Molecular Spectroscopy In The Study of Wood & Biomass
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1 Molecular Spectroscopy In The Study of Wood & Biomass Society of Wood Science and Technology 50th Annual Convention Knoxville, Tennessee June 10, 2007 Timothy G. Rials Forest Products Center The University of Tennessee Knoxville, TN 37996
2 The Electromagnetic Spectrum Wavelength, Meters Cosmic Rays -Rays X-Ray UV Visible IR Microwave TV Radio 3x x x x10 8 Seconds Frequency,
3 Everyday Infrared Approaching the microwave region; wavelength ca. size of a pinhead ( μ) nm cm nm cm -1
4 Beer s Law The equation that relates absorbance to concentration and takes the form: Where: A = l C A = absorbance = molar absorptivity (a proportionality constant) l = pathlength of the sample C = concentration of the sample
5 Spectroscopy Instrumentation Bond Stretching Bond Bending & Wagging Spectroscopy measures interaction of light with materials Polyatomic molecule with N atoms: 3N-6 vibrations
6 Spectroscopy Instrumentation Fourier Transform Infrared (FT-IR) system Advantages Higher signal-to-noise ratio Better spectral resolution (0.01 cm -1 ) Faster (seconds instead of minutes)
7 Mid-Infrared Spectrum Aspen 0 Absorbance O-H stretching C-H stretching C=O stretching Hemicelluloses C=C stretching Lignin C-O stretching Cellulose Wavenumber (cm-1)
8 Sampling Alternatives Transmission Thin films, liquids Prepared KBr disc Reflectance Diffuse reflectance (DRIFT) Attenuated total reflectance (ATR) Variable angle Single bounce HATR
9 Attenuated Total Reflectance - IR To Detector Incoming Beam IR Wavelength Penetration Depth Incident Angle Sample Contact Effective Pathlength ATR Crystal ZnSe Ge (less efficient)
10 Diffuse Reflectance IR (DRIFT) Minimal sample prep Very high sensitivity Analyze most nonreflecting materials Analyze irregular surfaces/coatings Analyze large samples I S R Refractive index Particle size Sample homogeneity and loading Concentration Uses Kubelka-Munk model for analysis
11 Monitoring Chemical Reactions
12 FTIR Microscopy C-H Stretching (2950 cm -1 ) Acid-Salt (1552 cm -1 ) Very versatile sampling capability μm Open ring (1712 cm -1 ) m μ m μ μm Anhydride (1788 cm -1 ) Sample modes incl. transmission reflectance attenuated total reflectance Visual maps available μm μm
13 Spectrum Spotlight Imaging Imaging at 6.25 and 25 micron resolution Mapping and line-scan modes Variable aperture, single-point microscope ATR
14 The FTIR Image Hypercube n m Chemical images can be created from the total absorbance, and from absorbance data for each wavelength (wavenumber). Image (y) Wavenumber (cm -1 ) Image (x)
15 FTIR Imaging of Wood Total Absorbance bark xylem to the pith Bark Phloem cambium xylem Radial section of the control sample 2000x2000 μm Absorbance at 1324 cm-1
16 PP/MAPP/Lubricant (1775 cm -1 ) Visible Image: apparent defect in polypropylene Amorphous zone between crystals nucleated from the wood surface and free crystals in the bulk of polymer. Chemical Image: very strong IR absorption for wood silver; increased absorption in defect region Concentration buildup of lubricant and coupling agent in the amorphous region
17 Chemical Data from Images MAPP-70/ ZnSt-30 Point mode 2 scan avg.; 8 cm -1 MAPP Decrease in C=O anhydride stretch at 1775 cm -1 Increase in C=O stretch of acid at 1712 cm -1 Indicates lubricant interference Zinc Stearate cm-1
18 Quantitative Analysis of Wood Bondlines
19 Quantitative Analysis of Wood Bondlines
20 ATR Imaging System Spectral performance (S/N) Image size and flexibility Ultimate spatial resolution Ease of use Background handling Information retrieval from images
21 ATR Imaging/Processing Paint Chip Image (200 m by 300 m,, 1.56 m pixel 8 cm -1, 16 scans / pixel) Processing: spectral differential, average subtract, PCA, colour compositing
22 Near Infrared Spectroscopy Advantages Fast data acquisition Versatile sampling Affordable technology Raw material information Absorbance DF Long PP Slash Limitations Difficult visual interpretation Too much data! Wavelength (nm)
23 NIR Band Assignments Second Overtone Region Combination Band Region Third Overtone Region First Overtone Region H O 2 H O 2 H O 2 H O 2 ROH ROH ROH RCO H 2 RCO R 2 ROH ArOH RNH 2 ArOH RNH 2 ArOH CONH 2 RNH 2 POH RNH 2 ArCH RNHR ArCH ArCH CONHR ArCH SH CONH 2 CONH 2 (H) CH CH CH CH CH CHO CH CH 2 CH 2 CH 2 CH 2 CH 2 CC CH 2 CH 3 CH 3 CH 3 CH 3 CH 3 CH ,100 1,300 1,500 1,700 1,900 2,100 2,300 2,500 Wavelength (nm)
24 NIR Spectra of Materials Distinctive peaks found at 2280, 1707 and 1215 nm I t it Wavelength (nm) PP no MAPP PE no MAPE PP w/ MAPP PE w/ MAPE Related to CH substitution patterns in polyolefins No obvious differences with coupling agent addition
25 Principal Component Analysis
26 Projection to Latent Structures Perform simultaneous extraction of orthogonal latent vectors that explain the variance of both matrices PLS Model
27 NIR/MVA Characterization of Wood Composition Measured with py- MBMS (wt%) Glu Lig Ext Measured Chemical Composition (wt%) Strength (MOR) Predicted with NIR (MPa) Lob Slash Long Short Measured Strength (MOR) (MPa) Fully cross-validated models for robustness Utilize calibration and validation set to evaluate performance Ensure data encompasses the full range of variable space
28 NIR Prediction of Internal Bond (Interior Spectra) 800 R = 0.86; % RMSEP = Measured Internal Bond (kpa) Calibration Validation
29 Reduced Wavelength Models Wavelength (nm) R=0.93 RMSEP= Wavelength (nm) R=0.79 RMSEP= Wavelength (nm) R=0.91 RMSEP= Measured MOE (MPa) Measured MOE (MPa) Measured MOE (MPa)
30 NIR Sampling Methods Field Sampling Process Monitoring
31 Summary Remarks Infrared spectroscopy offers unrivaled versatility in sampling Advances in technology have expanded access to data/information Near infrared has emerged as a valuable analytical instrument for wood products Quantitative analysis of IR data expanded using multivariate statistics IR is relevant to all stages of wood use: (1) raw material, (2) furnish, (3) QA/QC, and (4) lifecycle or in-service
32 For Additional Information References H. Martens and T. Naes. Multivariate Calibration, Wiley, New York Ciurczik, et al. Hdbk. Of NIR Spectroscopy. Mfr. Web Sites Foss NIR ( Analytical Spectral Devices ( Bruker Optics ( Ocean Optics ( PerkinElmer Instr. ( Thermo-Nicolet ( Spectral Dimensions ( Camo (
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