Determination of ethenzamide and acetoaminophen in quaternary powdered samples by near infrared spectroscopy and searching combination moving window partial least squares algorithm: effects of spectral resolution and signal-to-noise ratio

The present study reports an application of the searching combination moving window partial least squares (SCMWPLS) algorithm to the determination of ethenzamide and acetoaminophen in quaternary powdered samples by near infrared (NIR) spectroscopy. Another purpose of the study was to examine the instrumentation effects of spectral resolution and signal-to-noise ratio of the Buchi NIRLab N-200 FT-NIR spectrometer equipped with an InGaAs detector. The informative spectral intervals of NIR spectra of a series of quaternary powdered mixture samples were first located for ethenzamide and acetoaminophen by use of moving window partial least squares regression (MWPLSR). Then, these located spectral intervals were further optimised by SCMWPLS for subsequent partial least squares (PLS) model development. The improved results are attributed to both the less complex PLS models and to higher accuracy of predicted concentrations of ethenzamide and acetoaminophen in the optimised informative spectral intervals that are featured by NIR bands. At the same time, SCMWPLS is also demonstrated as a viable route for wavelength selection.

Self-assembled monolayer growth of octanol on mica: Atomic force microscopy and Fourier-transform infrared spectroscopy studies

The growth kinetics of self-assembled monolayers formed by exposing freshly cleaved mica to octanol solution has been studied by atomic force microscopy (AFM) and Fourier-transform infrared spectroscopy (FTIR). AFM images of samples immersed in octanol for varying exposure times showed that before forming a complete monolayer the octanol molecules aggregated in the form of small islands on the mica surface. With the proceeding of immersion, these islands gradually grew and merged into larger patches. Finally, a close-packed film with uniform appearance and few defects was formed. The thickness of the final film showed 0.8 nm in height, which corresponded to the 40degrees tilt molecular conformation of the octanol monolayer. The growth mechanisms consisted of nucleation, growth, and coalescence of the submonolayer films. The growth process was also confirmed by FTIR. And the surface coverage of the submonolayer islands estimated from AFM images and FTIR spectra as a function of immersion time was quite consistent.

Infrared spectrum of 2-octadecyl-7,7,8,8-tetracyanoquinodimethane

Infrared spectrum of 2-octadecyl-7,7,8,8-tetracyanoquinodimethane was dealt with 2nd-derivative and deconvolution methods. It was first discovered that the band near 2849 cm(-1) assigned to the CH2 Symmetric stretching mode splited into two bands and this splitting might result from the coexistence of two kinds of conformations of CH2 in the hydrocarbon chain.

Infrared and MAS NMR spectroscopic studies of Al18B4O33

The IR spectrum and B-11 and Al-27 MAS NMR spectra of Al18B4O33 are presented and discussed in relation to the possible existence of boron atoms substituting for aluminum atoms. The IR spectrum shows that the strong vibrations of the BO3 groups are present in the 1 500 similar to1 200 cm(-1) region, and very weak bands of BO4 units art present in the region from 1 000 to 1 100 cm(-1). B-11 MAS NMR spectrum indicates that the strong signal for BOB units appears in the region from delta +5 to delta +20, and the very weak signal for BO4 units is at about delta -1, while Al-27 MAS NMR spectrum shows five peaks at about delta +62, +42.1, +14, -4.7 and -6.4, originating from AlO4, AlO4, AlO5, AlO6 and AlO6, respectively, These results reveal that there are minor BO4 units in Al18B4O33, indicating that a small amount of B atoms substitute for Al atoms in the 4-fold coordination.

1.54 mu m infrared photoluminescence and electroluminescence from an erbium organic compound

Infrared emission at 1.54 mu m excited optically and electrically from an erbium organic compound tris(acetylacetonato)(1,10-phenanthroline) erbium [Er(acac)(3)(phen)] is observed. The rare-earth complex is dispersed into a polymer matrix of poly(N-vinylcarbazole) (PVK) to fabricate an electroluminescent (EL) device with an ITO/PVK:Er(acac)(3)(phen)/Al:Li/Ag structure, where ITO represents indium-tin-oxide-coated glass. The device shows infrared EL emission at 1.54 mu m, which suggests a simple and cheap method to obtain a light source for 1.54-mu m-wavelength devices in optical communications. (C) 2000 American Institute of Physics. [S0021-8979(00)00301-7].

Investigation of thermal unfolding process of cyanic adduct of horseradish peroxidase by Fourier transform infrared and circular dichroism spectrometry

Detailed circular dichroism(CD) and Fourier transform infrared (FTIR) studies have been carried out to monitor thermal unfolding of horseradish peroxidase isoenzyme C(HRP) inhibited by CN(HRP-CN). The results suggest that HRP-CN is quite different from native HRP with different spin states of Fe of heme and different coordinated states. Cyanide becomes the sixth ligand of Fe(I) of heme and the hydrogen-binding network is destroyed partly at the same time, which cause the drastic decrease of thermal stability of HRP. The FTIR and Soret-CD spectra analysis demonstrate that during the heating process there is an intermediate state(I') which has both partly destroyed secondary and tertiary structures of native HRP, then it is the appearance of protein aggregation state(A) after fully unfolding. The unfolding pathway thus can be shown as follows: I -->I'-->U -->A.

Infrared spectra and VUV excitation properties of BaLnB(9)O(16): Re (Ln = La, Gd; Re = Eu, Tb)

The infrared spectra of BaLnB(9)O(16):Re, along with the VUV excitation spectra, have been measured. The spectra were tentatively interpreted in terms of the data on absorptions of the borate groups and band structure. It was observed that there are absorption due to BO3 and BO4 groups, indicating that there are BO3 and BO4 groups in BaLnB(9)O(16). It is found that absorption of the borate groups is located in the range from 120 to 170 mn. This result reveals that there is an energy transfer from host to the rare earth ions. It also observed that the energy of charge transfer band, the host absorption, the total crystal field splitting of d-levels of Tb3+ increase with the decrease in the Ln(3+) radius. (C) 2001 Elsevier Science B.V. All rights reserved.

In situ infrared spectroelectrochemical studies on adsorption and oxidation of nucleic acids at glassy carbon electrode

The adsorption and oxidation of yeast RNA and herring sperm DNA (HS DNA) at glass carbon (GC) electrode are studied by differential pulse voltammetry (DPV) and in situ FTIR spectroelectrochemistry. Two oxidation peaks of yeast RNA are obtained by DPV, whose peak potentials shift negatively with increasing pH. The peak currents decrease gradually in successive scans and no corresponding reduction peaks occur, thus indicating that the oxidation process of yeast RNA is completely irreversible. The IR bands in the 1200-1800 cm-l range, attributed to the stretching and ring vibrations of nucleic acid bases, show the main spectral changes when the potential is shifted positively, which gives evidence that the oxidation process takes place in the base residues. The oxidation process of HS DNA is similar to that of yeast RNA. The results both from DPV and in situ FTIR spectroelectrochemistry confirm that the guanine and adenine residues can be oxidized at the electrode surface, which is consistent with the oxidation mechanism of nucleic acids proposed previously. (C) 2001 Elsevier Science B.V. All rights reserved.

Potential-induced transformation for surfactant aggregates on a metal surface

Surfactant adsorption on metal surfaces has been used to limit the activity of the electrode surface and to stabilize colloidal clusters and nanoparticles in solution, but the adsorption and relative potential-induced structure change of the surfactant were not known. Here, the adsorption of sodium dodecyl sulfate (SDS) on a Au(111) surface under potential control was investigated by in situ scanning tunneling microscopy (STM). The STM images showed that the morphology of SDS on Au(111) was changed from a hemi-cylindrical micellar monolayer to a compact and uniform bilayer through control of the potential. The transition between the hemimicellar monolayer and the compact bilayer is not reversed after a period of time. The model of potential-induced transformation for SDS aggregates on Au(111) was established. (C) 2001 Elsevier Science B.V. All rights reserved.

In-situ microscopic Fourier transform infrared spectroelectrochemistry of redox mechanism for electroactive species in polyelectrolyte

Studies for the development of the in-situ microscopic FTIR spectroelectrochemistry (MFTIRS) have been carried out in polyethylene glycol(PEG) polyelectrolyte, Redox reaction mechanisms of various electroactive substances involving inorganic salt, organic compound and inorganic polymeric particles have been studied.

In-situ Fourier transform infrared spectroelectrochemistry as a probe of the glassy carbon electrode chemically modified by nickel (II)-cyanometallates

A new nickel (II)-cyanometallates modified on glassy carbon electrode was prepared by a new method and studied by cyclic voltammetry and in situ Fourier transform infrared (FTIR) spectroelectrochemistry. It was found that the NiHCF film existed in two forms: Ni2Fe(II)-(CN)(6) and M2NiFe(II)(CN)(6), Fe(CN)(3)(6-) codeposited in the NiHCF film existing in free cation or bridged-bond state depended on the property of the cations in electrolyte: in NaCl and LiCl solution, it is in bridges-bonded, but in HCl and KCl, it is free.

Influence of cation concentration on 7,7,8,8-tetracyanoquinodimethane in polyelectrolyte by using in-situ microscopic Fourier transform infrared spectroelectrochemistry

The ion pair between the dianion of 7,7,8, 8-tetracyanoquinodimethane(TCNQ) and Li+ were investigated by in - situ microscopic Fourier transform infrared( FTIR) spectroelectrochemical technique. The effect of ion pair increases with increasing the concentration of cation. We observed a new band at 2130 cm(-1).

Cyclic voltammetric and in situ Fourier transform infrared spectroelectrochemical studies on the reaction of Cd2+ on the plussian blue/platinum modified electrode

Plussian blue(PB)/Pt modified electrode Tvas studied in the CdCl2 electrolyte solution by cyclic voltammetry and in situ FTIR spectroelectrochemistry. It was found that Cadmium ion was capable of substituting the high-spin iron of PB in an electrochemically induced substitution reaction and hexacyanoferrate cadmium (CdHCF) can be formed in the PB film. But PB and CdHCF in mixture film showed their own electrochemistry properties without serious effect on each other. The mechanism of substitution reaction has been given in detail.

Direct visualization of collapse process of porphyrin monolayers and porphyrin exclusion for mixed monolayers at the air-water interface

The collapse process of porphyrin monolayers at the air-water interface was studied by Brewster angle microscopy and by compression-recompression isotherms. It was found that the start of collapse observed by BAM is accordant with that measured by compression-recompression isotherms. The behavior of mixed monolayers was studied also and the results showed that porphyrin islands were excluded from mixed monolayers at 35mN/m.