Analysis of texture and microstructure of anatase thin films by Fourier transform infrared spectroscopy

This work provides the basis for a “fingerprint” analysis of the microstructure and the texture of anatase thin films by using Fourier transform infrared spectroscopy. For this, a formalism that reproduces the experimental spectra has been developed and its applicability is analysed for anatase thin films with different microstructure (columnar and porous, with varying degrees of compactness) and texture. The rather good agreement between calculated and experimental spectra observed in all cases demonstrated that a systematic use of this non-destructive technique can be very useful for the characterization of thin films.     

傅立叶变换红外光谱法分析市售食品中反式脂肪酸

建立了一种快速测定食品中反式脂肪酸含量的方法,用索氏提取法或氯仿—甲醇提取法提取食品中脂肪,经甲醇-BF3快速甲酯化后,采用Avatar 370傅立叶变换红外光谱对反式脂肪酸进行定性定量分析,回收率为89.5%~103.3%,相对标准偏差为1.80%,重复性好,准确度高,适用于一般食品营养标签的测定。对我国市场上的涂抹奶油、派和蛋糕、饼干、巧克力、冰淇淋、薯片和薯条等6大类食品中20种样品中反式脂肪酸进行测定。结果表明,16种检出样品中反式脂肪酸含量在0.18%~10.34%之间,反式脂肪酸含量随食品种类不同存在显著差异,涂抹奶油、蛋黄派、威化饼干是反式脂肪酸含量较高的食品类别。     

Determining cement composition by Fourier transform infrared spectroscopy

A diffuse reflectance mid-infrared Fourier transform spectroscopy (DRIFTS) method is described for obtaining high quality Fourier transform infrared (FTIR) spectra of cements. DRIFT spectra of synthetic C₃S, C₂S, C₃A, and C₄AF and of pure gypsum, bassanite, anhydrite, syngenite, and calcite are shown. Typical spectra of American Petroleum Institute class G and class A cements display characteristic features which can be related qualitatively to variations in the constituent minerals. For quantitative analysis, the FTIR spectra of 156 cements of varied origin and known elemental composition have been used to construct multivariate calibration models. These relate the spectrum to composition (expressed in terms of nine mineral components and five minor oxides) and allow the composition of unknown cements to be determined rapidly from the FTIR spectrum alone. Error estimates are given.     

Thermal imidization optimization of polyimide thin films using Fourier transform infrared spectroscopy and electrical measurements

The influence of the imidization temperature on the molecular structure and on the thermal and electrical properties of polyimide thin films is investigated. The effects of the imidization temperature on the formation of the imide rings are studied by Fourier transform infrared (FTIR) spectroscopy through the changes of the extent of imidization. However, the determination of the optimal imidization temperature shows a poor accuracy through this technique. Therefore, the quantification of several electrical properties used as probes of the imidization reaction advancement (particularly high field electrical measurements) allows obtaining a highest accuracy of the optimal imidization temperature. An optimum temperature is found at 400 °C while desimidization is observed at 450 °C. This is in good agreement with FTIR results.     

Quantitative analysis of polyethylene blends by Fourier transform infrared spectroscopy

The quantitative analysis of binary polyethylene (PE) blends by Fourier transform infrared (FT-IR) spectroscopy has been achieved based on the ratio of two absorbance peaks in an FT-IR spectrum. The frequencies for the absorbance ratio are selected based on structural entities of the PE components in the blend. A linear relationship between the absorbance ratio and the blend composition was found to exist if one of the absorbance peaks is distinct to one of the components and the other peak is common to both components. It was also found that any peak resulting from short-chain branching in copolymers (such as linear low-density polyethylene (LLDPE) or metallocene-catalyzed LLDPE (mLLDPE)), is suitable for use as the peak that is designated as being distinct to that component. In order to optimize the linearity of the equation, however, the selection of the second common peak is the most important and depends on the blend system studied. Indeed, under certain circumstances peaks that are not spectrally distinct can be used successfully to apply the method. The method exhibits potential for the routine analysis of PE blends that have been calibrated prior to its application.     

Fourier transform spectroscopy of LaS in the infrared

We recorded the emission spectrum of diatomic lanthanum sulfide on the Los Alamos Fourier transform spectrometer. In the region 7500-16,000 cm(-1), we identified over 120 bands and assigned them to the A(2)∏(r)-X(2)Σ(+) and B(2)Σ(+)-X(2)Σ(+) transitions. Each of these bands is four headed.     

Near infrared absorption coefficient of molten glass by emission spectroscopy

Emission spectroscopy is applied in the determination of the near infrared spectral absorption coefficient of molten glass. The glass is held in a small horizontal platinum alloy crucible, within an electrically heated cell, optically coupled to a Fourier transform spectrometer. A formula is derived which relates emissivity to absorption coefficient, thickness, and reflectivities for the glass-air and glass-metal interfaces. The reflectivity parameters are determined, in effect, by varying the thickness. Spectral absorption coefficient results are compared with results of transmission spectroscopy. The emission technique is advantageous in that it eliminates the problem of chemical reactions with window materials used in the transmission method, and sample preparation and interfacing to commercially available spectrometers is simplified.     

Quantitative determination of moisture in lubricants by Fourier transform infrared spectroscopy

This paper describes the development of a practical Fourier transform infrared (FT-IR) method for the determination of moisture in lubricants through the combined use of signal transduction and differential spectroscopy to circumvent matrix effects. The acid-catalyzed stoichiometric reaction of 2,2-dimethoxypropane (DMP) with moisture to produce acetone was used to provide IR signals proportional to the amount of moisture present in oils. Calibration standards were prepared by spiking polyalphaolefin (PAO) gravimetrically with water using dioxane as a carrier. For FT-IR analysis, standards and samples were diluted with acidified isooctane and then split, with one aliquot treated with DMP and the other with a blank reagent. The spectra of the two aliquots were collected, and a differential spectrum was obtained so as to ratio out the invariant spectral contributions from the sample. Quantitation for moisture was based on measurement of the peak height of the nu(C=O) absorption of acetone at 1717 cm(-1), yielding a standard error of calibration of approximately 40 ppm H2O. The method was validated by standard addition of water in dioxane to PAO containing added base as well as to new and used oils. In all cases the method responded quantitatively to standard addition, the average standard error of prediction being approximately 80 ppm, with the results showing only a minor dependence on the oil formulation. From an analytical perspective, the FT-IR method is both more reproducible and more accurate than Karl Fischer methods and has advantages in terms of environmental considerations, sample size, and speed of analysis as well as the variety of oil types that can be handled. Signal transduction/differential spectroscopy may have broader utility as an alternative means for the determination of low levels of moisture in complex matrices.     

Study of a chemically amplified resist for X-ray lithography by Fourier transform infrared spectroscopy

Future applications of microelectromechanical systems (MEMS) require lithographic performance of very high aspect ratio. Chemically amplified resists (CARs) such as the negative tone commercial SU-8 provide critical advantages in sensitivity, resolution, and process efficiency in deep ultraviolet, electron-beam, and X-ray lithographies (XRLs), which result in a very high aspect ratio. In this investigation, an SU-8 resist was characterized and optimized for X-ray lithographic applications by studying the cross-linking process of the resist under different conditions of resist thickness and X-ray exposure dose. The exposure dose of soft X-ray (SXR) irradiation at the average weighted wavelength of 1.20 nm from a plasma focus device ranges from 100 to 1600 mJ/cm(2) on the resist surface. Resist thickness varies from 3.5 to 15 mum. The cross-linking process of the resist during post-exposure bake (PEB) was accurately monitored using Fourier transform infrared (FT-IR) spectroscopy. The infrared absorption peaks at 862, 914, 972, and 1128 cm(-1) in the spectrum of the SU-8 resist were found to be useful indicators for the completion of cross-linking in the resist. Results of the experiments showed that the cross-linking of SU-8 was optimized at the exposure dose of 800 mJ/cm(2) for resist thicknesses of 3.5, 9.5, and 15 microm. PEB temperature was set at 95 degrees C and time at 3 min. The resist thickness was measured using interference patterns in the FT-IR spectra of the resist. Test structures with an aspect ratio 3:1 on 10 microm thick SU-8 resist film were obtained using scanning electron microscopy (SEM).     

Prion protein alpha-to-beta transition monitored by time-resolved Fourier transform infrared spectroscopy

The conformational change of the recombinant, murine prion protein (PrP) from an alpha-helical to a beta-sheet enriched state was monitored by time-resolved Fourier transform infrared (FT-IR) spectroscopy. The alpha-to-beta transition is induced by reduction of the single disulfide bond in PrP. This transition is believed to generate the scrapie form PrP(Sc), the supposed infectious agent of transmissible spongiform encephalopathies. We followed the kinetics of this conformational change using a novel method for amide I band analysis of the infrared (IR) spectra. The amide I analysis provides the secondary structure. The amide I decomposition was calibrated with the three dimensional structure of cellular PrP solved by nuclear magnetic resonance (NMR). The novel secondary structure analysis provides a root mean squared deviation (RMSD) of only 3% as compared to the NMR structure. Reduction of alpha-helical PrP caused the transient accumulation of a partially unfolded intermediate, followed by formation of a state with higher beta-sheet than alpha-helical structure contents. The novel approach allows us to now determine the secondary structure of the beta-sheet conformation. This was not determined by either NMR or X-ray. The experiments were performed in a double-sealed security cuvette developed for IR analysis of potentially infectious PrP samples outside the biosafety laboratory.     

Fourier transform infrared spectroscopy characterization of AlN thin films grown on sacrificial silicon oxide layers via metal organic vapor phase epitaxy

Aluminum nitride (AlN) films were grown using metal organic vapor phase epitaxy techniques on Si (111) substrates patterned with silicon oxide (SiO_x) stripes and the vibrational properties of these films were investigated by Fourier transform infrared (FTIR) techniques. The grown films contained a predominantly wurtzite AlN phase. The AlN film on SiO_x was prone to corrosion when subjected to wet etching in buffered hydrofluoric acid solution thereby changing the material properties of the AlN film on SiO_x. The change in the material properties of the AlN films on SiO_x can be gauged from the decrease in the relative integrated areas under the A1 (TO) and E1 (TO) modes of the AlN film. The analysis shows that FTIR is a viable tool for investigating the material properties of AlN thin film structures with lateral dimensions as low as 100 μm.     

Characterization of magnetic paper using Fourier transform infrared spectroscopy

Magnetic papers were prepared by using the co-precipitation method. The spectral data of the magnetic fibres were obtained by using the photoacoustic Fourier transform infrared spectroscopy (FTIR-PAS) and attenuated total reflection (ATR). It was found that the elevated loading degree increased the IR absorption and reduced the tensile strength of the paper. The partial-least-squares analyses showed that the FTIR-ATR data were strongly correlated with the degree of loading and the correlation obtained was better than that of the FTIR-PAS spectral data.     

Identification of scrapie infection from blood serum by Fourier transform infrared spectroscopy

We describe a new Fourier transform infrared (FT-IR) spectroscopy-based diagnostic approach, which may provide for the first time a rapid, reliable, and inexpensive blood test for scrapie and related transmissible spongiform encephalopathies (TSE). Blood serum from 146 terminally ill Syrian hamsters infected with 263K scrapie via different routes of inoculation and from 166 healthy control animals was analyzed by FT-IR spectroscopy and artificial neural networks (ANN). This revealed characteristic molecular alterations in the serum of infected donors. Different ANN models were constructed and challenged with previously unknown samples in test runs in order to establish whether the new method is able to discriminate between normal and infected animals. Optimized ANNs consistently yielded test sensitivities and specificities of 97% and 100%, respectively. The predictive value of a positive (negative) test was 100% (98%). The proposed serum test circumvents substantial drawbacks of conventional TSE diagnostics and can be fully automated.     

Fourier transform infrared spectroscopic estimation of crystallinity in SiO<Subscript>2</Subscript> based rocks

We present here optical properties and crystallinity index of quartz (SiO₂) in natural rocks samples from the Mikir and Khasi hills, Assam, India. Infrared spectroscopy has been used to study the structure of quartz in rock samples and estimate the mining quality of quartz mineral, which is substantiated by calculating the crystallinity index. Systematic investigations of structure have been carried out in between 10 μm (1000 cm⁻¹) and 20 μm (500 cm⁻¹) bands of silicates. Investigation is based on the assignment of infrared bands to certain structural groups of SiO₄ tetrahedra. The crystallinity of samples has been ascertained by comparing the ratio of intensity of the characteristic peak at 778 and 695 cm⁻¹ with the corresponding ratio for a standard sample. The crystallinity parameter is calculated by using a standard procedure which can be used to estimate the distribution of quartz in various rocks for mining purpose. The infrared spectroscopic investigation is found to be an ideal tool for structure elucidation and for estimating quartz crystallinity of the natural samples.     

Application of Fourier transform infrared spectroscopy in cement Alkali quantification

Alkali in cement is responsible for the Alkali–silica-reaction phenomenon that manifests itself in the form of premature cracking in concrete structures such as bridge decks and concrete pavements. X-ray fluorescence spectroscopy (XRF) is commonly used for cement Alkali quantification but a simpler and faster analytical procedure based on Fourier transform infrared spectroscopy (FTIR) has been expanded for this purpose. An analytical absorption band at 750 cm^?1 in the FTIR spectra of cement samples belonging to Alkali solid solution of tricalcium aluminate [C₃A(ss)] is used for Alkali quantification. Regression analysis of a plot correlating FTIR absorption band area ratio (750/923 cm^?1) to equivalent Alkali Na₂O _e (Na₂O _e  = % Na₂O + 0.658 × % K₂O) measured by XRF shows a linear correlation coefficient, R ², of 0.97. High Alkali cement samples show a higher microstructural disorder coefficient, C _d, which is a reactivity criterion introduced by Bachiorrini and co-authors (Proceedings of the seventh international conference on concrete alkali-aggregate reactions? 1986) for ASR-susceptible aggregates. Results of this research indicate applicability of FTIR technique to quantitatively predict cement vulnerability to ASR through the \( A_{{750\,{\text{cm}}^{ - 1} }} \) to \( A_{{923\,{\text{cm}}^{ - 1} }} \) band area ratio and the magnitude of the disorder coefficient (C _d).     

Characterization of infrared matrix-assisted laser desorption ionization samples by Fourier transform infrared attenuated total reflection spectroscopy

Fourier transform infrared attenuated total reflection (FT-IR ATR) spectroscopy was used to characterize thin films of succinic acid, a matrix compound commonly used with infrared matrix-assisted laser desorption ionization (IR-MALDI) mass spectrometry. IR spectra of succinic acid thin films deposited alone and in combination with the analyte biomolecules insulin and cytochrome c were obtained by FT-IR ATR spectroscopy. Spectra of analyte and matrix alone were similar to those obtained previously from KBr pellets, Nujol mull, or thin-film absorption, although the ATR spectra have significantly lower background interferences. Thin films deposited from mixtures of water and methanol have additional peaks compared to films deposited from a methanol solution. These additional peaks are attributed to carboxylate groups stabilized by residual water molecules. No evidence was found to suggest that residual water absorption contributes to absorption at wavelengths typically used for IR-MALDI. Absorption of energy by analyte vibrational modes with rapid energy transfer to the matrix is suggested as a contributor to desorption and ionization consistent with the FT-IR ATR results.     

Fourier transform infrared spectroscopy of size-segregated aerosol deposits on foil substrates

A method based on Fourier transform infrared (FTIR) double-pass transmittance spectroscopy was developed for determining functional group loading in size-segregated ambient aerosol deposits. The impactor employed for sample collection utilized rotating stages, which produced uniform particulate matter (PM) deposits on standard Al foil substrates. Each sample was analyzed without extraction using an FTIR spectrometer equipped with a reflectometer accessory. The use of the reflectometer obviated the need for infrared window materials as substrates. (NH(4))(2)SO(4) aerosol generated under laboratory conditions were used to calibrate deposit mass to the band strength of the relatively isolated nu(4) bending mode of SO(2-)(4) centered near 620 cm(-1). Atmospheric PM was sampled during the summer of 2004 in Huntsville, Ala. Sulfate concentrations determined in this initial study correlated well with measurements made by collocated EPA air samplers.     

Fluorescence lifetime imaging and Fourier transform infrared spectroscopy of Michelangelo's David

We developed a combined procedure for the analysis of works of art based on a portable system for fluorescence imaging integrated with analytical measurements on microsamples. The method allows us to localize and identify organic and inorganic compounds present on the surface of artworks. The fluorescence apparatus measures the temporal and spectral features of the fluorescence emission, excited by ultraviolet (UV) laser pulses. The kinetic of the emission is studied through a fluorescence lifetime imaging system, while an optical multichannel analyzer measures the fluorescence spectra of selected points. The chemical characterization of the compounds present on the artistic surfaces is then performed by means of analytical measurements on microsamples collected with the assistance of the fluorescence maps. The previous concepts have been successfully applied to study the contaminants on the surface of Michelangelo's David. The fluorescence analysis combined with Fourier transform infrared (FT-IR) measurements revealed the presence of beeswax, which permeates most of the statue surface, and calcium oxalate deposits mainly arranged in vertical patterns and related to rain washing.     

Stability of Nextel fibres in aqueous environments detected by photoacoustic Fourier transform infrared spectroscopy

Photoacoustic Fourier transform infrared spectroscopy was utilized to monitor the effect of basic, acidic and neutral aqueous environments on the stability of Nextel ceramic fibres. Such treatments led to the removal of a residual hydrocarbon phase from the fibre and formation of boric acid. The presence of boric acid upon the treatment does not effect the stability of the fibre at high temperatures. At high temperatures, B(OH)₃ is apparently converted to B₂O₃, this process enhancing the surface stability and improving the adhesive properties of fibres to the polymer matrix.