Fourier Transform Infrared. Spectrometry

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1 Fourier Transform Infrared. Spectrometry Second Editio n PETER R. GRIFFITH S JAMES A. de HASETH

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3 PREFACE x v CHAPTER 1 INTRODUCTION TO VIBRATIONAL SPECTROSCOPY Introduction Molecular Vibrations Vibration-Rotation Spectroscopy Widths of Bands and Lines in Infrared Spectra Vibration-Rotation Spectra of Gases Spectra of Condensed-Phase Samples Quantitative Considerations Beer's Law Optical Constants Polarized Radiation Raman Spectrometry Summary 1 8 CHAPTER 2 THEORETICAL BACKGROUND Michelson Interferometer Generation of an Interferogram Effect of Finite Resolution Apodization Phase Effects Effect of Beam Divergence Effect of Mirror Misalignment Effect of a Poor Mirror Drive Rapid-Scan Interferometers Step-Scan Interferometers 53

4 CHAPTER 3 SAMPLING THE INTERFEROGRAM Sampling Frequency Nyquist Frequency Conceptual Discussion of Aliasing Mathematical Discussion of Aliasing Aliasing Dynamic Range ADC Specifications Digitization Noise Gain Ranging Chirping Analog-to-Digital Converters 7 1 CHAPTER 4 FOURIER TRANSFORMS Classical Fourier Transform Elementary Concepts Mathematical Basis Fast Fourier Transform Phase Correction Fourier Transform : Pictorial Essay Data Systems 9 3 CHAPTER 5 TWO-BEAM INTERFEROMETERS Michelson-Type Interferometers Introduction Drive Bearings Fringe Referencing Dynamic Alignment Tilt-Compensated Interferometers Cube-Corner Interferometers Other Designs Refractively Scanned Interferometers Polarization Interferometers Step-Scan Interferometers Stationary Interferometers Beamsplitters 132

5 5.8. Lamellar Grating Interferometers 13 8 Appendix: Manufacturers of FT-IR Spectrometers 142 CHAPTER 6 OTHER COMPONENTS OF FT-I R SPECTROMETERS Infrared Radiation Sources for Transmissio n and Reflection Spectrometry Mid-Infrared Sources Near-Infrared Sources Far-Infrared Sources Detectors Thermal Detectors Quantum Detectors Optics Paraboloidal Mirrors Plane Mirrors Ellipsoids, Toroids, and Other Aspherical Mirrors Spectrometer Design 15 6 CHAPTER 7 SIGNAL-TO-NOISE RATIO Detector Noise Trading Rules in FT-IR Spectrometry Effect of Resolution an d Throughput on SNR Effect of Apodization Effect of Changing Mirror Velocity Digitization Noise Other Sources of Noise Sampling Error Folding Fluctuation Noise Shot Noise Interferometers Versus Grating Spectrometers Fellgett's Advantage Jacquinot's Advantage Other Factors 173

6 CHAPTER 8 PHOTOMETRIC ACCURACY IN FT-IR SPECTROMETRY Introduction Effect of Spectral Resolution Effect of Apodization Triangular Apodization Norton-Beer Apodization Functions % Lines Short-Term Performance Glitches (Nonrandom Noise Sources) Long-Term Performance Effect of Sample Diameter and Thickness Zero Energy Level Detector Response Nonlinearity Changes in Modulation Efficiency Sampling Effects Linearity Between 100% and 0%T 194 CHAPTER 9 QUANTITATIVE ANALYSIS Introduction Beer's Law Spectral Subtraction Linear Least-Squares Fitting Methods Classical Least Squares Inverse Least-Squares Regression Principal Component Analysis Principal Component Regression Partial Least-Squares Regression Validation Multivariate Curve Resolution General Guidelines for Calibration Data Sets Neural Networks 22 1 CHAPTER 10 DATA PROCESSING Baseline Correction Interpolation Peak Picking Spectral Smoothing 232

7 10.5. Band Fitting Derivatives of Spectra Fourier Self-Deconvolution Spectral Searching 24 6 CHAPTER 11 CONVENTIONAL TRANSMISSIO N SPECTROMETRY Condensed-Phase Samples Window Materials Band Intensities Interference Fringes Trace Analysis Gas- and Vapor-Phase Samples 25 6 CHAPTER 12 POLARIZATION Plane-Polarized Radiation Circular Polarization Polarization Modulation Applications of Linear Dichroism Vibrational Circular Dichroism 26 9 CHAPTER 13 SPECULAR REFLECTION Introduction Fresnel Reflection from Bulk Samples Fresnel Equations Nonabsorbing Materials Absorbing Materials Infrared Reflection-Absorption Spectrometry with Metal Substrates Effect of Incidence Angle and Polarization Polarization Modulation Surface Selection Rule IRRAS with Dielectric Substrates Transflection Thick Films on Metal Substrates Liquid Sampling for Near-Infrared Spectrometry Summary 300

8 CHAPTER 14 MICROSPECTROSCOPY AND IMAGING Microsampling with Beam Condensers Microscopes Diamond Anvil Cells Reflection Microscopy Hyperspectral FT-IR Imaging Hyperspectral Imaging with a Step-Scanning Interferometer Hyperspectral Imaging with a Continuous-Scanning Interferometer Signal-to-Noise Ratio Software Applications of Hyperspectral Imaging 319 CHAPTER 15 ATTENUATED TOTAL REFLECTION Introduction Theory Practical Considerations Accessories for Multiple Internal Reflection Single-Reflection Accessories Infrared Fibers Summary 347 CHAPTER 16 DIFFUSE REFLECTION Theory of Diffuse Reflection Accessories for Diffuse Reflection Applications of Mid-Infrared Diffus e Reflection Spectrometry Applications of Near-Infrared Diffuse Reflection Spectrometry Reference Materials for Diffuse Reflectio n Spectrometry 36 1 CHAPTER 17 EMISSION Introduction Infrared Emission Spectra of Gases 363

9 17.3. Infrared Emission Spectra o f Condensed-Phase Samples Transient Infrared Emission Spectroscopy 36 8 CHAPTER 18 FOURIER TRANSFORM RAMAN SPECTROMETRY Introduction Instrumentation Nd : YAG Laser Filters Collection Optics Interferometer Detector Spectrometer FT Raman Versus CCD Raman Spectrometry Applications of FT-Raman Spectrometry Standard Raman Spectroscopy Surface-Enhanced Raman Spectroscopy Summary 39 1 CHAPTER 19 TIME-RESOLVED SPECTROMETRY Continuous-Scanning Interferometers Instrumental Considerations Applications Time-Resolved Measurements Using Step-Scan Interferometers Instrumental Considerations Applications of Time-Resolve d Spectroscopy with a Step-Sca n Interferometer Stroboscopic Spectrometry Asynchronous Time-Resolved Ff-I R Spectrometry Instrumental Considerations Application to Liquid-Crystal Orientation Dynamics 412

10 CHAPTER 20 PHOTOACOUSTIC SPECTROMETRY Photoacoustic Spectroscopy of Gases Photoacoustic Spectroscopy of Solids with a Rapid-Scanning Interferometer Photoacoustic Spectroscopy of Solids with a Step-Scan Interferometer Phase Modulation Depth Profiling by Varying th e Photoacoustic Phase Multifrequency Measurements 43 1 CHAPTER 21 SAMPLE MODULATION SPECTROMETR Y WITH A STEP-SCAN INTERFEROMETER Dynamic Infrared Linear Dichroism Measure d with a Monochromator DIRLD Spectrometry with a Step-Scan Fourier Transform Spectrometer Two-Dimensional Correlation Plots DIRLD Spectrometry with a FT-IR Spectrometer y and Digital Signal Processing Other Sample Modulation Measurement s with Step-Scan Interferometers Liquid-Crystal Electroreorientation Infrared Spectroelectrochemistry 46 0 CHAPTER 22 ATMOSPHERIC MONITORING Extractive Atmospheric Monitoring Open-Path Atmospheric Monitoring 46 6 CHAPTER 23 COUPLED TECHNIQUES Introduction Light-Pipe-Based GC/FT-IR Interfaces Instrumental Considerations Spectroscopic Considerations Chromatogram Construction Example of GC/FT-IR Mobile-Phase Elimination Approaches for GC/FT-IR 491

11 Introduction Matrix Isolation G0Fr-4R Direct Deposition,GCYI'T-IR HPLC/Ff-IR interface Measurements Made with Flow Cells Mobile-Phase Ceimination Technique s Cot I-1PLCl' :'=' SFC/FT-IR Interact TGA/Fi'-IR Other Coupled Tetbiwes 504 INDEX 509

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