm-1 in wavenumbers Wavelength (λ) Wavelength = (1/wavenumber)*10,000 Wavenumber (cm-1) Wavenumber = (1/λ)*10,000 IR Molecules :  IR Molecules Not every molecule absorbs infrared light Monoatomic He, Ar, Ne, etc… Homoatomic diatomic N2, O2, H2, etc… N N Molecules that do absorb infrared light Water is a good example O H H Michelson Interferometer:  Michelson Interferometer Step 1: Beam leaves IR source and hits beamsplitter where it is sent straight through and at a 90° angle Step 2: The 90° angle beam hits a fixed mirror and is sent back to the beamsplitter Step 3: The beam that went straight through hits a movable mirror and is sent back to beamsplitter Step 4: The two beams recombine, go through the gas cell and travel to the detector 1 2 3 4 Michelson Interferometer:  Michelson Interferometer When AB=AC the phase of the frequencies look the same When AB=AC+1/4λ, then the phase of the frequencies are opposite in regards to maximums and minimums Michelson Interferometer:  Michelson Interferometer When AB=AC and the two recombine you get stronger maximums and minimums When AB=AC+1/4λ and the two recombine they cancel one another out and result in a flat line ABB Bomem Michelson Interferometer:  ABB Bomem Michelson Interferometer It has two sets of mirrors that move by a pivoting motion This design is called a wishbone configuration This configuration is more robust It can be placed in any orientation This configuration only has to be smooth at one point vs. the traditional interferogram that has to be smooth along a rail ABB Bomem Michelson Interferometer:  ABB Bomem Michelson Interferometer ABB Bomem Michelson Interferometer:  ABB Bomem Michelson Interferometer Laser Fast Fourier Transform:  Fast Fourier Transform The highest peak intensity is attained when AB=AC The maximum of the highest intensity peak is called the zero path difference (ZPD) point After the interferogram has been created by the instrument, the Fourier transform is applied to it, which then results in a single beam spectrum Single Beam Spectrum:  Single Beam Spectrum Single Beam Spectrum:  Single Beam Spectrum Single Beam Spectrum:  Single Beam Spectrum Single Beam Spectrum:  Single Beam Spectrum Transmission:  Transmission The ratio between the sample and the background spectrum Transmittance Spectrum:  Transmittance Spectrum Chemometrics:  Chemometrics Based on the transmission spectrum chemometrics can be applied Chemometrics: The application of statistical and mathematical methods for the design or optimization of chemical experiments and for the efficient extraction of information from chemical data Two types of chemometrics: Qualitative (identification) Quantitative (quantity) Absorbance:  Absorbance Beer’s Law:  Beer’s Law Says that concentration is directly proportional to absorbance (linearity) Beer’s law equation is A= abC Where A = absorbance a = absorptivity of the molecule b = pathlength that the light travels C = concentration Instrument Resolution:  Instrument Resolution The more points per peak the higher the resolution The higher the resolution the more noise, but the better peak separation Common resolution used for an ABB Bomem instrument is 2 cm-1 Ranges between 1 cm-1 to 128 cm-1 Why Do We Need a Gas Cell:  Why Do We Need a Gas Cell Intensity of a peak is directly related to the # of moles in a sample In the same area: Solid will be very packed Liquid will be less packed Gas will be even less packed Long Path Gas Cell:  Long Path Gas Cell 4Runner 6 Meter Gas Cell:  4Runner 6 Meter Gas Cell Gas Cell Mirrors:  Gas Cell Mirrors Top view of field mirror IR Beam Path:  IR Beam Path Classical Least Squares (CLS):  Classical Least Squares (CLS) The base equation is As = Ac*K + e Where As = sample absorption Ac = calibrated absorption K = concentration e = noise Using the above equation find K that minimizes e To minimize e we use the CLS method In this situation there are more equations then variables Classical Least Squares (CLS):  Classical Least Squares (CLS) To simplify matters we assume that e = 0 The equation then becomes: As = Ac*K Matrix form: Classical Least Squares (CLS):  Classical Least Squares (CLS) In order to solve for K (Ac-1*As = K), Ac needs to be an inverse matrix Therefore: AcT*As = (AcTAc)*K (1x1) = (1x1)*K Problems with Initial CLS Approach:  Problems with Initial CLS Approach Baseline becomes unstable throughout the day It can shift, slope, or curve These changes can be compensated for in the calibrated absorption matrix Classical Least Squares (CLS):  Classical Least Squares (CLS) Accounting for these baselines changes the equation The eqn. becomes: As = AcK1+ K2+ K3+ K4 The calibrated absorption matrix can be increased to accommodate the number of species being tested Weighted Multi-band CLS:  Weighted Multi-band CLS A more complex version of the standard CLS The spectrum is separated into bands Each band is then calculated After all the bands are calculated they are added in a weighted averaged fashion The ones with the highest error and lowest signal are counted for less then the ones with the lowest error and highest signal Hardware Description:  Hardware Description Tab 2, 3, & 4 IRGAS Systems:  IRGAS Systems Thus far the oldest system in the field without maintenance is 4 yrs Out of 20-30 systems, there has only be a need to perform maintenance on 3 of them The Bomem spectrometer is high in reliability and low in maintenance There has been 2 hardware failures There was a burned out IR source IRGAS Systems:  IRGAS Systems There is one basic package that can be dressed up in several different ways One reason our throughput is higher than competitors is because of mirror quality and coating Our objective mirrors are adjustable Sideways Rotational Competitors have mirror that are locked into place ABB Bomem WorkIR:  ABB Bomem WorkIR Manual Manifold:  Manual Manifold Manifold Parameters:  Manifold Parameters Flow Restrictor A flow of 30 psi in will give a flow of 5 slpm to the instrument Purifier Gives dry N2 to below 2 ppb Has a lifetime of more than a year if it is used 24/7 Vibrations:  Vibrations There are a number of designs of suspension systems to counteract vibrations These designs help to keep the data from being affected by a simple bump of the instrument bench Typical Gas Cells:  Typical Gas Cells Have a flow similar to turbulent flow and have a longer residence time Laminar Flow Gas Cells:  Laminar Flow Gas Cells The flow is like a waterfall Therefore there will be less turbulence Heated laminar flow gas cells The gas is in contact with the walls letting it reach a temperature similar to the gas cell prior to entering the cell Gas Cell Flow Diagrams:  Gas Cell Flow Diagrams f/5 Beam Geometry:  f/5 Beam Geometry The higher the f / #, the smaller the objective mirrors, the more light that is lost, the smaller the throughput SPGAS Software:  SPGAS Software Tab 6, 7, 8, 9, & 10 Specialty Gas Analysis Software (SPGAS):  Specialty Gas Analysis Software (SPGAS) IRGAS 100 system Collection & quantification Qmax Quantification manager IRGAS Configuration Manager Configures parameters Quantification Reprocessing Tool Recalculating spectra IRGAS 100 System:  IRGAS 100 System After opening the software the first window is the monitor screen On the right side there is the available species On the bottom is the legend of the species that are being shown in the top window The top shows the concentration of all the species over time IRGAS 100 Monitor Screen:  IRGAS 100 Monitor Screen IRGAS 100 System:  IRGAS 100 System Collecting a background After opening the program, pressing the start button will automatically send the spectrometer to collect a background and then begin collecting a sample Seeing the sample Clicking on the desired species tab at the top will show you that species in real time That screen shows the fast concentration tracker (FCT) and the averaged sample Advantages to Spectra Stream:  Advantages to Spectra Stream Provides high sensitivity detection of impurities (low ppb) Reduces the time response typically associated with FTIR (from minutes to seconds) Continuous collection of background Running average spectra Reduction in spectrometer drift Reduction of contribution of moisture System is very easy to use IRGAS Configuration Manager:  IRGAS Configuration Manager IRGAS Configuration Manager:  IRGAS Configuration Manager IRGAS Configuration Manager:  IRGAS Configuration Manager IRGAS Configuration Manager:  IRGAS Configuration Manager IRGAS Configuration Manager:  IRGAS Configuration Manager Data Retrieval:  Data Retrieval Data storage By default the data gets stored on the C drive C:\Program Files\CIC Photonics\IRGAS IRGAS data Quantification log Spectral records Quantification Log Folder:  Quantification Log Folder Data stored as a text file Can be converted to an excel file Copy file, paste in the same folder, rename with an .xls extension In the excel file Data storage names Folder with YY-MM Folder with Quan YY-MM-DD.log Spectral Records Folder:  Spectral Records Folder Stored with a .spc extension All market software writes and reads this format This was created by Galatic, now ThermoGalactic Data storage names Folder with YY-MM-DD Absorbance File Abs YY-MM-DD HH:MM.zip Background File Bck YY-MM-DD HH:MM.zip Sample File Smp YY-MM-DD HH:MM.zip Residual File Res YY-MM-DD HH:MM.zip QMax:  QMax Using existing calibration file: QMax:  QMax Quantification Set Spectral Set Calibrated Spectral Record of specific molecule Non-linear Behavior:  Non-linear Behavior As a rule of thumb a species behaves non-linear when it is higher than 0.1 a.u. The non-linear correction graph’s curve is modeled by ax3+bx2+cx+d = 0 In this equation the values that are necessary to find are a, b, and c To do this non-linear correction there needs to be at least 3 spectral records In general when the residual curve is flat line that indicates that there is non-linear behavior QMax:  QMax Starting a calibration from scratch: Synthetic Calibration Set:  Synthetic Calibration Set Instrument Line Shape (ILS) Each instrument has its own HITRAN database Contains the absorption coefficients of different components Doesn’t contain the ILS of specific instruments MALT software Created by Dr. David Griffith from the University of Wollongong in Australia Models ILS parameters MALT:  MALT Calculates spectra for single homogeneous path or for multiple layers Includes instrumental parameters into the calculations so the calculated spectra match the line shape, resolution and wavelength shift of the measured spectra Uses HITRAN molecular spectroscopy databases Gas Calibration:  Gas Calibration When a gas is not in the HITRAN system, it is necessary to produce the calibration non-synthetically Start collecting data Flush the gas cell several times with the gas During this time find the equilibrium point of each flush Take these points and average them to use for the calibration This will give a better signal to noise ratio HITRAN/MALT vs. Actual Calibration:  HITRAN/MALT vs. Actual Calibration Advantages Calibration data free of noise Best match to the measured spectrum according to the least squares criteria Operational costs reduction Non-time consuming calibrations Precision at least as good as that of traditional methods (  3%) HITRAN/MALT vs. Actual Calibration:  HITRAN/MALT vs. Actual Calibration Disadvantages Provides analysis only over gases included in the HITRAN database* System requires regeneration of calibration data if spectrometer or gas cell change *additional gases by standard calibration procedures IRGAS Spectra Reprocessing:  IRGAS Spectra Reprocessing IRGAS Spectra Reprocessing:  IRGAS Spectra Reprocessing Gas Analysis Modules:  Gas Analysis Modules Absorbance Data @ 1ppm/meter:  Absorbance Data @ 1ppm/meter Software Installation:  Software Installation Software Installation:  Software Installation The installation window should automatically pop-up After the installation has been completed, check that the computer and spectrometer are communicating with each other Establishing Communication:  Establishing Communication Network: Instrument address: 192.168.0.127 Computer address: 192.168.0.YYY Where YYY is any number between 0 and 225 that is not 127 Establishing Communication:  Establishing Communication Two Ethernet configurations: Straight through Crossover Ethernet Connection:  Ethernet Connection Straight through configuration 1 1 2 2 3 3 4 4 5 5 6 6 7 7 8 8 Ethernet Connection:  Ethernet Connection Crossover configuration 1 1 2 2 3 3 4 4 5 5 6 6 7 7 8 8 Verifying Communication:  Verifying Communication Changing network address Control panel Network connection Local network Properties Last check for communication Control panel ABB Bomem Marketing and Selling Strategies and Techniques:  Marketing and Selling Strategies and Techniques Tab 13 Worldwide Customers:  Worldwide Customers Semiconductor Applications:  Semiconductor Applications Wafer yield enhancement By reducing O-atom defects Process reaction monitoring By confirming reactants/products Supply gas quality monitoring Abatement tool efficiency Semiconductor Dry Process:  Semiconductor Dry Process http://www.jp.horiba.com/semicon_e/measurement/gas.htm Semiconductor Industry:  Semiconductor Industry Semiconductor Applications:  Semiconductor Applications A large amount is spent on equipment in the fab area In-situ monitoring is being looked at to prevent the damage of large quantities of goods The equipment section is also supplying the raw materials section, not just the Semi fab Getting the companies to upgrade current equipment is difficult but results is a large sale Chemical Applications:  Chemical Applications Specialty gas purification Combustion thermodynamics Aero-engine optimization Destructive testing: release of hazardous gases Gas blending Environmental Applications:  Environmental Applications Plant air monitoring Stack gas emissions PFC emissions Homeland Security Chemical Weapon Agents Toxic Industrial Chemicals Illicit Drugs Our Product Line:  Our Product Line FTIR gas analyzer systems Long and short path gas cells Custom gas cells Fiber optic probes (UV/VIS/NIR) Resell UV/VIS FO spectrometers FTIR sampling accessories ATR, transmission, reflectance, M-Press Competitor Analysis:  Competitor Analysis Research conducted by Los Alamos National Laboratories marketing interns Competitors and Competing Products:  Competitors and Competing Products Tab 5,12,14 Competitors:  Competitors FTIR gas analyzers MKS Instrument MIDAC Thermo Nicolet Other technologies Tiger Optics Delta F Other Technology Competitors:  Other Technology Competitors Tiger Optics Cavity Ring Down Spectroscopy (CRDS) Single gas at a time Delta F Tunable laser Single gas at a time Differentiators:  Differentiators Gas Cells:  Gas Cells Laminar flow Faster gas exchange Eliminates dead space 316L Stainless steel / Nickel plated body More chemically resistant to acid gases and retain less moisture 304 Stainless steel mirror Proprietary fabrication and coating process Radius of curvature Surface finish smoothness 98.5% reflectivity High pressure tolerance 20 atm, 300 psi Hand aligned by expert personal to maximize throughput IRGAS System:  IRGAS System Spectrometer ABB Bomem WorkIR Industrial ruggedness Compactness Very low failure rate Cost competitive Software Unique because it offers the weighted multi-band, multi-variant classical least squares method Patented on Spectra Stream w/ the fast tracker for early warning User friendly Configurations One package that can be dressed different ways Pre and post technical support Scientific Package:  Scientific Package 4Runner gas cell ABB Bomem WorkIR spectrometer Coupling optics Suspension system The 4Runner:  The 4Runner 0.6 liter volume 125 mm base path 304 stainless steel body Metal and Kalrez® seals Welded VCR fittings for gas porting Heatable to 260°C Integrated purge box with movable reference optics MgF2 protected, gold-coated stainless steel mirrors Evacuable & pressurizable: 10-4 Torr to 300 psig Ranger-EN:  Ranger-EN 9.6 meter fixed pathlength 1.7 liter cell volume 0.05 sq. m/L surface/volume Gold-coated SS mirrors All-metal, electropolished SS body External transfer optics Heatable to 200°C Optional aluminum body & glass mirror Pathfinder-EN:  Pathfinder-EN 0.4-10 meter variable pathlength Pressurizable to 50 psig Heatable to 200°C Gold-coated SS mirrors All-metal, electropolished SS body Very high energy throughput Extremely chemically-inert Scout-EN:  Scout-EN Nickel plated stainless steel 10cm gas cell for toxic and corrosive gas analyses; heated and unheated versions. 28-cm3 volume Teflon-encapsulated Viton®, Viton®, or Kalrez® O-rings for chemical resistance and temperature considerations KBr, CaF2, ZnSe, quartz, or sapphire window materials for UV-VIS and FTIR applications Evacuable and pressurizable: 10-4 Torr to 150 psig Heatable to 200°C with heating mantle, tape, or dual bands 5 cm & 15 cm pathlength versions also available Optional temperature controller Easy adaptation to all spectrometers Montero:  Montero 1.0 meter fixed pathlength 82.6 mm basepath Anodized aluminum cell body Gold-coated Pyrex mirrors Internal transfer optics Low 600 ml volume Purgeable beam conduits Swagelok (tm) gas ports Viton® O-rings Choice of windows High energy throughput Unheated and heated versions Fits totally inside FTIR compartments CR-V:  CR-V Extremely short path length 0.5mm to 1cm High Pressure Up to 100 atm Heated Option IRGAS Options:  IRGAS Options Tab 11 O-Ring Material Working Temperature Ranges:  O-Ring Material Working Temperature Ranges Window Thickness:  Window Thickness Options:  Options Pressure and temperature based on ideal gas parameters Automated manifold systems System outputs Text based Analog and digital outputs IRGAS Moisture+ Plus:  IRGAS Moisture+ Plus IRGAS-SP:  IRGAS-SP IRGAS EPI:  IRGAS EPI IRGAS 100T:  IRGAS 100T IRGAS 100MT:  IRGAS 100MT IRGAS 200RM:  IRGAS 200RM IRGAS 400:  IRGAS 400 IRGAS XFlo:  IRGAS XFlo IRGAS Worksheet:  IRGAS Worksheet Tab 13 IRGAS Worksheet:  IRGAS Worksheet Important because it guides us in system parameters, options, and price quoting Important parameters Gases present in the mixture Estimated concentrations Temperature and pressure range Sampling time The parameters help to determine: O-Ring material Window material Gas cell All of these can really vary the price of the product IRGAS Worksheet:  IRGAS Worksheet Part A of the worksheet is for customers that only want a gas cell The entire worksheet is necessary for customers that want the whole IRGAS system Customers should fill out as much of the worksheet as possible Warranties and Technical Support:  Warranties and Technical Support Tab 16 Warranty:  Warranty 1 yr parts and labor for gas cell and software 30 day on critical optical elements, ex. mirrors This is because we have no control over how the system is treated by the user 1 yr telephone and e-mail technical supprt Technical Support:  Technical Support 24/7 technical support is provided to the best of our abilities System Maintenance:  System Maintenance Tab 15 Service and Maintenance:  Service and Maintenance Handled on a case to case basis Repair, test, ship System repaired Quality tested Shipped back to customer CIC Photonics pays the shipment back to customer if still under warranty, if not it is paid both ways by the user Contact Information (505) 343-1489 (505) 343-9520 TechSupport@cicp.com :  Contact Information (505) 343-1489 (505) 343-9520 TechSupport@cicp.com

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