Hydrolysates were obtained from dilute sulfuric acid pretreatment of whole-tree softwood forest thinnings and softwood sawdust. Mid-infrared (IR) spectra were obtained on sample sets of wet washed hydrolysates, and 45°C vacuum-dried washed hydrolysates, using a Fourier transform infrared (FTIR) spectrophotometrer equipped with a diamond-composite attenuated total reflectance (ATR) cell. Partial least squares (PLS) analyiss of spectra from each sample set was performed. Regression analyses for sugar components and lignin were generated using results obtained from standard wet chemical and high-performance liquid chromatography methods. The correlation coefficients of the predicted and measured values were >0.9. The root mean square standard error of the estimate for each component in the residues was generally within 2 wt% of the measured value except where reported in the tables. The PLS regression analysis of the wet washed solids was similar to the PLS regression analysis on the 45°C vacuum-dried sample set. The FTIR-ATR technique allows mid-IR spectra to be obtained in a few minutes from wet washed or dried washed pretreated biomass solids. The prediction of the solids composition of an unknown washed pretreated solid is very rapid once the PLS method has been calibrated with known standard solid residues.

We investigated spatial non-uniformity and optical anisotropy in hydrogenated silicon thin films using infrared spectroscopy and other techniques. The films ranged in morphology from amorphous to micro-crystalline, as determined by Raman spectroscopy and X-ray diffraction (XRD). Trace element analysis of the films was carried out using secondary ion mass spectrometry (SIMS). We used polarized attenuated total reflection (ATR) measurements together with Fourier transform infrared (FTIR) spectroscopy to investigate anisotropy in the Si-H covalent bonding structure of the films, and also to detect oxide impurity phases present at certain sites in some samples. The FTIR-ATR measurements were performed using a germanium (Ge) contact microprobe with a 100-micron sampling area, as well as on films deposited on standard crystalline Si and Ge ATR substrates. The Ge contact ATR microprobe enabled relatively interference-free measurements of the IR spectra of a-Si:H and µc-Si:H films deposited on conductive substrates such as stainless steel and transparent conductive oxides, and is also sensitive to the spatial distribution of oxide precipitates in the films. This measurement is difficult or impossible using transmission or reflection IR spectroscopy.

The process of converting renewable lignocellulosic biomass to ethanol requires a number of steps, and pretreatment is one of the most important. Pretreatment usually in volves a hydrolysis of the easily hydrolyzed hemicellulosic component of biomass using some form of thermal/chemical/mechanical action that results in a product that can be further hydrolyzed by cellulase enzymes (the cellulosic portion). The sugars produced can then befermented to ethanol by fermentative microorganisms. If the pretreatment step is not severe enough, the resultant residue is not as easily hydrolyzed by the cellulase enzyme. More severe pretreatment conditions result in the production of degradation products that are toxic to the fermentative microorgan ism. In this article, wereport the quantitative analysis of glucose, mannose, xylose, and acetic acid using Fourier transform infrared (FTIR) spectroscopy on liquors from dilute-acid-pretreated softwood and hard wood slurries. Comparison of FTIR and high-performance liquid chromatography quantitative analyses of these liquorsare reported. Recent developments in infrared probe technology has enabled the rapid quantification of these sugars by FTIR spectroscopy in the batch reactor during optimization of the pretreatment conditions, or interfaced to the computer controlling a continuous reactor for on-line monitoring and control.

We grow hydrogenated amorphous silicon–germanium alloys by the hot-wire chemical vapor deposition (HWCVD) technique at deposition rates between 0.5 and 1.4 nm per second. We prepared a set of these alloys to determine the concentrations of the alloying elements as measured by various techniques. This set consists of samples throughout the range of germanium alloying from 0% (a-Si:H) to 100% (a-Ge:H). We find that by making the appropriate calibrations and corrections, our compositional measurements agree between the various techniques. Nuclear reaction analysis (NRA), Fourier transform infrared spectroscopy (FTIR)and secondary ion mass spectrometry (SIMS) all yield similar hydrogen contents, within ±20% for each sample. Electron probe micro-analysis (EPMA) and SIMS yield silicon and germanium contents within ±7% of each other with results being confirmed by Rutherford backscattering (RBS). EPMA oxygen measurements are affected by oxidized surface layers, thus these data show larger O concentrations than those measured by SIMS.