Portable Fourier Transform Spectroscopy for Analysis of Surface Contamination and Quality Control

NASA Technical Reports Server (NTRS)

Pugel, Diane

2012-01-01

Progress has been made into adapting and enhancing a commercially available infrared spectrometer for the development of a handheld device for in-field measurements of the chemical composition of various samples of materials. The intent is to duplicate the functionality of a benchtop Fourier transform infrared spectrometer (FTIR) within the compactness of a handheld instrument with significantly improved spectral responsivity. Existing commercial technology, like the deuterated L-alanine triglycine sulfide detectors (DLATGS), is capable of sensitive in-field chemical analysis. This proposed approach compares several subsystem elements of the FTIR inside of the commercial, non-benchtop system to the commercial benchtop systems. These subsystem elements are the detector, the preamplifier and associated electronics of the detector, the interferometer, associated readout parameters, and cooling. This effort will examine these different detector subsystem elements to look for limitations in each. These limitations will be explored collaboratively with the commercial provider, and will be prioritized to meet the deliverable objectives. The tool design will be that of a handheld gun containing the IR filament source and associated optics. It will operate in a point-and-shoot manner, pointing the source and optics at the sample under test and capturing the reflected response of the material in the same handheld gun. Data will be captured via the gun and ported to a laptop.

Synthesis and surface activity properties of alkylphenol polyoxyethylene nonionic trimeric surfactants

NASA Astrophysics Data System (ADS)

Yang, Fang; Li, Gang; Qi, Jian; Zhang, Song-Mei; Liu, Rong

2010-10-01

A series of trimeric n-alkylphenol polyoxyethylene surfactants (TAP) were successfully synthesized and the molecular structure were confirmed by NMR, FTIR spectrum and elemental analysis. Using the same synthesis route, the trimeric nonylphenol polyoxyethylene surfactant (TNP) was synthesized using industrial product nonylphenol and paraformaldehyde, and its molecular structure was characterized by 1HNMR, FTIR spectrum and elemental analysis. The optimal reaction conditions were established. The surface activity properties of TAP and TNP (such as the critical micelle concentration (cmc), the values of surface tension at the cmc ( γcmc), the maximum surface excess concentration ( Γcmc), and the minimum surface area per surfactant molecule ( Acmc)), were determined by means of Wilhelmy plate method and steady-state fluorescence probe method, respectively. The experimental results show that the lengths of the hydrophilic group oxyethylene (EO) chains and hydrophobic group methylene chains have an influence on the cmc, γcmc, Γcmc, and Acmc of series of surfactants. Furthermore, TAP are arranged to staggered three-dimensional array mode at the air-water interface, which has exhibited better surface properties, such as low cmc values, strong adsorption affinities and wet abilities.

Elemental composition and molecular structure of Botryococcus alginite in Westphalian cannel coals from Kentucky

USGS Publications Warehouse

Mastalerz, Maria; Hower, J.C.

1996-01-01

Botryococcus-derived alginites from the Westphalian Skyline, No. 5 Block, Leatherwood (eastern Kentucky) and Breckinridge (western Kentucky) coal beds have been analyzed for elemental composition and functional group distribution using an electron microprobe and micro-FTIR, respectively. The alginites from Kentucky show a carbon range of 81.6 to 92% and oxygen content of 3.5 to 9.5%. Sulphur content ranges from 0.66 to 0.84% and Fe, Si, Al and Ca occur in minor quantities. FTIR analysis demonstrates dominant CH2, CH3 bands and subordinate aromatic carbon in all alginites. The major differences between alginites are in the ratios of CH2 and CH3 groups and ratios between aromatic bands in the out-of-plane region. These differences suggest that, although the ancient Botryococcus derives from a selective preservation of a resistant polymer, it undergoes molecular and some elemental changes through the rank equivalent to vitrinite reflectance of 0.5-0.85%. Other differences, such as intensities of ether bridges and those of carboxyl/carbonyl groups, are attributed to differences in depositional environments.

Growth and characterization of metal halide perovskite crystals: Benzyltributyl ammonium tetrachloro manganate(II) monohydrate

NASA Astrophysics Data System (ADS)

Dhandapani, M.; Sugandhi, K.; Nithya, S.; Muthuraja, P.; Balachandar, S.; Aranganayagam, K. R.

2018-05-01

The perovskite type organic-inorganic hybrid benzyltributyl ammoniumtetrachloro manganate (II) monohydrates (BTBA-Mn) are synthesized and the single crystals are grown by slow evaporation solution growth technique. The structure of the grown crystals are confirmed by using X-ray diffraction (XRD), unit cell parameter analysis, Fourier transform Infrared (FTIR), elemental analysis and 13C-NMR spectral studies. Thermogravimetry (TG), differential thermal analysis (DTA) and differential scanning colorimetric (DSC) analysis were carried out to understand thermal stability and occurrence of phase transition.

Novel selenium containing boro-phosphate glasses: preparation and structural study.

PubMed

Ciceo-Lucacel, R; Radu, T; Ponta, O; Simon, V

2014-06-01

We synthesized a new boro-phosphate glass system with different %mol SeO2 content by conventional melt quenching technique. All samples were obtained in a glassy state with the vitreous structure confirmed by X-ray diffraction analysis. Scanning electron microscopy (SEM) revealed some non-homogeneous domains on the glasses surface, and their tendency to link each other once the selenium oxide content increases. Energy-dispersive X-ray analysis (EDAX) indicated similar elemental composition in different regions of each sample. X-ray photoelectron spectroscopy (XPS) was used to determine the nature of chemical bonding and the elemental composition at the sample surfaces, and Fourier transform infrared (FT-IR) spectroscopy was used to determine the structural groups in the obtained glass structure. Based on FT-IR results, the glass structure at short range order consists mainly of small phosphate units such as pyrophosphate (i.e. P2O7(4-) dimmers or terminating groups at the end of phosphate chains) and some metaphosphate (i.e. PO3(-) middle groups in the phosphate chains) units. The boron atoms are mainly placed in three-coordinated sites in BØ3 or BØ2O(-) units. A small contribution of BØ4(-) units was also detected from the FT-IR spectra of glasses. For SeO2 content higher than 5mol%, the modifier role of selenium ions is strongly reflected on the local structure dominated in this case by pyrophosphate units. Copyright © 2014 Elsevier B.V. All rights reserved.

Surface grafting of Corchorus olitorius fibre: a green approach for the development of activated bioadsorbent.

PubMed

Roy, Aparna; Chakraborty, Sumit; Kundu, Sarada Prasad; Majumder, Subhasish Basu; Adhikari, Basudam

2013-02-15

The present work is an endeavor to prepare lignocellulosic biomass based adsorbent, suitable for removal of organic and inorganic pollutants from industrial effluents. Lignocellulosic Corchorus olitorius fibre (jute fibre) surface was grafted with naturally available polyphenol, tannin, preceded by the epoxy-activation of fibre surface with epichlorohydrin under mild condition in an aqueous suspension. The reaction parameters for the modification, viz., concentration of epichlorohydrin and tannin, time, and temperature were optimized. The successful occurrence of surface modification of jute fibre (JF) was characterized and estimated from weight gain percent, elemental analysis, Fourier transform infrared spectroscopy (FTIR), X-ray diffraction, scanning electron and atomic force microscopy, and thermogravimetric analysis. An extensive analysis of deconvoluted FTIR spectra using the Voigt model was utilized to ensure the surface grafting. The microbiological susceptibility study revealed high persistency of JF towards biodegradation after efficient grafting with tannin. Copyright © 2012 Elsevier Ltd. All rights reserved.

Structural and photoluminescence properties of Ce, Dy, Er-doped ZnO nanoparticles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jayachandraiah, C.; Kumar, K. Siva; Krishnaiah, G., E-mail: ginnerik@gmail.com

2015-06-24

Undoped ZnO and rare earth elements (Ce, Dy and Er with 2 at. %) doped nanoparticles were synthesized by wet chemical co-precipitation method at 90°C with Polyvinylpyrrolidone (PVP) as capping agent. The structural, morphological, compositional and photoluminescence studies were performed with X-ray diffraction (XRD), Transmission electron microscopy (TEM), Energy dispersive spectroscopy (EDS), FTIR spectroscopy and Photoluminescence (PL) respectively. XRD results revealed hexagonal wurtzite structure with average particle size around 18 nm - 14 nm and are compatible with TEM results. EDS confirm the incorporation of Ce, Dy and Er elements into the host ZnO matrix and is validated by FTIR analysis. PLmore » studies showed a broad intensive emission peak at 558 nm in all the samples. The intensity for Er- doped ZnO found maximum with additional Er shoulder peaks at 516nm and 538 nm. No Ce, Dy emission centers were found in spectra.« less

Molecular Chemistry and Engineering of Boron-Modified Polyorganosilazanes as New Processable and Functional SiBCN Precursors.

PubMed

Viard, Antoine; Fonblanc, Diane; Schmidt, Marion; Lale, Abhijeet; Salameh, Chrystelle; Soleilhavoup, Anne; Wynn, Mélanie; Champagne, Philippe; Cerneaux, Sophie; Babonneau, Florence; Chollon, Georges; Rossignol, Fabrice; Gervais, Christel; Bernard, Samuel

2017-07-06

A series of boron-modified polyorganosilazanes was synthesized from a poly(vinylmethyl-co-methyl)silazane and controlled amounts of borane dimethyl sulfide. The role of the chemistry behind their synthesis has been studied in detail by using solid-state NMR spectroscopy, FTIR spectroscopy, and elemental analysis. The intimate relationship between the chemistry and the processability of these polymers is discussed. Polymers with low boron contents displayed appropriate requirements for facile processing in solution, such as impregnation of host carbon materials, which resulted in the design of mesoporous monoliths with a high specific surface area after pyrolysis. Polymers with high boron content are more appropriate for solid-state processing to design mechanically robust monolith-type macroporous and dense structures after pyrolysis. Boron acts as a crosslinking element, which offers the possibility to extend the processability of polyorganosilazanes and suppress the distillation of oligomeric fragments in the low-temperature region of their thermal decomposition (i.e., pyrolysis) at 1000 °C under nitrogen. Polymers with controlled and high ceramic yields were generated. We provide a comprehensive mechanistic study of the two-step thermal decomposition based on a combination of thermogravimetric experiments coupled with elemental analysis, solid-state NMR spectroscopy, and FTIR spectroscopy. Selected characterization tools allowed the investigation of specific properties of the monolith-type SiBCN materials. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Abiotic association of PAEs with humic substances and its influence on the fate of PAEs in landfill leachate.

PubMed

Xiaoli, Chai; Rong, Ji; Jun, Wu; Huanhuan, Tong; Youcai, Zhao

2010-03-01

An equilibrium dialysis combined with a (14)C-labeling method was used to study the abiotic association of phthalic acid esters (PAEs) with dissolved humic substances (HS) and its influence on the fate of PAEs in landfill leachate. Elemental analysis and FTIR spectral analysis were carried out on the humic acid (HA) and fulvic acid (FA) components of HS to examine the relationship between the structure of HS and the intensity of the association of the PAEs with HS (K(A)). The results show that the association intensity of HS with PAEs depends greatly on both the properties of the PAEs and the source of HS. The HS have a strong association reaction with dibutyl phthalic acid, which might explain the higher concentration of dibutyl phthalic acid detected in landfill leachate. The pH value strongly affects the K(A) of HS, and it decreases radically when the pH increase from 3.0 to 9.0. The non-specific hydrophobic interaction between HS and PAEs plays a more important role in the abiotic association of HS with PAEs. Elemental analysis and FTIR spectra suggest that the high K(A) values are related to the high aromatic content and larger molecular weight of HS. Copyright (c) 2010 Elsevier Ltd. All rights reserved.

Molecules with polymerizable ligands as precursors to porous doped materials

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hubert-Pfalzgraf, L.G.; Pajot, N.; Papiernik, R.

1996-12-31

Titanium and aluminum alkoxide derivatives with polymerizable ligands such as 2-(methacryloyloxy)ethylacetoacetate (HAAEMA), oleic acid and geraniol (HOGE) have been obtained. The various compounds have been characterized by FT-IR and NMR {sup 1}H. Copolymerization with styrene and divinylbenzene affords porous doped organic materials which have been characterized by scanning electron microscopy (SEM), elemental analysis, density measurements.

Fractionation and physicochemical characterization of lignin from waste jute bags: Effect of process parameters on yield and thermal degradation.

PubMed

Ahuja, Dheeraj; Kaushik, Anupama; Chauhan, Ghanshyam S

2017-04-01

In this work lignin was extracted from waste jute bags using soda cooking method and effect of varying alkali concentration and pH on yield, purity, structure and thermal degradation of lignin were studied. The Lignin yield, chemical composition and purity were assessed using TAPPI method and UV-vis spectroscopy. Yield and purity of lignin ranged from 27 to 58% and 50-94%, respectively for all the samples and was maximum for 8% alkali concentration and at pH 2 giving higher thermal stability. Chemical structure, thermal stability and elementary analysis of lignin were studied using FTIR, H NMR, thermo gravimetric analysis (TGA) and Elemental analyzer. FTIR and H NMR results showed that core structure of lignin starts breaking beyond 10% alkali concentration. S/G ratio shows the dominance of Syringyl unit over guaiacyl unit. Copyright © 2017 Elsevier B.V. All rights reserved.

Analysis of molecular structure, spectroscopic properties (FT-IR, micro-Raman and UV-vis) and quantum chemical calculations of free and ligand 2-thiopheneglyoxylic acid in metal halides (Cd, Co, Cu, Ni and Zn).

PubMed

Gökce, Halil; Bahçeli, Semiha

2013-12-01

In this study, molecular geometries, experimental vibrational wavenumbers, electronic properties and quantum chemical calculations of 2-thiopheneglyoxylic acid molecule, (C6H4O3S), and its metal halides (Cd, Co, Cu, Ni and Zn) which are used as pharmacologic agents have been investigated experimentally by FT-IR, micro-Raman and UV-visible spectroscopies and elemental analysis. Meanwhile the vibrational calculations were verified by DFT/B3LYP method with 6-311++G(d,p) and LANL2DZ basis sets in the ground state, for free TPGA molecule and its metal halide complexes, respectively, for the first time. The calculated fundamental vibrational frequencies for the title compounds are in a good agreement with the experimental data. Copyright © 2013 Elsevier B.V. All rights reserved.

Immobilization of Chlorosulfonyl-Calix[4]arene onto the surface of silica gel through the directly estrification

NASA Astrophysics Data System (ADS)

Taghvaei-Ganjali, Saeed; Zadmard, Reza; Saber-Tehrani, Mandana

2012-06-01

For the first time Chlorosulfonyl-Calix[4]arene has been chemically bonded to silica gel through the directly estrification without silane coupling agent to prepare Chlorosulfonyl-Calix[4]arene-bonded silica gel. Sample characterization was performed by various techniques such as elemental analysis, Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDAX), powder X-ray diffraction (XRD), N2 adsorption-desorption, thermal gravimetric analysis (TGA), 29Si CP/MAS spectroscopy and acid-base titration. All data approve the successful incorporation of organic group via covalent bond. From the comparison between sulfur content determined by elemental analysis and the number of H+ determined by acid-base titration, it was shown that two ester units took place onto the new synthesized sample and two acidic sites exist on the surface.

Fourier Transform Infrared (FT-IR) and Laser Ablation Inductively Coupled Plasma-Mass Spectrometry (LA-ICP-MS) Imaging of Cerebral Ischemia: Combined Analysis of Rat Brain Thin Cuts Toward Improved Tissue Classification.

PubMed

Balbekova, Anna; Lohninger, Hans; van Tilborg, Geralda A F; Dijkhuizen, Rick M; Bonta, Maximilian; Limbeck, Andreas; Lendl, Bernhard; Al-Saad, Khalid A; Ali, Mohamed; Celikic, Minja; Ofner, Johannes

2018-02-01

Microspectroscopic techniques are widely used to complement histological studies. Due to recent developments in the field of chemical imaging, combined chemical analysis has become attractive. This technique facilitates a deepened analysis compared to single techniques or side-by-side analysis. In this study, rat brains harvested one week after induction of photothrombotic stroke were investigated. Adjacent thin cuts from rats' brains were imaged using Fourier transform infrared (FT-IR) microspectroscopy and laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). The LA-ICP-MS data were normalized using an internal standard (a thin gold layer). The acquired hyperspectral data cubes were fused and subjected to multivariate analysis. Brain regions affected by stroke as well as unaffected gray and white matter were identified and classified using a model based on either partial least squares discriminant analysis (PLS-DA) or random decision forest (RDF) algorithms. The RDF algorithm demonstrated the best results for classification. Improved classification was observed in the case of fused data in comparison to individual data sets (either FT-IR or LA-ICP-MS). Variable importance analysis demonstrated that both molecular and elemental content contribute to the improved RDF classification. Univariate spectral analysis identified biochemical properties of the assigned tissue types. Classification of multisensor hyperspectral data sets using an RDF algorithm allows access to a novel and in-depth understanding of biochemical processes and solid chemical allocation of different brain regions.

Differentiations of Chitin Content and Surface Morphologies of Chitins Extracted from Male and Female Grasshopper Species

PubMed Central

Kaya, Murat; Lelešius, Evaldas; Nagrockaitė, Radvilė; Sargin, Idris; Arslan, Gulsin; Mol, Abbas; Baran, Talat; Can, Esra; Bitim, Betul

2015-01-01

In this study, we used Fourier transform infrared spectroscopy (FT-IR), elemental analysis (EA), thermogravimetric analysis (TGA), X-ray diffractometry (XRD), and scanning electron microscopy (SEM) to investigate chitin structure isolated from both sexes of four grasshopper species. FT-IR, EA, XRD, and TGA showed that the chitin was in the alpha form. With respect to gender, two main differences were observed. First, we observed that the quantity of chitin was greater in males than in females and the dry weight of chitin between species ranged from 4.71% to 11.84%. Second, using SEM, we observed that the male chitin surface structure contained 25 – 90nm wide nanofibers and 90 – 250 nm nanopores, while no pores or nanofibers were observed in the chitin surface structure of the majority of females (nanofibers were observed only in M. desertus females). In contrast, the elemental analysis, thermal properties, and crystalline index values for chitin were similar in males and females. Also, we carried out enzymatic digestion of the isolated chitins using commercial chitinase from Streptomyces griseus. We observed that there were no big differences in digestion rate of the chitins from both sexes and commercial chitin. The digestion rates were for grasshoppers’ chitins; 88.45–95.48% and for commercial chitin; 94.95%. PMID:25635814

Synthesis of metal complexes involving Schiff base ligand with methylenedioxy moiety: spectral, thermal, XRD and antimicrobial studies.

PubMed

Sundararajan, M L; Jeyakumar, T; Anandakumaran, J; Karpanai Selvan, B

2014-10-15

Metal complexes of Zn(II), Cd(II), Ni(II), Cu(II), Fe(III), Co(II), Mn(II) Hg(II), and Ag(I) have been synthesized from Schiff base ligand, prepared by the condensation of 3,4-(methylenedioxy)aniline and 5-bromo salicylaldehyde. All the compounds have been characterized by using elemental analysis, molar conductance, FT-IR, UV-Vis, (1)H NMR, (13)C NMR, mass spectra, powder XRD and thermal analysis (TG/DTA) technique. The elemental analysis suggests the stoichiometry to be 1:1 (metal:ligand). The FT-IR, (1)H NMR, (13)C NMR and UV-Vis spectral data suggest that the ligand coordinate to the metal atom by imino nitrogen and phenolic oxygen as bidentate manner. Mass spectral data further support the molecular mass of the compounds and their structure. Powder XRD indicates the crystalline state and morphology of the ligand and its metal complexes. The thermal behaviors of the complexes prove the presence of lattice as well as coordinated water molecules in the complexes. Melting point supports the thermal stability of all the compounds. The in vitro antimicrobial effects of the synthesized compounds were tested against five bacterial and three fungal species by well diffusion method. Antioxidant activities have also been performed for all the compounds. Metal complexes show more biological activity than the Schiff base. Copyright © 2014 Elsevier B.V. All rights reserved.

Data on Molluscan Shells in parts of Nellore Coast, southeast coast of India.

PubMed

Lakshmanna, B; Jayaraju, N; Prasad, T Lakshmi; Sreenivasulu, G; Nagalakshmi, K; Kumar, M Pramod; Madakka, M

2018-02-01

X-ray diffraction (XRD), Scanning Electron Microscope-Energy Dispersive Spectroscopy (SEM-EDS), and Fourier Transform Infrared Spectroscopy (FT-IR), were applied to analyze the organic matrix of two Molluscan shells . The Mollusca shells are mineral structure and calcium carbonate crystallized as aragonite. The FT-IR spectra showed Alkyl Halide, Alkanes, Alcohols, Amides, Aromatic, and Hydroxyl groups in the organic matrix of the whole (organic and mineral) Molluscan shells. SEM images of particles of the two Molluscan shells at different magnifications were taken. The morphologies of the samples show a flake like structures with irregular grains, their sizes are at micrometric scale and the chemical analysis of EDS indicated that the major elements of Cardita and Gastropoda were C, O, and Ca, consistent with the results of XRD analysis. The results of the analysis of the EDS spectra of the shells showed that the content of most of the powder composition of shells is the element carbon, calcium oxygen, aluminium, and lead peaks that appear on the Cardita and Gastropoda and shells powders tap EDS spectra. The present work examined organic matrix of the selected shells of the heavily polluted and light polluted sites, along Nellore Coast, South East Coast of India. The heavily polluted sites have significantly thickened shells. The data demonstrated the sensitivity of this abundant and widely distributed intertidal fragile environment.

Torrefaction of landfill food waste for possible application in biomass co-firing.

PubMed

Pahla, G; Ntuli, F; Muzenda, E

2018-01-01

Greenhouse gas emissions and municipal solid waste management have presented challenges globally. This study aims to produce a high-quality biochar with properties close to bituminous coal from landfill food waste (FW). FW was analyzed by proximate and ultimate analyses to determine its fuel properties and elemental composition before torrefaction. Temperature was varied from 200 to 300 °C at a constant residence time of 40 min and 10 °C/min heating rate. Calorific value, mass yield, energy yield and energy density were computed and used to determine the quality of the resulting biochar. Quality of raw food waste was also determined by elemental analysis. Thermal evolution was then investigated using hyphenated Thermogravimetric Analysis (TGA) and Fourier Transform Infra-Red Spectrometry (FTIR). Torrefaction was done at 225 °C, 275 °C and 300 °C. The calorific value was upgraded from 19.76 MJ/kg for dried raw food waste to 26.15 MJ/kg for torrefied food waste at the appropriate conditions which were 275 °C, 40 min and 10 °C/min. The higher heating value was comparable to that of bituminous coal from Anglo Mafube in South Africa. Elemental analysis of biochar showed an increase in carbon content with temperature due to loss of oxygen containing volatiles. This agreed with TG curves and FTIR spectra which confirmed release of H 2 O, CO and CO 2 . This resulted in a more hydrophobic solid fuel with high energy density. Food waste can therefore be upgraded to a biochar with similar fuel properties as pulverized coal used in coal fired boilers. Copyright © 2017 Elsevier Ltd. All rights reserved.

Analysis of heterogeneous gallstones using laser-induced breakdown spectroscopy (LIBS) and wavelength dispersive X-ray fluorescence (WD-XRF).

PubMed

Jaswal, Brij Bir S; Kumar, Vinay; Sharma, Jitendra; Rai, Pradeep K; Gondal, Mohammed A; Gondal, Bilal; Singh, Vivek K

2016-04-01

Laser-induced breakdown spectroscopy (LIBS) is an emerging analytical technique with numerous advantages such as rapidity, multi-elemental analysis, no specific sample preparation requirements, non-destructiveness, and versatility. It has been proven to be a robust elemental analysis tool attracting interest because of being applied to a wide range of materials including biomaterials. In this paper, we have performed spectroscopic studies on gallstones which are heterogeneous in nature using LIBS and wavelength dispersive X-ray fluorescence (WD-XRF) techniques. It has been observed that the presence and relative concentrations of trace elements in different kind of gallstones (cholesterol and pigment gallstones) can easily be determined using LIBS technique. From the experiments carried out on gallstones for trace elemental mapping and detection, it was found that LIBS is a robust tool for such biomedical applications. The stone samples studied in the present paper were classified using the Fourier transform infrared (FTIR) spectroscopy. WD-XRF spectroscopy has been applied for the qualitative and quantitative analysis of major and trace elements present in the gallstone which was compared with the LIBS data. The results obtained in the present paper show interesting prospects for LIBS and WD-XRF to study cholelithiasis better.

Vibrational spectra, powder X-ray diffractions and physical properties of cyanide complexes with 1-ethylimidazole

NASA Astrophysics Data System (ADS)

Kürkçüoğlu, Güneş Süheyla; Kiraz, Fulya Çetinkaya; Sayın, Elvan

2015-10-01

The heteronuclear tetracyanonickelate(II) complexes of the type [M(etim)Ni(CN)4]n (hereafter, abbreviated as M-Ni-etim, M = Mn(II), Fe(II) or Co(II); etim = 1-ethylimidazole, C5H8N2) were prepared in powder form and characterized by FT-IR and Raman spectroscopy, powder X-ray diffraction (PXRD), thermal (TG; DTG and DTA), and elemental analysis techniques. The structures of these complexes were elucidated using vibrational spectra and powder X-ray diffraction patterns with the peak assignment to provide a better understanding of the structures. It is shown that the spectra are consistent with a proposed crystal structure for these compounds derived from powder X-ray diffraction measurements. Vibrational spectra of the complexes were presented and discussed with respect to the internal modes of both the etim and the cyanide ligands. The C, H and N analyses were carried out for all the complexes. Thermal behaviors of these complexes were followed using TG, DTG and DTA curves in the temperature range 30-700 °C in the static air atmosphere. The FT-IR, Raman spectra, thermal and powder X-ray analyses revealed no significant differences between the single crystal and powder forms. Additionally, electrical and magnetic properties of the complexes were investigated. The FT-IR and Raman spectroscopy, PXRD, thermal and elemental analyses results propose that these complexes are similar in structure to the Hofmann-type complexes.

Synthesis, X-ray crystallography characterization, vibrational spectroscopic, molecular electrostatic potential maps, thermodynamic properties studies of N,N'-di(p-thiazole)formamidine.

PubMed

Rofouei, M K; Fereyduni, E; Sohrabi, N; Shamsipur, M; Attar Gharamaleki, J; Sundaraganesan, N

2011-01-01

In this work, we will report a combined experimental and theoretical study on molecular and vibrational structure of N,N'-di(p-thiazole)formamidine (DpTF). DpTF has been synthesized and characterized by elemental analysis, FT-IR, FT-Raman, 1H NMR, 13C NMR spectroscopy and X-ray single crystal diffraction. The FT-IR and FT-Raman spectra of DpTF were recorded in the solid phase. The optimized geometry was calculated by HF and B3LYP methods using 6-31G(d) basis set. The FT-IR and FT-Raman spectra of DpTF was calculated at the HF/B3LYP/6-31G(d) level and were interpreted in terms of potential energy distribution (PED) analysis. The scaled theoretical wavenumber showed very good agreement with the experimental values. A detailed interpretation of the infrared and Raman spectra of DpTF was reported. On the basis of vibrational analyses, the thermodynamic properties of the title compound at different temperatures have been calculated, revealing the correlations between Cp,m°, Sm°, Hm° and temperatures. Furthermore, molecular electrostatic potential maps (MESP) and total dipole moment properties of the compound have been calculated. Copyright © 2010 Elsevier B.V. All rights reserved.

Synthesis and characterization of an octaimidazolium-based polyhedral oligomeric silsesquioxanes ionic liquid by an ion-exchange reaction.

PubMed

Tan, Jinglin; Ma, Depeng; Sun, Xingrong; Feng, Shengyu; Zhang, Changqiao

2013-04-07

Preparation of POSS-min-DS, an octaimidazolium-based polyhedral oligomeric silsesquioxanes (POSS) room temperature ionic liquid, by an ion-exchange reaction between POSS and sodium dodecyl sulfate was reported. Octaimidazolium-based POSS was synthesized with more than 98% yield within 3 h. POSS-min-DS and octaimidazolium-based POSS were confirmed by (1)H, (13)C, and (29)Si NMR, FT-IR and elemental analysis.

Acetone sensor based on zinc oxide hexagonal tubes

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hastir, Anita, E-mail: anitahastir@gmail.com; Singh, Onkar, E-mail: anitahastir@gmail.com; Anand, Kanika, E-mail: anitahastir@gmail.com

2014-04-24

In this work hexagonal tubes of zinc oxide have been synthesized by co-precipitation method. For structural, morphological, elemental and optical analysis synthesized powders were characterized by using x-ray diffraction, field emission scanning microscope, EDX, UV-visible and FTIR techniques. For acetone sensing thick films of zinc oxide have been deposited on alumina substrate. The fabricated sensors exhibited maximum sensing response towards acetone vapour at an optimum operating temperature of 400°C.

Hydrothermal synthesis and characterization of a novel supramolecular network compound of Co(NIA) 2(H 2O) 4 with molecular ladder hydrogen bond chains (NIA=nicotinate)

NASA Astrophysics Data System (ADS)

Jia, Hong-Bin; Yu, Jie-Hui; Xu, Ji-Qing; Ye, Ling; Ding, Hong; Jing, Wei-Jie; Wang, Tie-Gang; Xu, Jia-Ning; Li, Zeng-Chun

2002-10-01

By hydrothermal method, a novel supramolecular compound, Co(NIA) 2(H 2O) 4 was synthesized and its structure was characterized with elemental analysis, FT-IR spectrum, TGA and X-ray diffractometer, indicating that it is a novel polyporous supramolecule with molecular ladder hydrogen-bonded chains. TGA curve shows its thermal stability up to 520 °C.

Attenuated total reflectance FT-IR imaging and quantitative energy dispersive-electron probe X-ray microanalysis techniques for single particle analysis of atmospheric aerosol particles.

PubMed

Ryu, JiYeon; Ro, Chul-Un

2009-08-15

This work demonstrates the practical applicability of the combined use of attenuated total reflectance (ATR) FT-IR imaging and low-Z particle electron probe X-ray microanalysis (EPMA) techniques for the characterization of individual aerosol particles. These two single particle analytical techniques provide complementary information on the physicochemical characteristics of the same individual particles, that is, the low-Z particle EPMA for the information on the morphology and elemental concentration and the ATR-FT-IR imaging on the functional group, molecular species, and crystal structure. It was confirmed that the ATR-FT-IR imaging technique can provide sufficient FT-IR absorption signals to perform molecular speciation of individual particles of micrometer size when applied to artificially generated aerosol particles such as ascorbic acid and NaNO(3) aerosols. An exemplar indoor atmospheric aerosol sample was investigated to demonstrate the practical feasibility of the combined application of ATR-FT-IR imaging and low-Z particle EPMA techniques for the characterization of individual airborne particles.

Comparison study on biosynthesis of silver nanoparticles using fresh and hot air oven dried IMPERATA CYLINDRICA leaf

NASA Astrophysics Data System (ADS)

Najmi Bonnia, Noor; Fairuzi, Afiza Ahmad; Akhir, Rabiatuladawiyah Md.; Yahya, Sabrina M.; Rani, Mohd Azri Ab; Ratim, Suzana; Rahman, Norafifah A.; Akil, Hazizan Md

2018-01-01

The perennial rhizomatous grass; Imperata cylindrica (I. cylindrica) has been reported rich in various phytochemicals. In present study, silver nanoparticles were synthesized from aqueous leaf extract of I. cylindrica at two different leaf conditions; fresh leaves and hot-air oven dried leaves. Biosynthesized silver nanoparticles were characterized by UV-visible spectroscopy, field emission scanning electron microscopy (FESEM) and Fourier transform infrared spectroscopy (FTIR). Maximum absorption was recorded between 400 nm to 500 nm. FESEM analysis revealed that the silver nanoparticles predominantly form spherical shapes. The particles sizes were ranging from 22-37 nm. The elemental composition of the synthesized silver nanoparticles was confirmed by using energy dispersive X-ray spectroscopy (EDX) analysis. Fourier transform infrared spectroscopy (FTIR) confirmed the reducing and stabilizing actions came from biomolecules associated with I. cylindrica leaf extract. Thus in this investigation, an environmentally safe method to synthesized silver nanoparticles using local plant extract was successfully established.

Characterization and thermogravimetric analysis of lanthanide hexafluoroacetylacetone chelates

DOE PAGES

Shahbazi, Shayan; Stratz, S. Adam; Auxier, John D.; ...

2016-08-30

This work reports the thermodynamic characterizations of organometallic species as a vehicle for the rapid separation of volatile nuclear fission products via gas chromatography due to differences in adsorption enthalpy. Because adsorption and sublimation thermodynamics are linearly correlated, there is considerable motivation to determine sublimation enthalpies. A method of isothermal thermogravimetric analysis, TGA-MS and melting point analysis are employed on thirteen lanthanide 1,1,1,5,5,5-hexafluoroacetylacetone complexes to determine sublimation enthalpies. An empirical correlation is used to estimate adsorption enthalpies of lanthanide complexes on a quartz column from the sublimation data. Additionally, four chelates are characterized by SC-XRD, elemental analysis, FTIR and NMR.

Progression in structural, magnetic and electrical properties of La-doped group IV elements

NASA Astrophysics Data System (ADS)

Deepapriya, S.; Annie Vinosha, P.; Rodney, John D.; Jerome Das, S.

2018-04-01

Progression of group IV elements such as zinc ferrite (ZnFe2O4), cobalt ferrite (CoFe2O4) was synthesized by doping lanthanum (La), via adopting a facile co-precipitation method. Doping hefty rare earth ion in spinel structure can amend to the physical properties of the lattice, which can be used in the enhancement of magnetic and electrical properties of the as-synthesized nanomaterial, it is vital to metamorphose and optimize its micro structural and magnetic features. The structural properties of the samples was analysed by powder X-ray diffraction (XRD), Fourier transform infrared (FTIR), Transmission electron microscopy (TEM) and UV-visible spectral analysis (UV-vis) reveals the optical property and optical band gap. The magnetic properties were evaluated using a vibrating sample magnetometer (VSM), the presence of functional group was confirmed by FTIR. XRD analyses elucidates that the synthesized samples zinc and cobalt had a spinel structure. From TEM analyses the morphology and diameter of the particle was observed. The substituted rare earth ions in Zinc ferrite inhibit the grain growth of the materials in an efficient manner compared with that of the Cobalt ferrite.

Characterization of plastic blends made from mixed plastics waste of different sources.

PubMed

Turku, Irina; Kärki, Timo; Rinne, Kimmo; Puurtinen, Ari

2017-02-01

This paper studies the recyclability of construction and household plastic waste collected from local landfills. Samples were processed from mixed plastic waste by injection moulding. In addition, blends of pure plastics, polypropylene and polyethylene were processed as a reference set. Reference samples with known plastic ratio were used as the calibration set for quantitative analysis of plastic fractions in recycled blends. The samples were tested for the tensile properties; scanning electron microscope-energy-dispersive X-ray spectroscopy was used for elemental analysis of the blend surfaces and Fourier transform infrared (FTIR) analysis was used for the quantification of plastics contents.

Exploring Biogeochemistry and Microbial Diversity of Extant Microbialites in Mexico and Cuba

PubMed Central

Valdespino-Castillo, Patricia M.; Hu, Ping; Merino-Ibarra, Martín; López-Gómez, Luz M.; Cerqueda-García, Daniel; González-De Zayas, Roberto; Pi-Puig, Teresa; Lestayo, Julio A.; Holman, Hoi-Ying; Falcón, Luisa I.

2018-01-01

Microbialites are modern analogs of ancient microbial consortia that date as far back as the Archaean Eon. Microbialites have contributed to the geochemical history of our planet through their diverse metabolic capacities that mediate mineral precipitation. These mineral-forming microbial assemblages accumulate major ions, trace elements and biomass from their ambient aquatic environments; their role in the resulting chemical structure of these lithifications needs clarification. We studied the biogeochemistry and microbial structure of microbialites collected from diverse locations in Mexico and in a previously undescribed microbialite in Cuba. We examined their structure, chemistry and mineralogy at different scales using an array of nested methods including 16S rRNA gene high-throughput sequencing, elemental analysis, X-Ray fluorescence (XRF), X-Ray diffraction (XRD), Scanning Electron Microscopy-Energy Dispersive Spectroscopy (SEM-EDS), Fourier Transformed Infrared (FTIR) spectroscopy and Synchrotron Radiation-based Fourier Transformed Infrared (SR-FTIR) spectromicroscopy. The resulting data revealed high biological and chemical diversity among microbialites and specific microbe to chemical correlations. Regardless of the sampling site, Proteobacteria had the most significant correlations with biogeochemical parameters such as organic carbon (Corg), nitrogen and Corg:Ca ratio. Biogeochemically relevant bacterial groups (dominant phototrophs and heterotrophs) showed significant correlations with major ion composition, mineral type and transition element content, such as cadmium, cobalt, chromium, copper and nickel. Microbial-chemical relationships were discussed in reference to microbialite formation, microbial metabolic capacities and the role of transition elements as enzyme cofactors. This paper provides an analytical baseline to drive our understanding of the links between microbial diversity with the chemistry of their lithified precipitations. PMID:29666607

Exploring Biogeochemistry and Microbial Diversity of Extant Microbialites in Mexico and Cuba.

PubMed

Valdespino-Castillo, Patricia M; Hu, Ping; Merino-Ibarra, Martín; López-Gómez, Luz M; Cerqueda-García, Daniel; González-De Zayas, Roberto; Pi-Puig, Teresa; Lestayo, Julio A; Holman, Hoi-Ying; Falcón, Luisa I

2018-01-01

Microbialites are modern analogs of ancient microbial consortia that date as far back as the Archaean Eon. Microbialites have contributed to the geochemical history of our planet through their diverse metabolic capacities that mediate mineral precipitation. These mineral-forming microbial assemblages accumulate major ions, trace elements and biomass from their ambient aquatic environments; their role in the resulting chemical structure of these lithifications needs clarification. We studied the biogeochemistry and microbial structure of microbialites collected from diverse locations in Mexico and in a previously undescribed microbialite in Cuba. We examined their structure, chemistry and mineralogy at different scales using an array of nested methods including 16S rRNA gene high-throughput sequencing, elemental analysis, X-Ray fluorescence (XRF), X-Ray diffraction (XRD), Scanning Electron Microscopy-Energy Dispersive Spectroscopy (SEM-EDS), Fourier Transformed Infrared (FTIR) spectroscopy and Synchrotron Radiation-based Fourier Transformed Infrared (SR-FTIR) spectromicroscopy. The resulting data revealed high biological and chemical diversity among microbialites and specific microbe to chemical correlations. Regardless of the sampling site, Proteobacteria had the most significant correlations with biogeochemical parameters such as organic carbon (C org ), nitrogen and C org :Ca ratio. Biogeochemically relevant bacterial groups (dominant phototrophs and heterotrophs) showed significant correlations with major ion composition, mineral type and transition element content, such as cadmium, cobalt, chromium, copper and nickel. Microbial-chemical relationships were discussed in reference to microbialite formation, microbial metabolic capacities and the role of transition elements as enzyme cofactors. This paper provides an analytical baseline to drive our understanding of the links between microbial diversity with the chemistry of their lithified precipitations.

Novel dextran derivatives with unconventional structure formed in an efficient one-pot reaction.

PubMed

Hotzel, Konrad; Heinze, Thomas

2016-11-03

An efficient one-pot synthesis of new dextran derivatives is described. The functional groups of β-alanine, i.e., the carboxyl- and amine group, are converted independently in one-step by iminium chloride to form products with a single substituent. The dextran N-[(dimethylamino)methylene]-β-alanine ester is formed selectively. The structure of the resulting polymers is unambiguously determined by means of NMR- and FTIR-spectroscopy and elemental analysis. Copyright © 2016 Elsevier Ltd. All rights reserved.

One-pot and two-step synthesis of novel carbonylthioureas and dicarbonyldithioureas derivatives

NASA Astrophysics Data System (ADS)

Banaei, Alireza; Shiran, Jafar Abbasi; Saadat, Afshin; Ardabili, Farnaz Fazlalizadeh; McArdle, Patrick

2015-11-01

One-pot, two-step synthesis of several 1-cyclopropanecarbonyl-3-(substituted phenyl)-thioureas and 1-(phenylene-1,4-dione)-3,3‧-(substituted phenyl)-dithioureas have been successfully prepared. The structures of the synthesized compounds were confirmed by elemental analysis, FT-IR spectroscopy and NMR. Also the crystal structure one of these compounds was determined by X-ray crystallography. All synthesized compounds were evaluated for antibacterial activity using Salmonella enterica (SE), Micrococcus luteus (ML), Bacillus subtilis (BS) and Pseudomonas aeruginosa (PS).

Characterization of Three Carbon- and Nitrogen-Rich Particles from Comet 81P/WILD

NASA Technical Reports Server (NTRS)

Gallien, J.-P.; Khodja, H.; Herzog, G. F.; Taylor, S.; Koepsell, E.; Daghlian, C. P.; Flynn, G. J.; Sitnitsky, I.; Lanzirotti, A.; Sutton, S. R.;

Experimental and theoretical studies on the structure and spectroscopic properties of (E)-1-(2-aminophenyl)-3-(pyridine-4-yl) prop-2-en-1-one

NASA Astrophysics Data System (ADS)

Cruz Ortiz, Andrés Felipe; Sánchez López, Alberto; García Ríos, Alejandro; Cuenú Cabezas, Fernando; Rozo Correa, Ciro Eduardo

2015-10-01

(E)-1-(2-aminophenyl)-3-(pyridine-4-yl)prop-2-en-1-one (or simply 2-aminochalcone) was synthetized and characterized by elemental analysis, FT-IR, NMR, MS and XRD. Molecular geometry optimization, vibrational harmonic frequencies, 1H and 13C NMR chemical shifts were calculated by ab initio (HF and MP2) and density functional theory (DFT) methods, with B3LYP and B3PW91 functionals, using GAUSSIAN 09 program package without any constraint on the geometry. With VEDA software vibrational frequencies were assigned in terms of the potential energy distribution. A detailed interpretation of the FT-IR, NMR and XRD, experimental and calculated, is reported. The HOMO and LUMO energy gap that reflects the chemical activity of the molecule were also studied by DFT and above basis set. All theoretical results correspond to a great extent to experimental ones.

Rapid degradation of phenol by ultrasound-dispersed nano-metallic particles (NMPs) in the presence of hydrogen peroxide: A possible mechanism for phenol degradation in water.

PubMed

Singh, Jiwan; Yang, Jae-Kyu; Chang, Yoon-Young

2016-06-15

The present study was carried out to investigate the degradation of phenol by ultrasonically dispersed nano-metallic particles (NMPs) in an aqueous solution of phenol. Leaching liquor from automobile shredder residue (ASR) was used to obtain the NMPs. The prepared NMPs were analyzed by scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FTIR), and by X-ray diffraction (XRD). The SEM images show that the diameters of the NMPs were less than 50 nm. An SEM-EDX elemental analysis reveals that Fe was the most commonly found element (weight %) in the NMPs. The FTIR and XRD peaks indicate the presence of metals oxides on the surfaces of the NMPs. The results of the XPS analysis indicate that various elements (e.g., C, O, Zn, Cu, Mn, Fe) are present on the surfaces of the NMPs. The effects of the NMP dose, the initial solution pH, and of different concentrations of phenol and H2O2 on the phenol degradation characteristics were evaluated. The results of this study demonstrate that phenol degradation can be improved by increasing the amount of NMPs, whereas it is reduced with an increase in the phenol concentration. The degradation of phenol by ultrasonically dispersed NMPs followed the pseudo-first-order kinetics. The probable mechanism of phenol degradation by ultrasonically dispersed NMPs was the oxidation of phenol caused by the hydroxyl radicals produced during the reaction between H2O2 and the NMPs during the ultrasonication process. Copyright © 2016 Elsevier Ltd. All rights reserved.

Extraction and Physicochemical Characterization of a New Polysaccharide Obtained from the Fresh Fruits of Abelmoschus Esculentus

PubMed Central

Emeje, Martins; Isimi, Christiana; Byrn, Stephen; Fortunak, Joseph; Kunle, Olobayo; Ofoefule, Sabinus

2011-01-01

This paper is the first multi-scale characterization of the fluidize-dried gum extracted from the fresh fruits of the plant Abelmoschus esculentus. It describes the physical, thermal, sorptional and functional properties of this natural gum. Elemental analysis, scanning electron microscopy (SEM), particle size analysis, X-ray powder diffraction (XPRD), thermo-gravimetric analysis (TGA), differential scanning calorimetry (DSC), fourier transmittance infra red (FT-IR), and nuclear magnetic resonance (NMR) spectroscopy were used to characterize the gum sample. Abelmoschus Esculentus Gum (AEG) had a glass transition temperature (Tg) of 70°C and no melting peak. It showed a 14.91% loss in weight at 195°C. X-ray diffractogram showed numerous broad halos for AEG. Elemental analysis showed that AEG contains 39.5, 7.3, 51.8, and 1.4% carbon, hydrogen, oxygen and nitrogen respectively. The results obtained in this study established the fundamental characteristics of AEG and suggests its potential application in the food, cosmetic and pharmaceutical sectors. PMID:24250349

Single-particle investigation of summertime and wintertime Antarctic sea spray aerosols using low-Z particle EPMA, Raman microspectrometry, and ATR-FTIR imaging techniques

NASA Astrophysics Data System (ADS)

Eom, Hyo-Jin; Gupta, Dhrubajyoti; Cho, Hye-Rin; Hwang, Hee Jin; Do Hur, Soon; Gim, Yeontae; Ro, Chul-Un

2016-11-01

Two aerosol samples collected at King Sejong Korean scientific research station, Antarctica, on 9 December 2011 in the austral summer (sample S1) and 23 July 2012 in the austral winter (sample S2), when the oceanic chlorophyll a levels on the collection days of the samples were quite different, by ˜ 19 times (2.46 vs. 0.13 µg L-1, respectively), were investigated on a single-particle basis using quantitative energy-dispersive electron probe X-ray microanalysis (ED-EPMA), called low-Z particle EPMA, Raman microspectrometry (RMS), and attenuated total reflection Fourier transform infrared (ATR-FTIR) imaging techniques to obtain their characteristics based on the elemental chemical compositions, molecular species, and mixing state. X-ray analysis showed that the supermicron summertime and wintertime Antarctic aerosol samples have different elemental chemical compositions, even though all the individual particles analyzed were sea spray aerosols (SSAs); i.e., the contents of C, O, Ca, S, and Si were more elevated, whereas Cl was more depleted, for sample S1 than for sample S2. Based on qualitative analysis of the chemical species present in individual SSAs by the combined application of RMS and ATR-FTIR imaging, different organic species were observed in samples S1 and S2; i.e., Mg hydrate salts of alanine were predominant in samples S1 and S2, whereas Mg salts of fatty acids internally mixed with Mg hydrate salts of alanine were significant in sample S2. Although CaSO4 was observed significantly in both samples S1 and S2, other inorganic species, such as Na2SO4, NaNO3, Mg(NO3)2, SiO2, and CH3SO3Mg, were observed more significantly in sample S1, suggesting that those compounds may be related to the higher phytoplankton activity in summer.

Lanthanide Oleates: Chelation, Self-assembly, and Exemplification of Ordered Nanostructured Colloidal Contrast Agents for Medical Imaging

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, Guozhen; Conn, Charlotte E.; Drummond, Calum J.

2010-01-12

Eight lanthanide(III) oleates have been prepared and characterized. The chelation and self-assembly structures of these rare-earth oleates have been studied by elemental analysis, Fourier transfer infrared spectroscopy (FTIR), and X-ray powder diffraction (XRD) analysis. Elemental analysis and FTIR results indicate that three oleate anions are complexed with one lanthanide cation and, with the exception of anhydrous cerium(III) oleate, form either a mono- or a hemihydrate. The X-ray analysis showed that the neat lanthanide soaps have a lamellar bilayer structure at room temperature. The thermal behavior has been investigated by cross-polarized optical microscopy (POM), differential scanning calorimetry (DSC), and thermogravimetric analysismore » (TGA). POM scans showed that all the lanthanide oleates form a lamellar phase in the presence of excess water. Small-angle X-ray scattering (SAXS) and XRD were used to investigate the internal structure of the bulk lanthanide oleates in excess water, and these X-ray results confirmed that the lanthanide oleates do not swell in water. Select lanthanide oleates were dispersed in water to form nonswelling lamellar submicrometer particles, confirmed by dynamic light scattering (DLS) and synchrotron SAXS measurements. NMR results indicated that colloidal dispersions of lanthanide oleates containing paramagnetic ions, such as gadolinium(III), terbium(III), and dysprosium(III), have a significant effect on the longitudinal (T{sub 1}) and transverse (T{sub 2}) relaxation times of protons in water. Time-resolved fluorescence measurements have demonstrated that colloidal dispersions of europium(III) oleate exhibit strong luminescence. The rare earth metal soaps exemplify the potential of self-assembled chelating amphiphiles as contrast agents in medical imaging modalities such as magnetic resonance imaging (MRI) and fluorescence imaging.« less

Effect of Heat Treatment Temperature on Chemical Compositions of Extracted Hydroxyapatite from Bovine Bone Ash

NASA Astrophysics Data System (ADS)

Younesi, M.; Javadpour, S.; Bahrololoom, M. E.

2011-11-01

This article presents the effect of heat treating temperature on chemical composition of hydroxyapatite (HA) that was produced by burning bovine bone, and then heat treating the obtained bone ash at different temperatures in range of 600-1100 °C in air. Bone ash and the resulting white powder from heat treating were characterized by Fourier transformed infrared spectroscopy (FT-IR) and x-ray diffractometry (XRD). The FT-IR spectra confirmed that heat treating of bone ash at temperature of 800 °C removed the total of organic substances. x-ray diffraction analysis showed that the white powder was HA and HA was the only crystalline phase indicated in heat treating product. x-ray fluorescence analyses revealed that calcium and phosphorous were the main elements and magnesium and sodium were minor impurities of produced powder at 800 °C. The results of the energy dispersive x-ray analysis showed that Ca/P ratio in produced HA varies in range of 1.46-2.01. The resulting material was found to be thermally stable up to 1100 °C.

Fabrication of novel metal ion imprinted xanthan gum-layered double hydroxide nanocomposite for adsorption of rare earth elements.

PubMed

Iftekhar, Sidra; Srivastava, Varsha; Hammouda, Samia Ben; Sillanpää, Mika

2018-08-15

The work focus to enhance the properties of xanthan gum (XG) by anchoring metal ions (Fe, Zr) and encapsulating inorganic matrix (M@XG-ZA). The fabricated nanocomposite was characterized by Transmission Electron Microscopy (TEM), Scanning Electron Microscopy (SEM), Energy-dispersive X-ray spectroscopy (EDX), Fourier Transform Infrared Spectroscopy (FTIR), surface area (BET) and zeta potential analysis. The adsorption of Sc, Nd, Tm and Yb was investigated after screening of synthesized materials in detail to understand the influence of pH, contact time, temperature and initial REE (rare earth element) concentration both in single and multicomponent system via batch adsorption. The adsorption mechanism was verified by FTIR, SEM and elemental mapping. The SEM images of Zr@XG-ZA demonstrate scutes structure, which disappeared after adsorption of REEs. The maximum adsorption capacities were 132.30, 14.01, 18.15 and 25.73 mg/g for Sc, Nd, Tm and Yb, respectively. The adsorption efficiency over Zr@XG-ZA in multicomponent system was higher than single system and the REEs followed the order: Sc > Yb > Tm > Nd. The Zr@XG-ZA demonstrate good adsorption behavior for REEs up to five cycles and then it can be used as photocatalyst for the degradation of tetracycline. Thus, the work adds a new insight to design and preparation of efficient bifunctional adsorbents from sustainable materials for water purification. Copyright © 2018 Elsevier Ltd. All rights reserved.

Synthesis, characterizations and anti-bacterial activities of pure and Ag doped CdO nanoparticles by chemical precipitation method

NASA Astrophysics Data System (ADS)

Sivakumar, S.; Venkatesan, A.; Soundhirarajan, P.; Khatiwada, Chandra Prasad

2015-02-01

In the present study, synthesized pure and Ag (1%, 2%, and 3%) doped Cadmium Oxide (CdO) nanoparticles by chemical precipitation method. Then, the synthesized products were characterized by thermo gravimetric-differential thermal analysis (TG-DTA), X-ray diffraction (XRD) analysis, Fourier transform infrared (FT-IR) spectroscopy, Ultra violet-Vis diffused reflectance spectroscopy (UV-Vis-DRS), Scanning electron microscopy (SEM), Energy dispersive X-rays (EDX) spectroscopy, and anti-bacterial activities, respectively. The transition temperatures and phase transitions of Cd(OH)2 to CdO at 400 °C was confirmed by TG-DTA analysis. The XRD patterns show the cubic shape and average particle sizes are 21, 40, 34, and 37 nm, respectively for pure and Ag doped samples. FT-IR study confirmed the presence of CdO and Ag at 677 and 459 cm-1, respectively. UV-Vis-DRS study shows the variation on direct and indirect band gaps. The surface morphologies and elemental analysis have been confirmed from SEM and with EDX. In addition, the synthesized products have been characterized by antibacterial activities against Gram-positive and negative bacteria. Further, the present investigation suggests that CdO nanoparticles have the great potential applications on various industrial and medical fields of research.

Characterization of Natural Dyes and Traditional Korean Silk Fabric by Surface Analytical Techniques.

PubMed

Lee, Jihye; Kang, Min Hwa; Lee, Kang-Bong; Lee, Yeonhee

2013-05-15

Time-of-flight secondary ion mass spectrometry (TOF-SIMS) and X-ray photoelectron spectroscopy (XPS) are well established surface techniques that provide both elemental and organic information from several monolayers of a sample surface, while also allowing depth profiling or image mapping to be carried out. The static TOF-SIMS with improved performances has expanded the application of TOF-SIMS to the study of a variety of organic, polymeric and biological materials. In this work, TOF-SIMS, XPS and Fourier Transform Infrared (FTIR) measurements were used to characterize commercial natural dyes and traditional silk fabric dyed with plant extracts dyes avoiding the time-consuming and destructive extraction procedures necessary for the spectrophotometric and chromatographic methods previously used. Silk textiles dyed with plant extracts were then analyzed for chemical and functional group identification of their dye components and mordants. TOF-SIMS spectra for the dyed silk fabric showed element ions from metallic mordants, specific fragment ions and molecular ions from plant-extracted dyes. The results of TOF-SIMS, XPS and FTIR are very useful as a reference database for comparison with data about traditional Korean silk fabric and to provide an understanding of traditional dyeing materials. Therefore, this study shows that surface techniques are useful for micro-destructive analysis of plant-extracted dyes and Korean dyed silk fabric.

Bacterial cellulose may provide the microbial-life biosignature in the rock records

NASA Astrophysics Data System (ADS)

Zaets, I.; Podolich, O.; Kukharenko, O.; Reshetnyak, G.; Shpylova, S.; Sosnin, M.; Khirunenko, L.; Kozyrovska, N.; de Vera, J.-P.

2014-03-01

Bacterial cellulose (BC) is a matrix for a biofilm formation, which is critical for survival and persistence of microbes in harsh environments. BC could play a significant role in the formation of microbial mats in pristine ecosystems on Earth. The prime objective of this study was to measure to what extent spectral and other characteristics of BC were changed under the performance of BC interaction with the earthly rock - anorthosite - via microorganisms. The spectral analyses (Fourier Transform Infrared FT-IR, spectroscopy, and atomic absorption spectroscopy) showed unprecedented accumulation of chemical elements in the BC-based biofilm. The absorption capacity of IR by BC was shielded a little by mineral crust formed by microorganisms on the BC-based biofilm surface, especially clearly seen in the range of 1200-900 cm-1 in FT-IR spectra. Confocal scanning laser microscopy analysis revealed that elements bioleached from anorthosite created surface coats on the BC nanofibril web. At the same time, the vibrational spectra bands showed the presence of the characteristic region of anomeric carbons (960-730 cm-1), wherein a band at 897 cm-1 confirmed the presence of β-1, 4-linkages, which may serve as the cellulose fingerprint region. Results show that BC may be a biosignature for search signs of living organisms in rock records.

Synthesis, crystal growth, structural, thermal and optical properties of naphthalene picrate an organic NLO material.

PubMed

Chandramohan, A; Bharathikannan, R; Kandavelu, V; Chandrasekaran, J; Kandhaswamy, M A

2008-12-01

Crystalline substance of naphthalene picrate (NP) was synthesized and single crystals were grown using slow evaporation solution growth technique. The solubility of the naphthalene picrate complex was estimated using different solvents such as chloroform and benzene. The material was characterized by elemental analysis, powder X-ray diffraction (XRD), nuclear magnetic resonance (NMR) and fourier transform-infrared (FT-IR) techniques. The electronic absorption was studied through UV-vis spectrophotometer. Thermal behavior and stability of the crystal were studied using thermogravimetric (TG) and differential thermal analysis (DTA) techniques. The second harmonic generation (SHG) of the material was confirmed using Nd:YAG laser.

Highly hydrophobic biopolymers prepared by the surface pentafluorobenzoylation of cellulose substrates.

PubMed

Cunha, Ana G; Freire, Carmen S R; Silvestre, Armando J D; Pascoal Neto, Carlos; Gandini, Alessandro; Orblin, Elina; Fardim, Pedro

2007-04-01

New highly hydrophobic/lipophobic biopolymers were prepared by the controlled heterogeneous pentafluorobenzoylation of cellulose substrates, i.e., plant and bacterial cellulose fibers. The characterization of the modified fibers was performed by elemental analysis, FTIR spectroscopy, X-ray diffraction, thermogravimetry, and surface analysis (XPS, ToF-SIMS, and contact angle measurements). The degree of substitution of the ensuing pentafluorobenzoylated fibers ranged from 0.014 to 0.39. The hydrolytic stability of these perfluorinated cellulose derivatives was also evaluated and showed that they were quite water stable, although of course the fluorinated moieties could readily be removed by hydrolysis in an aqueous alkaline medium.

Synthesis, spectroscopic, fluorescence properties and biological evaluation of novel Pd(II) and Cd(II) complexes of NOON tetradentate Schiff bases.

PubMed

Ali, Omyma A M

2014-01-01

The solid complexes of Pd(II) and Cd(II) with N,N/bis(salicylaldehyde)4,5-dimethyl-1,2-phenylenediamine (H2L(1)), and N,N/bis(salicylaldehyde)4,5-dichloro-1,2-phenylenediamine (H2L(2)) have been synthesized and characterized by several techniques using elemental analysis (CHN), FT-IR, (1)H NMR, UV-Vis spectra and thermal analysis. Elemental analysis data proved 1:1 stoichiometry for the reported complexes while spectroscopic data indicated square planar and octahedral geometries for Pd(II) and Cd(II) complexes, respectively. The prepared ligands, Pd(II) and Cd(II) complexes exhibited intraligand (π-π(∗)) fluorescence and can potentially serve as photoactive materials. Thermal behavior of the complexes was studied and kinetic parameters were determined by Coats-Redfern method. Both the ligands and their complexes have been screened for antimicrobial activities. Copyright © 2013 Elsevier B.V. All rights reserved.

Polymer monolithic capillary microextraction combined on-line with inductively coupled plasma MS for the determination of trace rare earth elements in biological samples.

PubMed

Zhang, Lin; Chen, Beibei; He, Man; Hu, Bin

2013-07-01

A rapid and sensitive method based on polymer monolithic capillary microextraction combined on-line with microconcentric nebulization inductively coupled plasma MS has been developed for the determination of trace/ultratrace rare earth elements in biological samples. For this purpose, the iminodiacetic acid modified poly(glycidyl methacrylate-trimethylolpropane trimethacrylate) monolithic capillary was prepared and characterized by SEM and FTIR spectroscopy. Factors affecting the extraction efficiency, such as sample pH, sample flow rate, sample/eluent volume, and coexisting ions were investigated in detail. Under the optimal conditions, the LODs for rare earth elements were in the range of 0.08 (Er) to 0.97 ng/L (Nd) with a sampling frequency of 8.5 h(-1), and the RSDs were between 1.5% (Sm) and 7.4% (Nd) (c = 20 ng/L, n = 7). The proposed method was successfully applied to the analysis of trace/ultratrace rare earth elements in human urine and serum samples, and the recoveries for the spiked samples were in the range of 82-105%. The developed method was simple, rapid, sensitive, and favorable for the analysis of trace/ultratrace rare earth elements in biological samples with limited sample volume. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Textural, Structural and Biological Evaluation of Hydroxyapatite Doped with Zinc at Low Concentrations

PubMed Central

Predoi, Daniela; Iconaru, Simona Liliana; Deniaud, Aurélien; Chevallet, Mireille; Michaud-Soret, Isabelle; Buton, Nicolas; Prodan, Alina Mihaela

2017-01-01

The present work was focused on the synthesis and characterization of hydroxyapatite doped with low concentrations of zinc (Zn:HAp) (0.01 < xZn < 0.05). The incorporation of low concentrations of Zn2+ ions in the hydroxyapatite (HAp) structure was achieved by co-precipitation method. The physico-chemical properties of the samples were characterized by X-ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), Scanning Electron Microscopy (SEM), zeta-potential, and DLS and N2-BET measurements. The results obtained by XRD and FTIR studies demonstrated that doping hydroxyapatite with low concentrations of zinc leads to the formation of a hexagonal structure with lattice parameters characteristic to hydroxyapatite. The XRD studies have also shown that the crystallite size and lattice parameters of the unit cell depend on the substitutions of Ca2+ with Zn2+ in the apatitic structure. Moreover, the FTIR analysis revealed that the water content increases with the increase of zinc concentration. Furthermore, the Energy Dispersive X-ray Analysis (EDAX) and XPS analyses showed that the elements Ca, P, O, and Zn were found in all the Zn:HAp samples suggesting that the synthesized materials were zinc doped hydroxyapatite, Ca10−xZnx(PO4)6(OH), with 0.01 ≤ xZn ≤ 0.05. Antimicrobial assays on Staphylococcus aureus and Escherichia coli bacterial strains and HepG2 cell viability assay were carried out. PMID:28772589

Evaluation of FTIR spectroscopy as diagnostic tool for colorectal cancer using spectral analysis

NASA Astrophysics Data System (ADS)

Dong, Liu; Sun, Xuejun; Chao, Zhang; Zhang, Shiyun; Zheng, Jianbao; Gurung, Rajendra; Du, Junkai; Shi, Jingsen; Xu, Yizhuang; Zhang, Yuanfu; Wu, Jinguang

2014-03-01

The aim of this study is to confirm FTIR spectroscopy as a diagnostic tool for colorectal cancer. 180 freshly removed colorectal samples were collected from 90 patients for spectrum analysis. The ratios of spectral intensity and relative intensity (/I1460) were calculated. Principal component analysis (PCA) and Fisher's discriminant analysis (FDA) were applied to distinguish the malignant from normal. The FTIR parameters of colorectal cancer and normal tissues were distinguished due to the contents or configurations of nucleic acids, proteins, lipids and carbohydrates. Related to nitrogen containing, water, protein and nucleic acid were increased significantly in the malignant group. Six parameters were selected as independent factors to perform discriminant functions. The sensitivity for FTIR in diagnosing colorectal cancer was 96.6% by discriminant analysis. Our study demonstrates that FTIR can be a useful technique for detection of colorectal cancer and may be applied in clinical colorectal cancer diagnosis.

Polycrystalline BiFeO{sub 3} thin film synthesized via sol-gel assisted spin coating technique for photosensitive application

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bogle, K. A., E-mail: kashinath.bogle@gmail.com; Narwade, R. D.; Mahabole, M. P.

2016-05-06

We are reporting photosensitivity property of BiFeO{sub 3} thin film under optical illumination. The thin film used for photosensitivity work was fabricated via sol-gel assisted spin coating technique. I-V measurements on the Cu/BiFeO{sub 3}/Al structure under dark condition show a good rectifying property and show dramatic blue shit in threshold voltage under optical illumination. The microstructure, morphology and elemental analysis of the films were characterized by using XRD, UV-Vis, FTIR, SEM and EDS.

Synthesis and In Vitro Antimicrobial Evaluation of New 1,3,4-Oxadiazoles Bearing 5-Chloro-2-methoxyphenyl Moiety.

PubMed

Prasanna Kumar, Basavapatna N; Mohana, Kikkeri N; Mallesha, Lingappa; Harish, Kikkeri P

2013-01-01

A series of new 1,3,4-oxadiazole derivatives, 4(a-h), containing 5-chloro-2-methoxy benzohydrazide moiety were synthesized by the reaction of 5-chloro-2-methoxybenzoate with different aromatic carboxylic acids. These newly synthesized compounds were characterized by FT-IR, (1)H NMR, mass spectra, and also by elemental analysis. All the newly synthesized compounds were screened for their antibacterial and antifungal activities. Antimicrobial studies revealed that compounds 4c, 4f, and 4g showed significant activity against tested strains.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Brozek, Eric M. ..; Washton, Nancy M.; Mueller, Karl T.

A series of silsesquioxane nanoparticles containing reactive internal organic functionalities throughout the entire particle body have been synthesized using a surfactant-free method with organosilanes as the sole precursors and a base catalyst. The organic functional groups incorporated are vinyl, allyl, mercapto, cyanoethyl, and cyanopropyl groups. The sizes and morphologies of the particles were characterized using SEM and nitrogen adsorption, while the compositions were confirmed using TGA, FT-IR, solid state NMR, and elemental analysis. The accessibility and reactivity of the functional groups inside the particles were demonstrated by performing bromination and reduction reactions in the interior of the particles.

Photophysical, electrochemical, thermal and aggregation properties of new metal phthalocyanines

NASA Astrophysics Data System (ADS)

Jeong, Jaemyeng; Kumar, Rangaraju Satish; Mergu, Naveen; Son, Young-A.

2017-11-01

In this study, the synthesis of di(ethylene glycol) naphthalene substituted metal-phthalocyanines was reported. These novel phthalocyanines were characterized by elemental and spectroscopic analysis, including 1H NMR, FT-IR, UV-Vis spectral and MALDI-TOF mass data. The aggregation behavior of these phthalocyanines was examined in chloroform at different concentrations, and we confirmed that the phthalocyanines were non-aggregated. Further thermal stability, electrochemical, theoretical studies and metal sensing properties also investigated. In addition, we successfully prepared phthalocyanine (6d) blended polyurethane electrospun (ES) nanofibers.

Cytotoxic evaluation of hydroxyapatite-filled and silica/hydroxyapatite-filled acrylate-based restorative composite resins: An in vitro study.

PubMed

Chadda, Harshita; Naveen, Sangeetha Vasudevaraj; Mohan, Saktiswaren; Satapathy, Bhabani K; Ray, Alok R; Kamarul, Tunku

2016-07-01

Although the physical and mechanical properties of hydroxyapatite-filled dental restorative composite resins have been examined, the biocompatibility of these materials has not been studied in detail. The purpose of this in vitro study was to analyze the toxicity of acrylate-based restorative composite resins filled with hydroxyapatite and a silica/hydroxyapatite combination. Five different restorative materials based on bisphenol A-glycidyl methacrylate (bis-GMA) and tri-ethylene glycol dimethacrylate (TEGDMA) were developed: unfilled (H0), hydroxyapatite-filled (H30, H50), and silica/hydroxyapatite-filled (SH30, SH50) composite resins. These were tested for in vitro cytotoxicity by using human bone marrow mesenchymal stromal cells. Surface morphology, elemental composition, and functional groups were determined by scanning electron microscopy (SEM), energy-dispersive x-ray spectroscopy (EDX), and Fourier-transformed infrared spectroscopy (FTIR). The spectra normalization, baseline corrections, and peak integration were carried out by OPUS v4.0 software. Both in vitro cytotoxicity results and SEM analysis indicated that the composite resins developed were nontoxic and supported cell adherence. Elemental analysis with EDX revealed the presence of carbon, oxygen, calcium, silicon, and gold, while the presence of methacrylate, hydroxyl, and methylene functional groups was confirmed through FTIR analysis. The characterization and compatibility studies showed that these hydroxyapatite-filled and silica/hydroxyapatite-filled bis-GMA/TEGDMA-based restorative composite resins are nontoxic to human bone marrow mesenchymal stromal cells and show a favorable biologic response, making them potential biomaterials. Copyright © 2016 Editorial Council for the Journal of Prosthetic Dentistry. Published by Elsevier Inc. All rights reserved.

Metal Complexes of New Bioactive Pyrazolone Phenylhydrazones; Crystal Structure of 4-Acetyl-3-methyl-1-phenyl-2-pyrazoline-5-one phenylhydrazone Ampp-Ph

PubMed Central

Idemudia, Omoruyi G.; Sadimenko, Alexander P.; Hosten, Eric C.

2016-01-01

The condensation reaction of phenylhydrazine and dinitrophenylhydrazine with 4-acetyl and 4-benzoyl pyrazolone precipitated air-stable acetyldinitrophenylhydrazone Ampp-Dh, benzoylphenylhydrazone Bmpp-Ph and benzoyldinitrophenylhydrazone Bmpp-Dh in their keto imine form; a study inspired by the burning interest for the development of new bioactive materials with novel properties that may become alternative therapeutic agents. Elemental analysis, FTIR, 1H, and 13C NMR, and mass spectroscopy have been used to justify their proposed chemical structures, which were in agreement with the single crystal structure of Bmpp-Dh earlier reported according to X-ray crystallography. The single crystal structure of 4-acetyl-3-methyl-1-phenyl--pyrazoline-5-one phenylhydrazone Ampp-Ph, which crystallizes in a triclinic crystal system with a P-1 (No. 2) space group is presented. Octahedral Mn(II), Ni(II), Co(II), and Cu(II) complexes of these respective ligands with two molecules each of the bidentate Schiff base, coordinating to the metal ion through the azomethine nitrogen C=N and the keto oxygen C=O, which were afforded by the reaction of aqueous solutions of the corresponding metal salts with the ligands are also reported. Their identity and proposed structures were according to elemental analysis, FTIR spectroscopy, UV-VIS spectrophotometry (electronic spectra) and Bohr magnetic moments, as well as thermogravimetric analysis (TGA) results. A look at the antibacterial and antioxidant activities of synthesized compounds using the methods of the disc diffusion against some selected bacterial isolates and 1,1-diphenyl-2-picryl-hydrazil (DPPH) respectively, showed biological activities in relation to employed standard medicinal drugs. PMID:27213342

Synthesis, spectroscopic characterization, crystal structure, DNA interaction study and invitro biological screenings of 4-(5-chloro-2-hydroxyphenylamino)-4-oxobut-2-enoic acid

NASA Astrophysics Data System (ADS)

Sirajuddin, Muhammad; Nooruddin; Ali, Saqib; McKee, Vickie; Khan, Shahan Zeb; Malook, Khan

2015-01-01

The titled compound, 4-(5-chloro-2-hydroxyphenylamino)-4-oxobut-2-enoic acid was synthesized and characterized by various techniques like elemental analyses, FT-IR, NMR (1H, and 13C) and single crystal X-ray structural analysis. The appearance of the OH peak of the carboxylic acid in the FT-IR and NMR spectra conform the formation of the compound. A good agreement was found between the calculated values of C, H, N and found values in elemental analysis that show the purity of the compound. Protons H2 and H3 are in cis conformation with each other as conformed both from 1H NMR as well as from single crystal X-ray analysis. The molecular structure of the title compound, C10H10NO3Cl, is stabilized by short intramolecular Osbnd H- - -O hydrogen bonds within the molecule. In the crystal structure, intermolecular Nsbnd H- - -O hydrogen bonds link molecules into zigzag chains resulting in a dendrimer like structure. The title compound was screened for biological activities like interaction with DNA, cytotoxicity, antitumor and antioxidant activities. DNA interaction study reveals that the binding mode of interaction of the compound with SS-DNA is intercalative as it results in hypochromism along with significant red shift of 5 nm. It was also found to be effective antioxidant of 2,2-diphenyl-1-picrylhydrazyl radical (DPPH) and show almost comparable antioxidant activity to that of the standard and known antioxidant, ascorbic acid, at higher concentration. The antitumor activity data of the compound shows that it can be used as potent antitumor agent.

Combining TXRF, FT-IR and GC-MS information for identification of inorganic and organic components in black pigments of rock art from Alero Hornillos 2 (Jujuy, Argentina).

PubMed

Vázquez, Cristina; Maier, Marta S; Parera, Sara D; Yacobaccio, Hugo; Solá, Patricia

2008-06-01

Archaeological samples are complex in composition since they generally comprise a mixture of materials submitted to deterioration factors largely dependent on the environmental conditions. Therefore, the integration of analytical tools such as TXRF, FT-IR and GC-MS can maximize the amount of information provided by the sample. Recently, two black rock art samples of camelid figures at Alero Hornillos 2, an archaeological site located near the town of Susques (Jujuy Province, Argentina), were investigated. TXRF, selected for inorganic information, showed the presence of manganese and iron among other elements, consistent with an iron and manganese oxide as the black pigment. Aiming at the detection of any residual organic compounds, the samples were extracted with a chloroform-methanol mixture and the extracts were analyzed by FT-IR, showing the presence of bands attributable to lipids. Analysis by GC-MS of the carboxylic acid methyl esters prepared from the sample extracts, indicated that the main organic constituents were saturated (C(16:0) and C(18:0)) fatty acids in relative abundance characteristic of degraded animal fat. The presence of minor C(15:0) and C(17:0) fatty acids and branched-chain iso-C(16:0) pointed to a ruminant animal source.

ATR-FTIR membrane-based sensor for the simultaneous determination of surfactant and oil total indices in industrial degreasing baths.

PubMed

Lucena, Rafael; Cárdenas, Soledad; Gallego, Mercedes; Valcárcel, Miguel

2006-03-01

Monitoring the exhaustion of alkaline degreasing baths is one of the main aspects in metal mechanizing industrial process control. The global level of surfactant, and mainly grease, can be used as ageing indicators. In this paper, an attenuated total reflection-Fourier transform infrared (ATR-FTIR) membrane-based sensor is presented for the determination of these parameters. The system is based on a micro-liquid-liquid extraction of the analytes through a polymeric membrane from the aqueous to the organic solvent layer which is in close contact with the internal reflection element and continuously monitored. Samples are automatically processed using a simple, robust sequential injection analysis (SIA) configuration, on-line coupled to the instrument. The global signal obtained for both families of compounds are processed via a multivariate calibration technique (partial least squares, PLS). Excellent correlation was obtained for the values given by the proposed method compared to those of the gravimetric reference one with very low error values for both calibration and validation.

An efficient and environment-friendly method of removing graphene oxide in wastewater and its degradation mechanisms.

PubMed

Zhang, Chao-Zhi; Li, Ting; Yuan, Yang; Xu, Jianqiang

2016-06-01

Graphene and graphene oxide (GO) have already existed in air, water and soil due to their popular application in functional materials. However, degradation of graphene and GO in wastewater has not been reported. Degradation of GO plays a key role in the elimination of graphene and GO in wastewater due to graphene being easily oxidized to GO. In this paper, GO was completely degraded to give CO2 by Photo-Fenton. The degradation intermediates were determined by UV-vis absorption spectra, elemental analysis (EA), fourier transform infrared (FT-IR) and liquid chromatography-mass spectrometry (LC-MS). Experimental results showed that graphene oxide was completely degraded to give CO2 after 28 days. Based on UV, FT-IR, LC-MS spectra and EA data of these degradation intermediates, the degradation mechanisms of GO were supposed. This paper suggests an efficient and environment-friendly method to degrade GO and graphene. Copyright © 2016 Elsevier Ltd. All rights reserved.

Ligand-tailored single-site silica supported titanium catalysts: Synthesis, characterization and towards cyanosilylation reaction

NASA Astrophysics Data System (ADS)

Xu, Wei; Li, Yani; Yu, Bo; Yang, Jindou; Zhang, Ying; Chen, Xi; Zhang, Guofang; Gao, Ziwei

2015-01-01

A successive anchoring of Ti(NMe2)4, cyclopentadiene and a O-donor ligand, 1-hydroxyethylbenzene (PEA), 1,1‧-bi-2-naphthol (Binol) or 2,3-dihydroxybutanedioic acid diethyl ester (Tartrate), on silica was conducted by SOMC strategy in moderate conditions. The silica, monitored by in-situ Fourier transform infrared spectroscopy (in-situ FT-IR), was pretreated at different temperatures (200, 500 and 800 °C). The ligand tailored silica-supported titanium complexes were characterized by in-situ FT-IR, 13C CP MAS-NMR, X-ray photoelectron spectroscopy (XPS), X-ray absorption near edge structure (XANES) and elemental analysis in detail, verifying that the surface titanium species are single sited. The catalytic activity of the ligand tailored single-site silica supported titanium complexes was evaluated by a cyanosilylation of benzaldehyde. The results showed that the catalytic activity is dependent strongly on the dehydroxylation temperatures of silica and the configuration of the ligands.

Silver nanoparticles with 4,4‧-dicyanamidobiphenyl ligand: Synthesis, photoluminescent and electroluminescent properties and DFT calculations

NASA Astrophysics Data System (ADS)

Chiniforoshan, Hossein; Khalesi, Sara Bahmanpour; Tabrizi, Leila; Hajipour, Abdol R.; Chermahini, Alireza Najafi; Karimzadeh, Morteza

2015-02-01

In this research, a new complex of 4,4‧-dicyanamidobiphenyl (bpH2) ligand, Ag(bpH) has been synthesized and characterized by FT-IR, UV-Vis spectroscopies, and elemental analysis. The morphology and size of complex were determined by the scanning electron microscopy (SEM) image. The diameter of the complex was about 61 nm and the nanoparticles were spherical. TGA result indicated that this complex was thermally stable. Also, photoluminescent and electroluminescent properties of Ag(bpH) were reported. The blue-green light emission was observed by fabricating double-layer devices using Ag(bpH) as electron-transport and NPB as hole-transport material. In addition, this complex was optimized by B3LYP/LANL2DZ method. The calculated FT-IR and UV-Vis data are in better agreement with the experimental results. In addition to DFT calculations, natural bond orbital (NBO) was also performed at the same level of theory.

Development of a percutaneous penetration predictive model by SR-FTIR.

PubMed

Jungman, E; Laugel, C; Rutledge, D N; Dumas, P; Baillet-Guffroy, A

2013-01-30

This work focused on developing a new evaluation criterion of percutaneous penetration, in complement to Log Pow and MW and based on high spatial resolution Fourier transformed infrared (FTIR) microspectroscopy with a synchrotron source (SR-FTIR). Classic Franz cell experiments were run and after 22 h molecule distribution in skin was determined either by HPLC or by SR-FTIR. HPLC data served as reference. HPLC and SR-FTIR results were compared and a new predictive criterion based from SR-FTIR results, named S(index), was determined using a multi-block data analysis technique (ComDim). A predictive cartography of the distribution of molecules in the skin was built and compared to OECD predictive cartography. This new criterion S(index) and the cartography using SR-FTIR/HPLC results provides relevant information for risk analysis regarding prediction of percutaneous penetration and could be used to build a new mathematical model. Copyright © 2012 Elsevier B.V. All rights reserved.

Synthesis, characterization and cytotoxicity of rare earth metal ion complexes of N,N‧-bis-(2-thiophenecarboxaldimine)-3,3‧-diaminobenzidene, Schiff base ligand

NASA Astrophysics Data System (ADS)

Shakir, Mohammad; Abbasi, Ambreen; Faraz, Mohammad; Sherwani, Asif

2015-12-01

Lanthanide complexes of La3+, Pr3+, Nd3+, Gd3+, Er3+ of general formula [Ln2 L(H2O)4(NO3)4](NO3)2·2H2O have been synthesized from Schiff base, N,N‧-bis-(2-thiophenecarboxaldimine)-3,3‧-diaminobenzidene. The complexes were characterized by elemental analysis, molar conductance, UV-Vis, fluorescence, FT-IR,1H NMR, mass spectroscopy, EDX, SEM and thermal analysis. FT-IR spectral data suggested that ligand coordinate with metal ions through azomethine nitrogen and uncondensed amino group. Molar conductance data revealed 1:2 electrolytic nature of complexes. From the analytical data, the stoichiometry of the complexes was found to be 1:2 (ligand:metal). Thephysico-chemical data suggested eight coordination number for Ln(III)Schiffbase complexes. SEM analysis shows morphological changes in the surfaces of complexes as compared to free ligand. Thermal decomposition profiles were consistent with proposed formulations. The anticancer activity of the complexes and theSchiffbase ligand has been studied towards human cervical cancer celllines (HeLa) and human breast cancer cell lines (MCF-7) and it was found that complexes exhibited greater activity than theSchiffbase.

Synthesis, spectral, crystallography and thermal investigations of novel Schiff base complexes of manganese (III) derived from heterocyclic β-diketone with aromatic and aliphatic diamine

NASA Astrophysics Data System (ADS)

Surati, Kiran R.; Thaker, B. T.

2010-01-01

The Schiff base tetradentate ligands N,N-bis-(3,5-dimethyl-1-p-tolyl-1H-pyrazol-4-ylmethylene)-ethane-1,2-diamine (H 2L 1), N,N-bis-(3,5-dimethyl-1-p-sulfonyl-1H-pyrazol-4-ylmethylene)-ethane-1,2-diamine (H 2L 2), N,N-bis-(3,5-dimethyl-1-p-tolyl-1H-pyrazol-4-ylmethylene)-benzene-1,2-diamine (H 2L 3) and N,N-bis-(3,5-dimethyl-1-p-sulfonyl-1H-pyrazol-4-ylmethylene)-benzene-1,2-diamine (H 2L 4) were prepared from the reaction between 5-oxo-3-methyl-1-p-tolyl-1H-pyrazole-4-carbaldehyde or 4-(4-formyl-5-oxo-3-methyl-pyrazol-1-yl)-benzenesulfonic acid and o-phenylenediamine or ethylenediamine. And these are characterized by elemental analysis, FT-IR, 1H NMR and GC-MS. The corresponding Schiff base complexes of Mn(III) were prepared by condensation of [Mn 3(μ 3-O)(OAc) 6(H 2O) 3]·3H 2O with ligands H 2L 1, H 2L 2, H 2L 3 and H 2L 4. All these complexes have been characterized by elemental analysis, magnetic susceptibility, X-ray crystallography, conductometry measurement, FT-IR, electronic spectra and mass (FAB) spectrometry. Thermal behaviour of the complexes has been studied by TGA, DTA and DSC. Electronic spectra and magnetic susceptibility measurements indicate octahedral stereochemistry of manganese (III) complexes, while non-electrolytic behaviour complexes indicate the absence of counter ion.

Synthesis, characterization, nucleic acid interactions and photoluminescent properties of methaniminium hydrazone Schiff base and its Mn(II), Co(II), Ni(II), Cu(II), Zn(II) and Cd(II) complexes

NASA Astrophysics Data System (ADS)

Sennappan, M.; Murali Krishna, P.; Hosamani, Amar A.; Hari Krishna, R.

2018-07-01

An environmental benign and efficient reaction was carried out via amine exchange and condensation reaction in water and methanol mixture (3:1) and absence of catalyst between 1-[3-(2-hydroxy benzylidene)amine)phenyl]ethanone and benzhydrazide yields methaniminium hydrazone Schiff base in high yield. The prepared ligand was structurally characterized by using single crystal XRD, elemental analysis and spectroscopy (UV-Vis, FT-IR, LC-MS and NMR) techniques. The crystal data indicates the ligand crystallizes in orthorhombic system with Pna21 space group. Further, the ligand was used in synthesis of mononuclear Mn(II), Co(II), Ni(II), Cu(II), Zn(II) and Cd(II) complexes and were characterized by elemental analysis, magnetic moment and spectroscopy (UV-Vis, FT-IR and ESR) studies. The spectral data showed that ligand is coordinated to the metal ion through azomethine nitrogen and methaniminium nitrogen. The DNA binding absorption titrations reveals that, ligand, L and its metal complexes, 1-6 are avid binders to CT- DNA. The apparent binding constant values of compounds are in the order of 106 M-1. The nuclease activity of ligand, L and its metal complexes, 1-6 were investigated by gel electrophoresis method using pUC18 DNA. The photoluminescent properties of the methaniminium hydrazone ligand, L and its various metal complexes, 1-6 were investigated. The emission spectra of both ligand (L) and metal complexes (1-6) exhibits emission in the range of blue to red.

On the Identification of Rayon/Viscose as a Major Fraction of Microplastics in the Marine Environment: Discrimination between Natural and Manmade Cellulosic Fibers Using Fourier Transform Infrared Spectroscopy

PubMed Central

Comnea-Stancu, Ionela Raluca; Wieland, Karin; Ramer, Georg; Schwaighofer, Andreas

2016-01-01

This work was sparked by the reported identification of man-made cellulosic fibers (rayon/viscose) in the marine environment as a major fraction of plastic litter by Fourier transform infrared (FT-IR) transmission spectroscopy and library search. To assess the plausibility of such findings, both natural and man-made fibers were examined using FT-IR spectroscopy. Spectra acquired by transmission microscopy, attenuated total reflection (ATR) microscopy, and ATR spectroscopy were compared. Library search was employed and results show significant differences in the identification rate depending on the acquisition method of the spectra. Careful selection of search parameters and the choice of spectra acquisition method were found to be essential for optimization of the library search results. When using transmission spectra of fibers and ATR libraries it was not possible to differentiate between man-made and natural fibers. Successful differentiation of natural and man-made cellulosic fibers has been achieved for FT-IR spectra acquired by ATR microscopy and ATR spectroscopy, and application of ATR libraries. As an alternative, chemometric methods such as unsupervised hierarchical cluster analysis, principal component analysis, and partial least squares-discriminant analysis were employed to facilitate identification based on intrinsic relationships of sample spectra and successful discrimination of the fiber type could be achieved. Differences in the ATR spectra depending on the internal reflection element (Ge versus diamond) were observed as expected; however, these did not impair correct classification by chemometric analysis. Moreover, the effects of different levels of humidity on the IR spectra of natural and man-made fibers were investigated, too. It has been found that drying and re-humidification leads to intensity changes of absorption bands of the carbohydrate backbone, but does not impair the identification of the fiber type by library search or cluster analysis. PMID:27650982

Green Synthesis of Silver Nanoparticles Using an Aqueous Extract of Monotheca buxifolia (Flac.) Dcne

NASA Astrophysics Data System (ADS)

Anwar, Natasha; Khan, Abbas; Shah, Mohib; Anwar, Saad

2018-01-01

This study deals with the synthesis and physicochemical investigation of silver nanoparticles using an aqueous extract of Monotheca buxifolia (Flac.). On the treatment of aqueous solution of silver nitrate with the plant extract, silver nanoparticles were rapidly fabricated. The synthesized particles were characterized by using UV-visible spectrophotometry (UV), Fourier transform infrared spectroscopy (FTIR), Energy dispersive X-ray (EDX) and Scanning electron microscopy (SEM). The formation of AgNPs was confirmed by noting the change in colour through visual observations as well as via UV-Vis spectroscopy. UV-Vis spectrum of the aqueous medium containing silver nanoparticles showed an absorption peak at around 440 nm. FTIR was used to identify the chemical composition of silver nanoparticles and Ag-capped plant extract. The presence of elemental silver was also confirmed through EDX analysis. The SEM analysis of the silver nanoparticles showed that they have a uniform spherical shape with an average size in the range of 40-78 nm. This green system showed better capping and stabilizing agent for the fine particles. Further, in vitro the antioxidant activity of Monotheca buxifolia (Flac.) and Ag-capped with the plant was also evaluated using FeCl3/K3Fe (CN)6 essay.

Structural and electrical properties of CZTS thin films by electrodeposition

NASA Astrophysics Data System (ADS)

Rao, M. C.; Basha, Sk. Shahenoor

2018-06-01

CZTS (Cu2ZnSnS4) thin films were coated on ITO glass substrates by single bath electrodeposition technique. The prepared films were subsequently characterized by XRD, SEM, FTIR, UV-visible spectroscopy and Raman studies. The thickness of the thin films was measured by wedge method. X-ray diffraction studies revealed the formation of polycrystalline phase. The morphological surface of the prepared thin films was examined by SEM and AFM and showed the presence of microcrystals on the surface of the samples. The elemental analysis and their compositional ratios present in the samples were confirmed by the energy dispersive X-ray analysis. Functional groups and the position of band structure involved in the materials were confirmed by FTIR. Optical absorption studies were performed on the prepared thin films in the wavelength ranging from 300 to 1000 nm and the energy bandgap values were found to be in the range from 1.39 to 1.60 eV. Raman spectral peak which was observed at 360 cm-1 correspond to kesterite phase, was formed due to the vibration of the molecules. Electrical measurements confirmed the nature of the thin film depending on the charge concentration present in the samples.

Copper(II) complexes of methimazole, an anti Grave's disease drug. Synthesis, characterization and its potential biological behavior as alkaline phosphatase inhibitor.

PubMed

Urquiza, Nora M; Manca, Silvia G; Moyano, María A; Dellmans, Raquel Arrieta; Lezama, Luis; Rojo, Teófilo; Naso, Luciana G; Williams, Patricia A M; Ferrer, Evelina G

2010-04-01

Methimazole (MeimzH) is an anti-thyroid drug and the first choice for patients with Grave's disease. Two new copper(II) complexes of this drug: [Cu(MeimzH)(2)(NO(3))(2)]*0.5H(2)O and [Cu(MeimzH)(2)(H(2)O)(2)](NO(3))(2)*H(2)O were synthesized and characterized by elemental analysis, dissolution behavior, thermogravimetric analysis and UV-vis, diffuse reflectance, FTIR and EPR spectroscopies. As it is known that copper(II) cation can act as an inhibitor of alkaline phosphatase (ALP), the inhibitory effect of methimazole and its copper(II) complexes on ALP activity has also been investigated.

Influence of boiling point range of feedstock on properties of derived mesophase pitch

NASA Astrophysics Data System (ADS)

Yu, Ran; Liu, Dong; Lou, Bin; Chen, Qingtai; Zhang, Yadong; Li, Zhiheng

2018-06-01

The composition of raw material was optimized by vacuum distillation. The carbonization behavior of two kinds of raw material was followed by polarizing microscope, softening point, carbon yield and solubility. Two kinds of mesophase pitch have been monitored by X-ray diffraction (XRD), Fourier transform infrared spectrometer (FTIR), elemental analysis and 1H nuclear magnetic resonance (1H-NMR). The analysis results suggested that raw material B (15wt% of A was distillated out and the residue named B) could form large domain mesophase pitch earlier. The shortened heat treat time favored the retaining of alkyl group in mesophase pitch and reduced the softening point of masophase pitch.

Sulfonamide-containing PTP 1B inhibitors: Docking studies, synthesis and model validation

NASA Astrophysics Data System (ADS)

Niu, Enli; Gan, Qiang; Chen, Xi; Feng, Changgen

2017-01-01

PTP 1B plays an important role in regulating insulin signaling pathway and is regarded as a valid target for curing diabetes and obesity. In this paper, two novel sulfonamide-containing PTP 1B inhibitors were designed, synthesized in mild condition, and characterized by FT-IR, 1H NMR, 13C NMR and elemental analysis. The single crystal of compounds 7 and 8 were obtained and their structures were determined by X-ray single crystal diffraction analysis. In addition, their inhibitory activity were predicted by genetic algorithm, and carried on in vitro enzyme activity test. Of which compound 8 showed good inhibitory activity, in consistent with docking studies.

SbCl3-catalyzed one-pot synthesis of 4,4′-diaminotriarylmethanes under solvent-free conditions: Synthesis, characterization, and DFT studies

PubMed Central

2011-01-01

Summary A simple, efficient, and mild procedure for a solvent-free one-step synthesis of various 4,4′-diaminotriarylmethane derivatives in the presence of antimony trichloride as catalyst is described. Triarylmethane derivatives were prepared in good to excellent yields and characterized by elemental analysis, FTIR, 1H and 13C NMR spectroscopic techniques. The structural and vibrational analysis were investigated by performing theoretical calculations at the HF and DFT levels of theory by standard 6-31G*, 6-31G*/B3LYP, and B3LYP/cc-pVDZ methods and good agreement was obtained between experimental and theoretical results. PMID:21445373

Synthesis, characterization and biological activities of copper(II) complex of 2-Benzimidazolyl-urea and the nitrate salt of 2-Benzimidazolyl-urea

NASA Astrophysics Data System (ADS)

Poyraz, Mehmet; Sari, Musa; Banti, Christina N.; Hadjikakou, Sotiris K.

2017-10-01

The synthesis of the complex {[Cu(BZIMU)2](NO3)2} (1) (BZIMU = 2-Benzimidazolyl-urea) is reported here. The complex 1 was characterized by elemental analysis, FT-IR, magnetic susceptibility and molar conductance measurements. The crystal structures of 1 and of the nitrate salt of [(BZIMUH+)(NO3)-] (2) were determined by X-ray diffraction analysis. The copper complex 1 and [(BZIMUH+)(NO3)-] (2) were evaluated for their in vitro cytotoxic activity (cell viability) against human cervix adenocarcinoma (HeLa) and human breast adenocarcinoma (MCF-7) cell line and normal human fetal lung fibroblast cells (MRC-5) with SRB assay.

Characterization of Natural Dyes and Traditional Korean Silk Fabric by Surface Analytical Techniques

PubMed Central

Lee, Jihye; Kang, Min Hwa; Lee, Kang-Bong; Lee, Yeonhee

2013-01-01

Time-of-flight secondary ion mass spectrometry (TOF-SIMS) and X-ray photoelectron spectroscopy (XPS) are well established surface techniques that provide both elemental and organic information from several monolayers of a sample surface, while also allowing depth profiling or image mapping to be carried out. The static TOF-SIMS with improved performances has expanded the application of TOF-SIMS to the study of a variety of organic, polymeric and biological materials. In this work, TOF-SIMS, XPS and Fourier Transform Infrared (FTIR) measurements were used to characterize commercial natural dyes and traditional silk fabric dyed with plant extracts dyes avoiding the time-consuming and destructive extraction procedures necessary for the spectrophotometric and chromatographic methods previously used. Silk textiles dyed with plant extracts were then analyzed for chemical and functional group identification of their dye components and mordants. TOF-SIMS spectra for the dyed silk fabric showed element ions from metallic mordants, specific fragment ions and molecular ions from plant-extracted dyes. The results of TOF-SIMS, XPS and FTIR are very useful as a reference database for comparison with data about traditional Korean silk fabric and to provide an understanding of traditional dyeing materials. Therefore, this study shows that surface techniques are useful for micro-destructive analysis of plant-extracted dyes and Korean dyed silk fabric. PMID:28809257

Multi-spectroscopic analysis of cholesterol gallstone using TOF-SIMS, FTIR and UV-Vis spectroscopy

NASA Astrophysics Data System (ADS)

Jaswal, Brij Bir S.; Kumar, Vinay; Swart, H. C.; Sharma, Jitendra; Rai, Pradeep K.; Singh, Vivek K.

2015-10-01

For the first time, spatial distribution of major and trace elements has been studied in cholesterol gallstones using time-of-flight secondary mass ion mass spectrometry (TOF-SIMS). The TOF-SIMS has been used to study the elemental constituents of the center and surface parts of the gallstone sample. We have classified the gallstone sample using Fourier transform spectroscopy. The detected elements in cholesterol gallstone sample were carbon (C), hydrogen (H), calcium (Ca), sodium (Na), potassium (K), strontium (Sr), copper (Cu), iron (Fe), chromium (Cr), mercury (Hg) and lead (Pb). The detected molecules in the cholesterol gallstone were CH3 +, CO3 +, CaCO3 + and C3H+. Our results revealed that the contents of these elements in cholesterol gallstone were higher in the center part than that in the surface part. In the present paper, we have also presented the UV-Vis spectroscopic studies of the center and surface parts of the gallstone sample which indicated the presence of a higher content of cholesterol in the surface part and bilirubin in the center part.

Synthesis, spectroscopic characterization and biological activities of N4O2 Schiff base ligand and its metal complexes of Co(II), Ni(II), Cu(II) and Zn(II)

NASA Astrophysics Data System (ADS)

Al-Resayes, Saud I.; Shakir, Mohammad; Abbasi, Ambreen; Amin, Kr. Mohammad Yusuf; Lateef, Abdul

The Schiff base ligand, bis(indoline-2-one)triethylenetetramine (L) obtained from condensation of triethylenetetramine and isatin was used to synthesize the complexes of type, [ML]Cl2 [M = Co(II), Ni(II), Cu(II) and Zn(II)]. L was characterized on the basis of the results of elemental analysis, FT-IR, 1H and 13C NMR, mass spectroscopic studies. The stoichiometry, bonding and stereochemistries of complexes were ascertained on the basis of results of elemental analysis, magnetic susceptibility values, molar conductance and various spectroscopic studies. EPR, UV-vis and magnetic moments revealed an octahedral geometry for complexes. L and its Cu(II) and Zn(II) complexes were screened for their antibacterial activity. Analgesic activity of Cu(II) and Zn(II) complexes was also tested in rats by tail flick method. Both complexes were found to possess good antibacterial and moderate analgesic activity.

Synthesis and In Vitro Antimicrobial Evaluation of New 1,3,4-Oxadiazoles Bearing 5-Chloro-2-methoxyphenyl Moiety

PubMed Central

Prasanna Kumar, Basavapatna N.; Mohana, Kikkeri N.; Mallesha, Lingappa; Harish, Kikkeri P.

2013-01-01

A series of new 1,3,4-oxadiazole derivatives, 4(a–h), containing 5-chloro-2-methoxy benzohydrazide moiety were synthesized by the reaction of 5-chloro-2-methoxybenzoate with different aromatic carboxylic acids. These newly synthesized compounds were characterized by FT-IR, 1H NMR, mass spectra, and also by elemental analysis. All the newly synthesized compounds were screened for their antibacterial and antifungal activities. Antimicrobial studies revealed that compounds 4c, 4f, and 4g showed significant activity against tested strains. PMID:25374693

Synthesis and characterization of bis-thiourea having amino acid derivatives

NASA Astrophysics Data System (ADS)

Fakhar, Imran; Yamin, Bohari M.; Hasbullah, Siti Aishah

2016-11-01

In this article four new symmetric bis-thiourea derivatives having amino acid linkers were reported with good yield. Isophthaloyl dichloride was used as spacer and L-alanine, L-aspartic acid, L-phenylalanine and L-glutamic acid were used as linkers. Bis-thiourea derivatives were prepared from relatively stable isophthaloyl isothiocyanate intermediate. Newly synthesized bis-thiourea derivatives were characterized by FTIR, H-NMR, 13C-NMR and CHNS-O elemental analysis techniques. Characterization data was in good agreement with the expected derivatives, hence confirmed the synthesis of four new derivatives of bis-thiourea having amino acids.

Synthesis of Novel Compounds as New Potent Tyrosinase Inhibitors

PubMed Central

Hamidian, Hooshang

2013-01-01

In the present paper, we report the synthesis and pharmacological evaluation of a new series of azo compounds with different groups (1-naphthol, 2-naphthol, and N,N-dimethylaniline) and trifluoromethoxy and fluoro substituents in the scaffold. All synthesized compounds (5a–5f) showed the most potent mushroom tyrosinase inhibition (IC50 values in the range of 4.39 ± 0.76–1.71 ± 0.49 µM), comparable to the kojic acid, as reference standard inhibitor. All the novel compounds were characterized by FT-IR, 1H NMR, 13C NMR, and elemental analysis. PMID:24260737

Sugar and acid content of Citrus prediction modeling using FT-IR fingerprinting in combination with multivariate statistical analysis.

PubMed

Song, Seung Yeob; Lee, Young Koung; Kim, In-Jung

2016-01-01

A high-throughput screening system for Citrus lines were established with higher sugar and acid contents using Fourier transform infrared (FT-IR) spectroscopy in combination with multivariate analysis. FT-IR spectra confirmed typical spectral differences between the frequency regions of 950-1100 cm(-1), 1300-1500 cm(-1), and 1500-1700 cm(-1). Principal component analysis (PCA) and subsequent partial least square-discriminant analysis (PLS-DA) were able to discriminate five Citrus lines into three separate clusters corresponding to their taxonomic relationships. The quantitative predictive modeling of sugar and acid contents from Citrus fruits was established using partial least square regression algorithms from FT-IR spectra. The regression coefficients (R(2)) between predicted values and estimated sugar and acid content values were 0.99. These results demonstrate that by using FT-IR spectra and applying quantitative prediction modeling to Citrus sugar and acid contents, excellent Citrus lines can be early detected with greater accuracy. Copyright © 2015 Elsevier Ltd. All rights reserved.

The characterization of natural gemstones using non-invasive FT-IR spectroscopy: New data on tourmalines.

PubMed

Mercurio, Mariano; Rossi, Manuela; Izzo, Francesco; Cappelletti, Piergiulio; Germinario, Chiara; Grifa, Celestino; Petrelli, Maurizio; Vergara, Alessandro; Langella, Alessio

2018-02-01

Fourteen samples of tourmaline from the Real Museo Mineralogico of Federico II University (Naples) have been characterized through multi-methodological investigations (EMPA-WDS, SEM-EDS, LA-ICP-MS, and FT-IR spectroscopy). The samples show different size, morphology and color, and are often associated with other minerals. Data on major and minor elements allowed to identify and classify tourmalines as follows: elbaites, tsilaisite, schorl, dravites, uvites and rossmanite. Non-invasive, non-destructive FT-IR and in-situ analyses were carried out on the same samples to validate this chemically-based identification and classification. The results of this research show that a complete characterization of this mineral species, usually time-consuming and expensive, can be successfully achieved through non-destructive FT-IR technique, thus representing a reliable tool for a fast classification extremely useful to plan further analytical strategies, as well as to support gemological appraisals. Copyright © 2017 Elsevier B.V. All rights reserved.

Composition of dissolved organic matter (DOM) from periodically submerged soils in the Three Gorges Reservoir areas as determined by elemental and optical analysis, infrared spectroscopy, pyrolysis-GC-MS and thermally assisted hydrolysis and methylation.

PubMed

Jiang, Tao; Kaal, Joeri; Liang, Jian; Zhang, Yaoling; Wei, Shiqiang; Wang, Dingyong; Green, Nelson W

2017-12-15

Soil-derived dissolved organic matter (DOM) has a major influence in biogeochemical processes related to contaminant dynamics and greenhouse gas emissions, due to its reactivity and its bridging role between the soil and aquatic systems. Within the Three Gorges Reservoir (TGR, China) area, an extensive water-fluctuation zone periodically submerges the surrounding soils. Here we report a characterization study of soil-derived DOM across the TGR areas, using elemental and optical analysis, infrared spectroscopy (FTIR), pyrolysis-GC-MS (Py-GC-MS) and thermally assisted hydrolysis and methylation (THM-GC-MS). The results showed that the soil DOM from the TGR area is a mixture of "allochthonous" (i.e., plant-derived/terrigenous) and "autochthonous" (i.e., microbial) origins. The terrigenous DOM is composed primarily of phenolic and aliphatic structures from lignin and aliphatic biopolymers (i.e. cutin, suberin), respectively. Multivariate statistics differentiated between two fractions of the microbial DOM, i.e. chitin-derived, perhaps from fungi and arthropods in soil, and protein-derived, partially sourced from algal or aquatic organisms. Molecular proxies of source and degradation state were in good agreement with optical parameters such as SUVA 254 , the fluorescence index (FI) and the humification index (HIX). The combined use of elemental analysis, fluorescence spectroscopy, and Py-GC-MS provides rigorous and detailed DOM characterization, whereas THM-GC-MS is useful for more precise but qualitative identification of the different phenolic (cinnamyl, p-hydroxyphenyl, guaiacyl, syringyl and tannin-derived) and aliphatic materials. With the multi-methodological approach used in this study, FTIR was the least informative, in part, because of the interference of inorganic matter in the soil DOM samples. The soil DOM from the TGR's water fluctuation zone exhibited considerable compositional diversity, mainly related to the balance between DOM source (microbial- or plant-derived), local vegetation and anthropogenic activities (e.g., agriculture). Finally, the relationship between DOM composition and its potential reactivity with substances of environmental concerns in the TGR area are also discussed. Copyright © 2017 Elsevier B.V. All rights reserved.

FTIR gas chromatographic analysis of perfumes

NASA Astrophysics Data System (ADS)

Diederich, H.; Stout, Phillip J.; Hill, Stephen L.; Krishnan, K.

1992-03-01

Perfumes, natural or synthetic, are complex mixtures consisting of numerous components. Gas chromatography (GC) and gas chromatography-mass spectrometry (GC-MS) techniques have been extensively utilized for the analysis of perfumes and essential oils. A limited number of perfume samples have also been analyzed by FT-IR gas chromatographic (GC-FTIR) techniques. Most of the latter studies have been performed using the conventional light pipe (LP) based GC-FTIR systems. In recent years, cold-trapping (in a matrix or neat) GC-FTIR systems have become available. The cold-trapping systems are capable of sub-nanogram sensitivities. In this paper, comparison data between the LP and the neat cold-trapping GC- FTIR systems is presented. The neat cold-trapping interface is known as Tracer. The results of GC-FTIR analysis of some commercial perfumes is also presented. For comparison of LP and Tracer GC-FTIR systems, a reference (synthetic) mixture containing 16 major and numerous minor constituents was used. The components of the mixture are the compounds commonly encountered in commercial perfumes. The GC-FTIR spectra of the reference mixture was obtained under identical chromatographic conditions from an LP and a Tracer system. A comparison of the two sets of data thus generated do indeed show the enhanced sensitivity level of the Tracer system. The comparison also shows that some of the major components detected by the Tracer system were absent from the LP data. Closer examination reveals that these compounds undergo thermal decomposition on contact with the hot gold surface that is part of the LP system. GC-FTIR data were obtained for three commercial perfume samples. The major components of these samples could easily be identified by spectra search against a digitized spectral library created using the Tracer data from the reference mixture.

Alteration behavior of mineral structure and hazardous elements during combustion of coal from a power plant at Huainan, Anhui, China.

PubMed

Tang, Quan; Sheng, Wanqi; Li, Liyuan; Zheng, Liugen; Miao, Chunhui; Sun, Ruoyu

2018-08-01

The alteration behavior of minerals and hazardous elements during simulated combustion (100-1200 °C) of a raw coal collected from a power plant were studied. Thermogravimetric analysis indicated that there were mainly four alteration stages during coal combustion. The transformation behavior of mineral phases of raw coal, which were detected by X-ray polycrystalline diffraction (XRD) technique, mainly relied on the combustion temperature. A series of changes were derived from the intensities of mineral (e.g. clays) diffraction peaks when temperature surpassed 600 °C. Mineral phases tended to be simple and collapsed to amorphous glass when temperature reached up to 1200 °C. The characteristics of functional groups for raw coal and high-temperature (1200 °C) ash studied by Fourier transform infrared spectroscopy (FTIR) were in accordance with the result obtained from XRD analysis. The volatilization ratios of Co, Cr, Ni and V increased consistently with the increase of combustion temperature, suggesting these elements were gradually released from the organic matter and inorganic minerals of coal. Copyright © 2018 Elsevier Ltd. All rights reserved.

The classification of lung cancers and their degree of malignancy by FTIR, PCA-LDA analysis, and a physics-based computational model.

PubMed

Kaznowska, E; Depciuch, J; Łach, K; Kołodziej, M; Koziorowska, A; Vongsvivut, J; Zawlik, I; Cholewa, M; Cebulski, J

2018-08-15

Lung cancer has the highest mortality rate of all malignant tumours. The current effects of cancer treatment, as well as its diagnostics, are unsatisfactory. Therefore it is very important to introduce modern diagnostic tools, which will allow for rapid classification of lung cancers and their degree of malignancy. For this purpose, the authors propose the use of Fourier Transform InfraRed (FTIR) spectroscopy combined with Principal Component Analysis-Linear Discriminant Analysis (PCA-LDA) and a physics-based computational model. The results obtained for lung cancer tissues, adenocarcinoma and squamous cell carcinoma FTIR spectra, show a shift in wavenumbers compared to control tissue FTIR spectra. Furthermore, in the FTIR spectra of adenocarcinoma there are no peaks corresponding to glutamate or phospholipid functional groups. Moreover, in the case of G2 and G3 malignancy of adenocarcinoma lung cancer, the absence of an OH groups peak was noticed. Thus, it seems that FTIR spectroscopy is a valuable tool to classify lung cancer and to determine the degree of its malignancy. Copyright © 2018 Elsevier B.V. All rights reserved.

Classification and identification of Rhodobryum roseum Limpr. and its adulterants based on fourier-transform infrared spectroscopy (FTIR) and chemometrics.

PubMed

Cao, Zhen; Wang, Zhenjie; Shang, Zhonglin; Zhao, Jiancheng

2017-01-01

Fourier-transform infrared spectroscopy (FTIR) with the attenuated total reflectance technique was used to identify Rhodobryum roseum from its four adulterants. The FTIR spectra of six samples in the range from 4000 cm-1 to 600 cm-1 were obtained. The second-derivative transformation test was used to identify the small and nearby absorption peaks. A cluster analysis was performed to classify the spectra in a dendrogram based on the spectral similarity. Principal component analysis (PCA) was used to classify the species of six moss samples. A cluster analysis with PCA was used to identify different genera. However, some species of the same genus exhibited highly similar chemical components and FTIR spectra. Fourier self-deconvolution and discrete wavelet transform (DWT) were used to enhance the differences among the species with similar chemical components and FTIR spectra. Three scales were selected as the feature-extracting space in the DWT domain. The results show that FTIR spectroscopy with chemometrics is suitable for identifying Rhodobryum roseum and its adulterants.

Study binding of Al-curcumin complex to ds-DNA, monitoring by multispectroscopic and voltammetric techniques

NASA Astrophysics Data System (ADS)

Ahmadi, F.; Alizadeh, A. A.; Shahabadi, N.; Rahimi-Nasrabadi, M.

2011-09-01

In this work a complex of Al 3+ with curcumin ([Al(curcumin) (EtOH) 2](NO 3) 2) was synthesized and characterized by UV-vis, FT-IR, elemental analysis and spectrophotometric titration techniques. The mole ratio plot revealed a 1:1 complex between Al 3+ and curcumin in solution. For binding studies of this complex to calf thymus-DNA various methods such as: UV-vis, fluorescence, circular dichroism (CD), FT-IR spectroscopy and cyclic voltammetry were used. The intrinsic binding constant of ACC with DNA at 25 °C was calculated by UV-vis and cyclic voltammetry as 2.1 × 10 4 and 2.6 × 10 4, respectively. The thermodynamic studies showed that the reaction is enthalpy and entropy favored. The CD results showed that only the Δ-ACC interacts with DNA and the Δ-ACC form has not any tendency to interact with DNA, also the pure curcumin has not any stereoselective interaction with CT-DNA. Fluorimetric studies showed that fluorescence enhancement was initiated by a static process in the ground state. The cyclic voltammetry showed that ACC interact with DNA with a binding site size of 2. From the FT-IR we concluded that the Δ-ACC interacts with DNA via partial electrostatic and minor groove binding. In comparison with previous works it was concluded that curcumin significantly reduced the affinity of Al 3+ to the DNA.

FTIR MONITORING OF THE VENTILATION AIR OF CRITICAL BUILDINGS

EPA Science Inventory

Fourier transform infrared (FTIR) spectroscopy has been used for detailed analysis of environmental and industrial process samples for many years. FTIR spectrometers have the capability of measuring multiple compounds simultaneously, thus providing an advantage over most other me...

Fourier Transform Infrared Spectroscopy (FTIR) and Multivariate Analysis for Identification of Different Vegetable Oils Used in Biodiesel Production

PubMed Central

Mueller, Daniela; Ferrão, Marco Flôres; Marder, Luciano; da Costa, Adilson Ben; de Cássia de Souza Schneider, Rosana

2013-01-01

The main objective of this study was to use infrared spectroscopy to identify vegetable oils used as raw material for biodiesel production and apply multivariate analysis to the data. Six different vegetable oil sources—canola, cotton, corn, palm, sunflower and soybeans—were used to produce biodiesel batches. The spectra were acquired by Fourier transform infrared spectroscopy using a universal attenuated total reflectance sensor (FTIR-UATR). For the multivariate analysis principal component analysis (PCA), hierarchical cluster analysis (HCA), interval principal component analysis (iPCA) and soft independent modeling of class analogy (SIMCA) were used. The results indicate that is possible to develop a methodology to identify vegetable oils used as raw material in the production of biodiesel by FTIR-UATR applying multivariate analysis. It was also observed that the iPCA found the best spectral range for separation of biodiesel batches using FTIR-UATR data, and with this result, the SIMCA method classified 100% of the soybean biodiesel samples. PMID:23539030

Group 12 dithiocarbamate complexes: Synthesis, spectral studies and their use as precursors for metal sulfides nanoparticles and nanocomposites

NASA Astrophysics Data System (ADS)

Ajibade, Peter A.; Ejelonu, Benjamin C.

2013-09-01

Zn(II), Cd(II) and Hg(II) dithiocarbamate complexes have been synthesized and characterized by elemental analysis, thermogravimetric analysis, UV-Vis, FTIR, 1H- and 13C NMR spectroscopy. The complexes were thermolysed at 180 °C and used as single molecule precursors for the synthesis of HDA capped ZnS, CdS and HgS nanoparticles and polymethylmethacrylate (PMMA) nanocomposites. The optical and structural properties of the nanoparticles and nanocomposites were studied by UV-Vis, PL, XRD and SEM. The crystallites sizes of the nanoparticles varied between 3.03 and 23.45 nm. SEM and EDX analyses of the nanocomposites confirmed the presence of the nanoparticles in the polymer matrix.

Synthesis and film formation of furfuryl- and maleimido carbonic acid derivatives of dextran.

PubMed

Elschner, Thomas; Obst, Franziska; Stana-Kleinschek, Karin; Kargl, Rupert; Heinze, Thomas

2017-04-01

Carbonic acid derivatives of dextran possessing furfuryl- and maleimido moieties were synthesized and processed into thin films by spin coating. First, products with different degrees of substitution (DS) of up to 3.0 and substitution patterns were obtained and characterized by NMR- and FTIR spectroscopy, as well as elemental analysis. Thin films possessing maleimide groups were obtained by spin coating of maleimido dextran (furan-protected) and dextran furfuryl carbamate that was converted with bismaleimide. The removal of the protecting group (furan) on the thin film was monitored by QCM-D and compared with gravimetric analysis of the bulk material. Film morphology and wettability were determined by means of AFM and contact angle measurements. Copyright © 2016 Elsevier Ltd. All rights reserved.

Synthesis, spectral, crystallography and thermal investigations of novel Schiff base complexes of manganese (III) derived from heterocyclic beta-diketone with aromatic and aliphatic diamine.

PubMed

Surati, Kiran R; Thaker, B T

2010-01-01

The Schiff base tetradentate ligands N,N-bis-(3,5-dimethyl-1-p-tolyl-1H-pyrazol-4-ylmethylene)-ethane-1,2-diamine (H(2)L(1)), N,N-bis-(3,5-dimethyl-1-p-sulfonyl-1H-pyrazol-4-ylmethylene)-ethane-1,2-diamine (H(2)L(2)), N,N-bis-(3,5-dimethyl-1-p-tolyl-1H-pyrazol-4-ylmethylene)-benzene-1,2-diamine (H(2)L(3)) and N,N-bis-(3,5-dimethyl-1-p-sulfonyl-1H-pyrazol-4-ylmethylene)-benzene-1,2-diamine (H(2)L(4)) were prepared from the reaction between 5-oxo-3-methyl-1-p-tolyl-1H-pyrazole-4-carbaldehyde or 4-(4-formyl-5-oxo-3-methyl-pyrazol-1-yl)-benzenesulfonic acid and o-phenylenediamine or ethylenediamine. And these are characterized by elemental analysis, FT-IR, (1)H NMR and GC-MS. The corresponding Schiff base complexes of Mn(III) were prepared by condensation of [Mn(3)(mu(3)-O)(OAc)(6)(H(2)O)(3)].3H(2)O with ligands H(2)L(1), H(2)L(2), H(2)L(3) and H(2)L(4). All these complexes have been characterized by elemental analysis, magnetic susceptibility, X-ray crystallography, conductometry measurement, FT-IR, electronic spectra and mass (FAB) spectrometry. Thermal behaviour of the complexes has been studied by TGA, DTA and DSC. Electronic spectra and magnetic susceptibility measurements indicate octahedral stereochemistry of manganese (III) complexes, while non-electrolytic behaviour complexes indicate the absence of counter ion. Copyright 2009. Published by Elsevier B.V.

TG-FTIR analysis on pyrolysis and combustion of marine sediment

NASA Astrophysics Data System (ADS)

Oudghiri, Fatiha; Allali, Nabil; Quiroga, José María; Rodríguez-Barroso, María Rocío

2016-09-01

In this paper, the pyrolysis and combustion of sediment have been compared using thermogravimetric analysis (TG) coupled with Fourier transform infrared spectrometry (TG-FTIR) analysis. The TG results showed that both the pyrolysis and combustion of sediment presented four weight loss stages, each. The evolving gaseous products during pyrolysis were H2O, CO2 and hydrocarbons, while combustion yielded considerable amounts of CO2, in addition to H2O, CO, Cdbnd C, Cdbnd O and NH3. Comparing the pyrolysis and combustion TG-FTIR curves, it is possible to evaluate the effect of oxygen presence in the temperature range of 200-600 °C, which increases the volatilisation rate of organic matter in sediment. For the better detection of organic and inorganic matter in sediment by TG-FTIR analysis it is recommended to work in combustion mode of sediment.

Analysis of environmental microplastics by vibrational microspectroscopy: FTIR, Raman or both?

PubMed

Käppler, Andrea; Fischer, Dieter; Oberbeckmann, Sonja; Schernewski, Gerald; Labrenz, Matthias; Eichhorn, Klaus-Jochen; Voit, Brigitte

2016-11-01

The contamination of aquatic ecosystems with microplastics has recently been reported through many studies, and negative impacts on the aquatic biota have been described. For the chemical identification of microplastics, mainly Fourier transform infrared (FTIR) and Raman spectroscopy are used. But up to now, a critical comparison and validation of both spectroscopic methods with respect to microplastics analysis is missing. To close this knowledge gap, we investigated environmental samples by both Raman and FTIR spectroscopy. Firstly, particles and fibres >500 μm extracted from beach sediment samples were analysed by Raman and FTIR microspectroscopic single measurements. Our results illustrate that both methods are in principle suitable to identify microplastics from the environment. However, in some cases, especially for coloured particles, a combination of both spectroscopic methods is necessary for a complete and reliable characterisation of the chemical composition. Secondly, a marine sample containing particles <400 μm was investigated by Raman imaging and FTIR transmission imaging. The results were compared regarding number, size and type of detectable microplastics as well as spectra quality, measurement time and handling. We show that FTIR imaging leads to significant underestimation (about 35 %) of microplastics compared to Raman imaging, especially in the size range <20 μm. However, the measurement time of Raman imaging is considerably higher compared to FTIR imaging. In summary, we propose a further size division within the smaller microplastics fraction into 500-50 μm (rapid and reliable analysis by FTIR imaging) and into 50-1 μm (detailed and more time-consuming analysis by Raman imaging). Graphical Abstract Marine microplastic sample (fraction <400 μm) on a silicon filter (middle) with the corresponding Raman and IR images.

Synthesis, Characterization, and Antibacterial Activity of Cross-Linked Chitosan-Glutaraldehyde

PubMed Central

Li, Bin; Shan, Chang-Lin; Zhou, Qing; Fang, Yuan; Wang, Yang-Li; Xu, Fei; Han, Li-Rong; Ibrahim, Muhammad; Guo, Long-Biao; Xie, Guan-Lin; Sun, Guo-Chang

2013-01-01

This present study deals with synthesis, characterization and antibacterial activity of cross-linked chitosan-glutaraldehyde. Results from this study indicated that cross-linked chitosan-glutaraldehyde markedly inhibited the growth of antibiotic-resistant Burkholderia cepacia complex regardless of bacterial species and incubation time while bacterial growth was unaffected by solid chitosan. Furthermore, high temperature treated cross-linked chitosan-glutaraldehyde showed strong antibacterial activity against the selected strain 0901 although the inhibitory effects varied with different temperatures. In addition, physical-chemical and structural characterization revealed that the cross-linking of chitosan with glutaraldehyde resulted in a rougher surface morphology, a characteristic Fourier transform infrared (FTIR) band at 1559 cm−1, a specific X-ray diffraction peak centered at 2θ = 15°, a lower contents of carbon, hydrogen and nitrogen, and a higher stability of glucose units compared to chitosan based on scanning electron microscopic observation, FTIR spectra, X-ray diffraction pattern, as well as elemental and thermo gravimetric analysis. Overall, this study indicated that cross-linked chitosan-glutaraldehyde is promising to be developed as a new antibacterial drug. PMID:23670533

Thermal, structural, functional, optical and magnetic studies of pure and Ba doped CdO nanoparticles.

PubMed

Sivakumar, S; Venkatesan, A; Soundhirarajan, P; Khatiwada, Chandra Prasad

2015-12-05

In this research, a chemical precipitation method was used to synthesize undoped and doped cadmium oxide nanoparticles and studied by TG-DTA, XRD, FT-IR, SEM, with EDX and antibacterial activities, respectively. The melting points, thermal stability and the kinetic parameters like entropy (ΔS), enthalpy (ΔH), Gibb's energy (ΔG), activation energy (E), frequency factor (A) were evaluated from TG-DTA measurements. X-ray diffraction analysis (XRD) brought out the information about the synthesized products exist in spherical in shape with cubic structure. The functional groups and band area of the samples were established by Fourier transform infrared (FT-IR) spectroscopy. The direct and indirect band gap energy of pure and doped samples were determined by UV-Vis-DRS. The surface morphological, elemental compositions and particles sizes were evaluated by scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDS). Finally, antibacterial activities indicated the Gram-positive and Gram-negative bacteria are more active in transporter, dehydrogenize and periplasmic enzymatic activities of pure and doped samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Structural studies of a green-emitting terbium doped calcium zinc phosphate phosphor

NASA Astrophysics Data System (ADS)

Ramesh, B.; Dillip, G. R.; Rambabu, B.; Joo, S. W.; Raju, B. Deva Prasad

2018-03-01

In this study, a new green emitting CaZn2(PO4)2:Tb3+ phosphors were synthesized through solid-state reaction route. The phosphors were characterized structurally by X-ray diffraction, Fourier transform infrared spectroscopy (FTIR) and X-ray photoelectron spectroscopy (XPS). All the synthesized phosphors were crystallized in triclinic crystal structure with P 1 bar space group. The phosphate groups in the phosphors were confirmed by FTIR analysis. The surface elements O 1s, P 2p, Ca 2p, Zn 2p and Tb 3d were studied by high-resolution XPS spectra. Upon excitation at 378 nm, the dominant green emission of CaZn2(PO4)2:Tb3+ phosphors at 542 nm were noticed in the emission spectra. For various emission wavelengths (at 435 and 489 nm) and constant excitation wavelength (at 378 nm), the decay curves have shown two different decay dynamics of phosphors. The lighting properties such as Commission International de l'Eclairage (x = 0.319, y = 0.398) and color temperature (5995 K) were calculated.

Influence of Pyrolysis Temperature on Physico-Chemical Properties of Corn Stover (Zea mays L.) Biochar and Feasibility for Carbon Capture and Energy Balance.

PubMed

Rafiq, Muhammad Khalid; Bachmann, Robert Thomas; Rafiq, Muhammad Tariq; Shang, Zhanhuan; Joseph, Stephen; Long, Ruijun

2016-01-01

This study examined the influence of pyrolysis temperature on biochar characteristics and evaluated its suitability for carbon capture and energy production. Biochar was produced from corn stover using slow pyrolysis at 300, 400 and 500°C and 2 hrs holding time. The experimental biochars were characterized by elemental analysis, BET, FTIR, TGA/DTA, NMR (C-13). Higher heating value (HHV) of feedstock and biochars was measured using bomb calorimeter. Results show that carbon content of corn stover biochar increased from 45.5% to 64.5%, with increasing pyrolysis temperatures. A decrease in H:C and O:C ratios as well as volatile matter, coupled with increase in the concentration of aromatic carbon in the biochar as determined by FTIR and NMR (C-13) demonstrates a higher biochar carbon stability at 500°C. It was estimated that corn stover pyrolysed at 500°C could provide of 10.12 MJ/kg thermal energy. Pyrolysis is therefore a potential technology with its carbon-negative, energy positive and soil amendment benefits thus creating win- win scenario.

Impact of gamma radiation on the eruption rate of rat incisors

NASA Astrophysics Data System (ADS)

El-Faramawy, Nabil; El-Haddad, Khaled; Ali, Mohamed; Talaat, Mona

2015-09-01

The present work aims to test the effect of gamma radiation on the rate of eruption of rat incisors. One hundred and five adult male albino rats were used and irradiated at different gamma doses. The effects of irradiation were investigated by numerical measurements of eruption rate, histological investigation using light microscope and spectral analysis using Fourier Transform Infra-Red (FTIR). No detectable changes were observed in the groups with smaller radiation doses. There was a significant decrease in the eruption rate starting from the 4 Gy radiation dose. The observation of histological sections revealed disturbance in cellular elements responsible for eruption as well as periodontal disturbance in the samples irradiated with 4 and 6 Gy. FTIR Spectroscopy of control group and the group irradiated by 0.5 Gy showed similar absorption bands with minor differences. However, samples irradiated by 1 Gy showed significant changes in both molecular structure and conformation related to carbonates and hydroxyl groups. From the previous results, it could be concluded that gamma irradiation negatively affects the eruption rate of the rat incisors especially with higher doses.

Perennial grass (Arundo donax L.) as a feedstock for thermo-chemical conversion to energy and materials.

PubMed

Saikia, Ruprekha; Chutia, Rahul Singh; Kataki, Rupam; Pant, Kamal K

2015-01-01

In the present study, perennial grass species Arundo donax L. was pyrolysed in a fixed-bed reactor and characterization was performed for the liquid and the solid products. The effect of process parameters such as temperature (350-650 °C), heating rate (10 °C and 40 °C min(-1)) and sweeping gas flow rate (50-250 ml min(-1)) was also investigated. Maximum bio-oil yield of ∼ 26% was observed at 500 °C for the heating rate of 40 °C min(-1). Chemical composition of the bio-oil was analysed through NMR, FTIR and GC-MS. The biochar was characterized by Scanning Electron Microscopy (SEM), Fourier Transform Infrared (FTIR) spectroscopy along with elemental analysis (CHN). The biochar produced as a co-product of A. donax pyrolysis can be a potential soil amendment with multiple benefits including increased soil fertility and C-sequestration. Current investigation suggests suitability of A. donax as a potential feedstock for exploitation of energy and biomaterials through pyrolytic route. Copyright © 2015 Elsevier Ltd. All rights reserved.

Synchrotron-based ν-XRF mapping and μ-FTIR microscopy enable to look into the fate and effects of tattoo pigments in human skin.

PubMed

Schreiver, Ines; Hesse, Bernhard; Seim, Christian; Castillo-Michel, Hiram; Villanova, Julie; Laux, Peter; Dreiack, Nadine; Penning, Randolf; Tucoulou, Remi; Cotte, Marine; Luch, Andreas

2017-09-12

The increasing prevalence of tattoos provoked safety concerns with respect to particle distribution and effects inside the human body. We used skin and lymphatic tissues from human corpses to address local biokinetics by means of synchrotron X-ray fluorescence (XRF) techniques at both the micro (μ) and nano (ν) scale. Additional advanced mass spectrometry-based methodology enabled to demonstrate simultaneous transport of organic pigments, heavy metals and titanium dioxide from skin to regional lymph nodes. Among these compounds, organic pigments displayed the broadest size range with smallest species preferentially reaching the lymph nodes. Using synchrotron μ-FTIR analysis we were also able to detect ultrastructural changes of the tissue adjacent to tattoo particles through altered amide I α-helix to β-sheet protein ratios and elevated lipid contents. Altogether we report strong evidence for both migration and long-term deposition of toxic elements and tattoo pigments as well as for conformational alterations of biomolecules that likely contribute to cutaneous inflammation and other adversities upon tattooing.

Carbohydrate and lipid spectroscopic molecular structures of different alfalfa hay and their relationship with nutrient availability in ruminants

PubMed Central

Yari, Mojtaba; Valizadeh, Reza; Nnaserian, Abbas Ali; Jonker, Arjan; Yu, Peiqiang

2017-01-01

Objective This study was conducted to determine molecular structures related to carbohydrates and lipid in alfalfa hay cut at early bud, late bud and early flower and in the afternoon and next morning using Fourier transform infrared spectroscopy (FT/IR) and to determine their relationship with alfalfa hay nutrient profile and availability in ruminants. Methods Chemical composition analysis, carbohydrate fractionation, in situ ruminal degradability, and DVE/OEB model were used to measure nutrient profile and availability of alfalfa hay. Univariate analysis, hierarchical cluster analysis (CLA) and principal components analysis (PCA) were conducted to identify FT/IR spectra differences. Results The FT/IR non-structural carbohydrate (NSCHO) to total carbohydrates and NSCHO to structural carbohydrate ratios decreased (p<0.05), while lignin to NSCHO and lipid CH3 symmetric to CH2 symmetric ratios increased with advancing maturity (p<0.05). The FT/IR spectra related to structural carbohydrates, lignin and lipids were distinguished for alfalfa hay at three maturities by PCA and CLA, while FT/IR molecular structures related to carbohydrates and lipids were similar between alfalfa hay cut in the morning and afternoon when analyzed by PCA and CLA analysis. Positive correlations were found for FT/IR NSCHO to total carbohydrate and NSCHO to structural carbohydrate ratios with non-fiber carbohydrate (by wet chemistry), ruminal fast and intermediately degradable carbohydrate fractions and total ruminal degradability of carbohydrates and predicted intestinal nutrient availability in dairy cows (r≥0.60; p<0.05) whereas FT/IR lignin to NSCHO and CH3 to CH2 symmetric stretching ratio had negative correlation with predicted ruminal and intestinal nutrient availability of alfalfa hay in dairy cows (r≥−0.60; p<0.05). Conclusion FT/IR carbohydrate and lipid molecular structures in alfalfa hay changed with advancing maturity from early bud to early flower, but not during the day, and these molecular structures correlated with predicted nutrient supply of alfalfa hay in ruminants. PMID:28335093

Synthesis of gadolinium carbonate-conjugated-poly(ethylene)glycol (Gd{sub 2}(CO{sub 3}){sub 3}@PEG) particles via a modified solvothermal method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nasution, Erika L. Y.; Ahab, Atika; Nuryadin, Bebeh W.

2016-02-08

PEGylated gadolinium carbonate ((Gd{sub 2}(CO{sub 3}){sub 3})@PEG) powder was successfully synthesized by a modified solvothermal method. The synthesized products were characterized by means of X-ray diffraction (XRD), Fourier Transform Infrared spectroscopy (FTIR), Scanning Electron Microscopy (SEM), and Energy Dispersive X-ray Spectroscopy (EDS). A systematic change in the chemical surface composition, crystallinity and size properties of the Gd{sub 2}(CO{sub 3}){sub 3}@PEG particles was observed by increasing the reaction time at 5 hours, 7 hours, and 8 hours. The corresponding XRD patterns showed that the Gd{sub 2}(CO{sub 3}){sub 3} particles had hexagonal symmetry (JCPDS No. 37-0559) with a crystallite size of 3.5,more » 2.9, and 4.6 nm. FTIR spectra showed that the Gd{sub 2}(CO{sub 3}){sub 3})@PEG particles were formed with the PEG as carbonyl and hydroxyl group attached to the surface. SEM analysis showed that the Gd{sub 2}(CO{sub 3}){sub 3})@PEG particles had a flake-like morphology of homogeneous sized particles and agglomerates. EDS analysis confirmed the presence of constituent Gd{sub 2}(CO{sub 3}){sub 3} elements.« less

FTIR Analysis of Functional Groups in Aerosol Particles

NASA Astrophysics Data System (ADS)

Shokri, S. M.; McKenzie, G.; Dransfield, T. J.

2012-12-01

Secondary organic aerosols (SOA) are suspensions of particulate matter composed of compounds formed from chemical reactions of organic species in the atmosphere. Atmospheric particulate matter can have impacts on climate, the environment and human health. Standardized techniques to analyze the characteristics and composition of complex secondary organic aerosols are necessary to further investigate the formation of SOA and provide a better understanding of the reaction pathways of organic species in the atmosphere. While Aerosol Mass Spectrometry (AMS) can provide detailed information about the elemental composition of a sample, it reveals little about the chemical moieties which make up the particles. This work probes aerosol particles deposited on Teflon filters using FTIR, based on the protocols of Russell, et al. (Journal of Geophysical Research - Atmospheres, 114, 2009) and the spectral fitting algorithm of Takahama, et al (submitted, 2012). To validate the necessary calibration curves for the analysis of complex samples, primary aerosols of key compounds (e.g., citric acid, ammonium sulfate, sodium benzoate) were generated, and the accumulated masses of the aerosol samples were related to their IR absorption intensity. These validated calibration curves were then used to classify and quantify functional groups in SOA samples generated in chamber studies by MIT's Kroll group. The fitting algorithm currently quantifies the following functionalities: alcohols, alkanes, alkenes, amines, aromatics, carbonyls and carboxylic acids.

The green synthesis of fine particles of gold using an aqueous extract of Monotheca buxifolia (Flac.)

NASA Astrophysics Data System (ADS)

Anwar, Natasha; Khan, Abbas; Shah, Mohib; Azam, Andaleeb; Zaman, Khair; Parven, Zahida

2016-12-01

This study deals with the synthesis and physicochemical investigation of gold nanoparticles using an aqueous extract of Monotheca buxifolia (Flac.). On the treatment of aqueous solution of tetrachloroauric acid with the plant extract, gold nanoparticles were rapidly fabricated. The synthesized particles were characterized by UV-Vis spectrophotometry (UV), Fourier transform infrared spectroscopy (FTIR), energy dispersive X-ray (EDX) and Scanning electron microscopy (SEM). The formation of AuNPs was confirmed by noting the change in color through visual observations as well as via UV-Vis spectroscopy. UV‒Vis spectrum of the aqueous medium containing gold nanoparticles showed an absorption peak at around 540 nm. FTIR was used to identify the chemical composition of gold nanoparticles and Au-capped plant extract. The presence of elemental gold was also confirmed through EDX analysis. SEM analysis of the gold nanoparticles showed that they have a uniform spherical shape with an average size in the range of 70-78 nm. This green system showed to be better capping and stabilizing agent for the fine particles. Further, the antioxidant activity of Monotheca buxifolia (Flac.) extract and Au-capped with the plant extract was also evaluated using FeCl3/K3[Fe(CN)]6 in vitro assay.

RIBAVIRIN: The analysis of a polymorphic substance by LC-MS and FTIR spectroscopy

NASA Astrophysics Data System (ADS)

Machal, A. C.; Flurer, R. A.; Brueggemeyer, T. W.; Ellis, L. E.; Satzger, R. D.; Stewart, K. R.

1998-06-01

The FTIR laboratory often has the task of identifying unknown pharmaceuticals. This case involves unknown capsules received at the Forensic Chemistry Center. Through extensive searching of pharmaceutical data bases, it was concluded that the capsules might contain ribavirin, which is classified as an anti-viral agent. Mass spectral analysis (LC-MS) concluded that the capsules contained ribavirin; however, the FTIR results did not agree with the mass spectral results. Additional experiments were performed and the results demonstrate the capabilities of FTIR to discern differences between polymorphic forms of a substance, such as ribavirin, when other techniques are unable to provide this information.

Characterization of Organosolv Lignins using Thermal and FT-IR Spectroscopic Analysis

Treesearch

Rhea J. Sammons; David P. Harper; Nicole Labbe; Joseph J. Bozell; Thomas Elder; Timothy G. Rials

2013-01-01

A group of biomass-derived lignins isolated using organosolv fractionation was characterized by FT-IR spectral and thermal property analysis coupled with multivariate analysis. The principal component analysis indicated that there were significant variations between the hardwood, softwood, and grass lignins due to the differences in syringyl and guaiacyl units as well...

FTIR characterization of Mexican honey and its adulteration with sugar syrups by using chemometric methods

NASA Astrophysics Data System (ADS)

Rios-Corripio, M. A.; Rios-Leal, E.; Rojas-López, M.; Delgado-Macuil, R.

2011-01-01

A chemometric analysis of adulteration of Mexican honey by sugar syrups such as corn syrup and cane sugar syrup was realized. Fourier transform infrared spectroscopy (FTIR) was used to measure the absorption of a group of bee honey samples from central region of Mexico. Principal component analysis (PCA) was used to process FTIR spectra to determine the adulteration of bee honey. In addition to that, the content of individual sugars from honey samples: glucose, fructose, sucrose and monosaccharides was determined by using PLS-FTIR analysis validated by HPLC measurements. This analytical methodology which is based in infrared spectroscopy and chemometry can be an alternative technique to characterize and also to determine the purity and authenticity of nutritional products as bee honey and other natural products.

Synthesis and characterization of Ni(II) complex with 5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradeca-7,14-dienium bromide

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yusoff, Latifah M.; Yusoff, Siti Fairus M.; Ismail, Wafiuddin

Nickel(II) complex have been synthesized by treating a 14-membered ring tetraaza macrocyclic compound, 5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradeca-7,14-dienium, bromide (Me{sub 6}N{sub 4}H{sub 4})Br{sub 2} with nickel acetate in metanol. The complex was characterized using elemental analysis, Fourier Transform Infrared (FTIR), Ultraviolet-Visible (UV-Vis), and single crystal diffraction (X-ray). The nickel atom coordinates through four nitrogen atoms in the ligand. Square planar geometry has been proposed for this complex.

Highly soluble 3,4-(dimethoxyphenylthio) substituted phthalocyanines: Synthesis, photophysical and photochemical studies

NASA Astrophysics Data System (ADS)

Öztürk, Cansu; Erdoğmuş, Ali; Durmuş, Mahmut; Uğur, Ahmet Lütfi; Kılıçarslan, Fatma Aytan; Erden, İbrahim

2012-02-01

The synthesis of a new 3,4-(dimethoxyphenylthio) substituted phthalonitrile ( 1) and its soluble metal free ( 2), zinc (II) ( 3), oxo-titanium (IV) ( 4) and nickel (II) ( 5) phthalocyanine derivatives are reported for the first time. The new compounds have been characterized by elemental analysis, FT-IR, 1H NMR, UV-Vis, fluorescence spectroscopies and mass spectra. General trends are described for fluorescence, photodegradation and singlet oxygen quantum yields and fluorescence lifetimes of oxo-titanium (IV) and zinc (II) phthalocyanine compounds in dimethylsulfoxide (DMSO). The effects of the metal ion on the photophysical and photochemical parameters for these phthalocyanines ( 3 and 4) are also reported.

Synthesis, biological activity and dyeing performance of some novel azo disperse dyes incorporating pyrazolo[1,5-a]pyrimidines for dyeing of polyester fabrics

NASA Astrophysics Data System (ADS)

Sayed, Ahmed Z.; Aboul-Fetouh, Mahmoud S.; Nassar, Hesham S.

2012-02-01

Several novel pyrazolopyrimidine azo compounds were achieved from diazotization of 4-aminoacetanilide and coupling with malononitrile and then refluxed with hydrazine hydrate to furnish 3,5-diamino-4-(4-acetamidophenylazo)-1H-pyrazole. The later compound was diazotized and coupled with substituted α-cyanocinnamate, α-cyanocinnamonitrile, 2-cyano-3-ethoxyacrylic acid ethyl ester, chalcones and ethylacetoacetate to produce novel dyestuffs. Structures of the dyes were fully characterized by using FT-IR, 1H NMR, mass spectroscopy and elemental analysis. The dyes were applied to polyester fiber, affording satisfactory results and showed biological activity towards various microorganisms.

Synthesis, spectroscopic, thermal and structural properties of [M(3-aminopyridine)2Ni(μ-CN)2(CN)2]n (M(II) = Co and Cu) heteropolynuclear cyano-bridged complexes

NASA Astrophysics Data System (ADS)

Kartal, Zeki

2016-01-01

Two novel cyano-bridged heteropolynuclear complexes, [Co(3-aminopyridine)2Ni(μ-CN)2(CN)2]n and [Cu(3-aminopyridine)2Ni(μ-CN)2(CN)2]n have been synthesized and characterized by elemental, thermal, FT-IR and FT-Raman spectroscopies. The structures of complexes have been determined by X-ray powder diffraction. The FT-IR and FT-Raman spectra of complexes have been recorded in the region of 3500-400 cm-1 and 3500-100 cm-1, respectively. General information was acquired about structural properties of these complexes from FT-IR and FT-Raman spectra by considering changes at characteristic peaks of the cyano group and 3AP. The splitting of the ν(Ctbnd N) stretching bands in the FT-IR spectra for complexes indicates the presence of terminal and bridging cyanides. The thermal behaviors of these complexes have been also investigated in the range of 25-950 °C using TG and DTG methods. Magnetic susceptibility measurements were made at room temperature using Gouy-balance.

[FTIR and 13C NMR Analysis of Dissolved Organic Matter (DOM) in the Treatment Process of Tannery Wastewater].

PubMed

Fan, Chun-hui; Zhang, Ying-chao; Tang, Ze-heng; Wang, Jia-hong

2015-05-01

Nowadays, the wastewater quantity discharged yearly from tannery industry is around 0. 2 billion t in China. The contaminants of tannery wastewater include macromolecular organic matters, such as grease, fur scraps and collagen, and the alkaline wastewater appears to be of high content of salt and COD. The quality of tannery wastewater is monitored strictly among all kinds of industry wastewater. In the treatment process of tannery wastewater, the quality of inlet and outlet water is generally analyzed. In fact, the transformation behavior of contaminants should be additionally checked to optimize the treatment conditions. Dissolved organic matter (DOM) is commonly existed in water-bodies and helpful to understand the physicochemical characteristics, while the related work should be further studied on tannery wastewater. The approaches of elemental analysis, thermal gravimetric analysis (TG), Fourier infrared spectroscopy (FTIR) and 13C nuclear magnetic resonance (13C NMR) were used to reveal the characteristics of DOM in the treatment process of tannery wastewater. The results showed the carbon content of DOM samples increased gradually, atomic ratios of H/C increased firstly and then decreased, indicating the organic matters were decomposed into chain structures firstly, finally forming the component hard to degraded. The pyrolysis process of DOM mainly proceeded in the regions of 110~530 °C (aliphatic compound, protein, etc. ) and 530~800 °C (aromatic ring, single bond of C-C, etc. ). The functional groups of DOM included -OH, -NH2, C=O and so on, and the aromatic substances were detected, shown from FTIR figures, in the later period of the reaction, caused by the metabolism effect of micro-organism. The content of alkoxy-C increased to the maximum in the second biochemical pond, and the minimum content of aromatic-C appeared in the second biochemical pond, suggesting the transformation behavior of carbon functional groups. The investigation on DOM in tannery wastewater is significant to understand the purification mechanism of contaminants in tannery wastewater.

Pretreatment and integrated analysis of spectral data reveal seaweed similarities based on chemical diversity.

PubMed

Wei, Feifei; Ito, Kengo; Sakata, Kenji; Date, Yasuhiro; Kikuchi, Jun

2015-03-03

Extracting useful information from high dimensionality and large data sets is a major challenge for data-driven approaches. The present study was aimed at developing novel integrated analytical strategies for comprehensively characterizing seaweed similarities based on chemical diversity. The chemical compositions of 107 seaweed and 2 seagrass samples were analyzed using multiple techniques, including Fourier transform infrared (FT-IR) and solid- and solution-state nuclear magnetic resonance (NMR) spectroscopy, thermogravimetry-differential thermal analysis (TG-DTA), inductively coupled plasma-optical emission spectrometry (ICP-OES), CHNS/O total elemental analysis, and isotope ratio mass spectrometry (IR-MS). The spectral data were preprocessed using non-negative matrix factorization (NMF) and NMF combined with multivariate curve resolution-alternating least-squares (MCR-ALS) methods in order to separate individual component information from the overlapping and/or broad spectral peaks. Integrated analysis of the preprocessed chemical data demonstrated distinct discrimination of differential seaweed species. Further network analysis revealed a close correlation between the heavy metal elements and characteristic components of brown algae, such as cellulose, alginic acid, and sulfated mucopolysaccharides, providing a componential basis for its metal-sorbing potential. These results suggest that this integrated analytical strategy is useful for extracting and identifying the chemical characteristics of diverse seaweeds based on large chemical data sets, particularly complicated overlapping spectral data.

Tunable microwave absorbing nano-material for X-band applications

NASA Astrophysics Data System (ADS)

Sadiq, Imran; Naseem, Shahzad; Ashiq, Muhammad Naeem; Khan, M. A.; Niaz, Shanawer; Rana, M. U.

2016-03-01

The effect of rare earth elements substitution in Sr1.96RE0.04Co2Fe27.80Mn0.2O46 (RE=Ce, Gd, Nd, La and Sm) X-type hexagonal ferrites prepared by using sol gel autocombustion method was studied. The XRD and FTIR analysis show the single phase of the prepared material. The lattice constants a (Å) and c (Å) varies with the additives. The particle size measured by Scherer formula for all the samples varies in the range of 54-100 nm and confirmed by the TEM analysis. The average grain size measured by SEM analysis lies in the range of 0.672-1.01 μm for all the samples. The Gd-substituted ferrite has higher value of coercivity (526.06 G) among all the samples which could be a good material for longitudinal recording media. The results also indicate that the Gd-substituted sample has maximum reflection loss of -25.2 dB at 11.878 GHz, can exhibit the best microwave absorption properties among all the substituted samples. Furthermore, the minimum value of reflection loss shifts towards the lower and higher frequencies with the substitution of rare earth elements which confirms that the microwave absorption properties can be tuned with the substitution of rare earth elements in pure ferrites. The peak value of attenuation constant at higher frequency agrees well the reflection loss data.

Investigation of cell wall composition related to stem lodging resistance in wheat (Triticum aestivum L.) by FTIR spectroscopy.

PubMed

Wang, Jian; Zhu, Jinmao; Huang, RuZhu; Yang, YuSheng

2012-07-01

We explored the rapid qualitative analysis of wheat cultivars with good lodging resistances by Fourier transform infrared resonance (FTIR) spectroscopy and multivariate statistical analysis. FTIR imaging showing that wheat stem cell walls were mainly composed of cellulose, pectin, protein, and lignin. Principal components analysis (PCA) was used to eliminate multicollinearity among multiple peak absorptions. PCA revealed the developmental internodes of wheat stems could be distributed from low to high along the load of the second principal component, which was consistent with the corresponding bands of cellulose in the FTIR spectra of the cell walls. Furthermore, four distinct stem populations could also be identified by spectral features related to their corresponding mechanical properties via PCA and cluster analysis. Histochemical staining of four types of wheat stems with various abilities to resist lodging revealed that cellulose contributed more than lignin to the ability to resist lodging. These results strongly suggested that the main cell wall component responsible for these differences was cellulose. Therefore, the combination of multivariate analysis and FTIR could rapidly screen wheat cultivars with good lodging resistance. Furthermore, the application of these methods to a much wider range of cultivars of unknown mechanical properties promises to be of interest.

[Revisiting the chemical diversity in prostatic calculi: a SEM and FT-IR investigation].

PubMed

Dessombz, A; Méria, P; Bazin, D; Foy, E; Rouzière, S; Weil, R; Daudon, M

2011-12-01

Revisiting the chemical diversity of the crystalline phases of prostatic calculi by means of SEM and FT-IR analysis. A set of 32 prostatic calculi has been studied by FT-IR and SEM. FT-IR analysis has determined the chemical composition of each prostatic calculus and the SEM observation has described the morphology of the calculi surfaces and layers. Infrared analysis revealed that 90.7% of the stones were mainly composed of calcium phosphates. However, several mineral phases previously not reported in prostatic calculi were observed, as brushite or octocalcium phosphate pentahydrate. Prostatic calculi exhibited a diversity of crystalline composition and morphology. As previously reported for urinary calculi, relationships between composition and morphology of prostatic stones and étiopathogenic conditions could be of interest in clinical practice. Copyright © 2011 Elsevier Masson SAS. All rights reserved.

Synthesis and characterization of ZnO–CuO nanocomposites powder by modified perfume spray pyrolysis method and its antimicrobial investigation

NASA Astrophysics Data System (ADS)

Saravanakkumar, D.; Sivaranjani, S.; Kaviyarasu, K.; Ayeshamariam, A.; Ravikumar, B.; Pandiarajan, S.; Veeralakshmi, C.; Jayachandran, M.; Maaza, M.

2018-03-01

Pure ZnO, ZnO–CuO nanocomposites can be synthesized by using a modified perfume spray pyrolysis method (MSP). The crystallite size of the nanoparticles (NPs) has been observed by X-ray diffraction pattern and is nearly 36 nm. Morphological studies have been analyzed by using Field Emission Scanning Electron Microscopy (FESEM) and its elemental analysis was reported by Elemental X-ray Analysis (EDX); these studies confirmed that ZnO and CuO have hexagonal structure and monoclinic structure respectively. Fourier Transform Infrared (FTIR) spectra revealed that the presence of functional frequencies of ZnO and CuO were observed at 443 and 616 cm‑1. The average bandgap value at 3.25 eV using UV–vis spectra for the entitled composite has described a blue shift that has been observed here. The antibacterial study against both gram positive and negative bacteria has been studied by the disc diffusion method. To the best of our knowledge, it is the first report on ZnO–CuO nanocomposite synthesized by a modified perfume spray pyrolysis method.

Chondroitin sulfate template-mediated biomimetic synthesis of nano-flake hydroxyapatite

NASA Astrophysics Data System (ADS)

He, Dan; Xiao, Xiufeng; Liu, Fang; Liu, Rongfang

2008-11-01

By Ca(NO 3) 2·4H 2O and (NH 4) 3PO 4·3H 2O as reagents and chondroitin sulfate (ChS) as a template, nano-flake hydroxyapatite (HA) is synthesized using a biomimetic method according to the biomineralization theory. HA crystals obtained are characterized in crystalline phase, microstructure, chemical composition and morphology by X-ray diffraction (XRD), Fourier transform infrared spectroscope (FTIR), transmission electron microscopy (TEM) and elemental analysis respectively. UV-vis spectrum is adopted to investigate interactions between functional groups ChS and HA. The results show that HA crystal nucleation and growth take place in chemical interactions between HA crystals and ChS as a template. And elemental analysis indicates that obtained HA contains a small amount of ChS. Furthermore, ChS concentration significantly affects the morphology of HA crystals. Staple-fiber-like HA crystals can be obtained at a low concentration in ChS, and flake-like HA crystals synthesized at a high concentration (≥0.5 wt.%) of ChS as a template.

Characterization and Activation of Indonesian Natural Zeolite from Southwest Aceh District-Aceh Province

NASA Astrophysics Data System (ADS)

Yulianis, Y.; Muhammad, S.; Pontas, K.; Mariana, M.; Mahidin, M.

2018-05-01

This study aims to identify the effect of activation processes of Indonesian zeolite from Southwest Aceh District, Aceh Province on the physical characteristics and chemical contents changes. The work was conducted by downsizing of natural zeolite into nano particle size, treating it physically (heated up to 105˚C) and chemically (soaked with 0.5 M HCl for 1 hour), and finally calcining it at the temperature of 350° C for 2 hours. The natural and activated nano zeolites were then characterized by using SEM, BET, XRD, XRF and FTIR in order to examine their characters and chemical contents. The characterization results showed that the activated nano zeolite has better appearances than the natural one. The XRD analysis showed that the main minerals of zeolite are quartz and calcite clinochlore. Further, the XRF analysis showed that there are elements of magnesium, calcium and potassium which can be as a cation exchange with other metal elements. Based on the identified properties, this zeolite showed a good performance to be used as an adsorbent in waste water treatment process, especially after activated.

Assessing the extent, stability, purity and properties of silanised detonation nanodiamond

NASA Astrophysics Data System (ADS)

Duffy, Emer; Mitev, Dimitar P.; Thickett, Stuart C.; Townsend, Ashley T.; Paull, Brett; Nesterenko, Pavel N.

2015-12-01

The functionalisation of nanodiamond is a key step in furthering its application in areas such as surface coatings, drug delivery, bio imaging and other biomedical avenues. Accordingly, analytical methods for the detailed characterisation of functionalised nano-material are of great importance. This work presents an alternative approach for the elemental analysis of zero-dimensional nanocarbons, specifically detonation nanodiamond (DND) following purification and functionalisation procedures. There is a particular emphasis on the presence of silicon, both for the purified DND and after its functionalisation with silanes. Five different silylation procedures for purified DND were explored and assessed quantitatively using inductively coupled plasma-mass spectrometry (ICP-MS) for analysis of dilute suspensions. A maximum Si loading of 29,300 μg g-1 on the DND was achieved through a combination of silylating reagents. The presence of 28 other elements in the DND materials was also quantified by ICP-MS. The characterisation of Si-bond formation was supported by FTIR and XPS evaluation of relevant functional groups. The thermal stability of the silylated DND was examined by thermogravimetric analysis. Improved particle size distribution and dispersion stability resulted from the silylation procedure, as confirmed by dynamic light scattering and capillary zone electrophoresis.

Dicoumarol complexes of Cu(II) based on 1,10-phenanthroline: Synthesis, X-ray diffraction studies, thermal behavior and biological evaluation

NASA Astrophysics Data System (ADS)

Dholariya, Hitesh R.; Patel, Ketan S.; Patel, Jiten C.; Patel, Kanuprasad D.

2013-05-01

A series of Cu(II) complexes containing dicoumarol derivatives and 1, 10-phenanthroline have been synthesized. Structural and spectroscopic properties of ligands were studied on the basis of mass spectra, NMR (1H and 13C) spectra, FT-IR spectrophotometry and elemental analysis, while physico-chemical, spectroscopic and thermal properties of mixed ligand complexes have been studied on the basis of infrared spectra, mass spectra, electronic spectra, powder X-ray diffraction, elemental analysis and thermogravimetric analysis. X-ray diffraction study suggested the suitable octahedral geometry for hexa-coordinated state. The kinetic parameters such as order of reaction (n), energy of activation (Ea), entropy (S*), pre-exponential factor (A), enthalpy (H*) and Gibbs free energy (G*) have been calculated using Freeman-Carroll method. Ferric-reducing antioxidant power (FRAP) of all complexes were measured. All the compounds were screened for their antibacterial activity against Escherichia coli, Pseudomonas aeruginosa, Streptococcus pyogenes and Bacillus subtilis, while antifungal activity against Candida albicans and Aspergillus niger have been carried out. Also compounds against Mycobacterium tuberculosis shows clear enhancement in the anti-tubercular activity upon copper complexation.

Spectroscopic and structural properties of 2,2'-dipyridylamine and its palladium and platinum complexes

NASA Astrophysics Data System (ADS)

Yurdakul, Ş.; Bilkana, M. T.

2015-10-01

The structural features such as geometric parameters, vibration frequencies and intensities of the vibrational bands of 2,2'-dipyridylamine ligand (DPA), its palladium (Pd(DPA)Cl2) and platinum (Pt(DPA)Cl2) complexes were studied by the density functional theory (DFT). The calculations were carried out by DFT / B3LYP method with 6-311++G(d,p) and LANL2DZ basis sets. All vibrational frequencies assigned in detail with the help of total energy distribution analysis (TED). Optimized geometric bond lengths and bond angles were compared with experimental X-ray data. Using DPA, K2PtCl4, and Na2PdCl4, the synthesized complex structures were characterized by the combination of elemental analysis, FT-IR (mid and far IR) and Raman spectroscopy.

Group 12 dithiocarbamate complexes: synthesis, spectral studies and their use as precursors for metal sulfides nanoparticles and nanocomposites.

PubMed

Ajibade, Peter A; Ejelonu, Benjamin C

2013-09-01

Zn(II), Cd(II) and Hg(II) dithiocarbamate complexes have been synthesized and characterized by elemental analysis, thermogravimetric analysis, UV-Vis, FTIR, (1)H- and (13)C NMR spectroscopy. The complexes were thermolysed at 180 °C and used as single molecule precursors for the synthesis of HDA capped ZnS, CdS and HgS nanoparticles and polymethylmethacrylate (PMMA) nanocomposites. The optical and structural properties of the nanoparticles and nanocomposites were studied by UV-Vis, PL, XRD and SEM. The crystallites sizes of the nanoparticles varied between 3.03 and 23.45 nm. SEM and EDX analyses of the nanocomposites confirmed the presence of the nanoparticles in the polymer matrix. Copyright © 2013 Elsevier B.V. All rights reserved.

Studies on novel radiopaque methyl methacrylate: glycidyl methacrylate based polymer for biomedical applications.

PubMed

Dawlee, S; Jayakrishnan, A; Jayabalan, M

2009-12-01

A new class of radiopaque copolymer using methyl methacrylate (MMA) and glycidyl methacrylate (GMA) monomers was synthesized and characterized. The copolymer was made radiopaque by the epoxide ring opening of GMA using the catalyst o-phenylenediamine and the subsequent covalent attachment of elemental iodine. The copolymer was characterized by Fourier transform infrared (FTIR) spectra, energy dispersive X-ray analysis using environmental scanning electron microscope (EDAX), thermogravimetric analysis (TGA), and differential scanning calorimetry (DSC). X-ray visibility of the copolymer was checked by X-radiography. Blood compatibility and cytotoxicity of the newly synthesized copolymer were also evaluated. The iodinated copolymer was thermally stable, blood compatible, non-cytotoxic, and highly radiopaque. The presence of bulky iodine group created a new copolymer with modified properties for potential use in biomedical applications.

Combining FT-IR spectroscopy and multivariate analysis for qualitative and quantitative analysis of the cell wall composition changes during apples development.

PubMed

Szymanska-Chargot, M; Chylinska, M; Kruk, B; Zdunek, A

2015-01-22

The aim of this work was to quantitatively and qualitatively determine the composition of the cell wall material from apples during development by means of Fourier transform infrared (FT-IR) spectroscopy. The FT-IR region of 1500-800 cm(-1), containing characteristic bands for galacturonic acid, hemicellulose and cellulose, was examined using principal component analysis (PCA), k-means clustering and partial least squares (PLS). The samples were differentiated by development stage and cultivar using PCA and k-means clustering. PLS calibration models for galacturonic acid, hemicellulose and cellulose content from FT-IR spectra were developed and validated with the reference data. PLS models were tested using the root-mean-square errors of cross-validation for contents of galacturonic acid, hemicellulose and cellulose which was 8.30 mg/g, 4.08% and 1.74%, respectively. It was proven that FT-IR spectroscopy combined with chemometric methods has potential for fast and reliable determination of the main constituents of fruit cell walls. Copyright © 2014 Elsevier Ltd. All rights reserved.

Semi-quantitative analysis of FT-IR spectra of humic fractions of nine US soils

USDA-ARS?s Scientific Manuscript database

Fourier Transform Infrared Spectroscopy (FT-IR) is a simple and fast tool for characterizing soil organic matter. However, most FT-IR spectra are only analyzed qualitatively. In this work, we prepared mobile humic acid (MHA) and recalcitrant calcium humate (CaHA) from nine soils collected from six ...

A chemometric method for correcting FTIR spectra of biomaterials for interference from water in KBr discs

USDA-ARS?s Scientific Manuscript database

FTIR analysis of solid biomaterials by the familiar KBr disc technique is very often frustrated by water interference in the important protein (amide I) and carbohydrate (hydroxyl) regions of their spectra. A method was therefore devised that overcomes the difficulty and measures FTIR spectra of so...

Tracking the conversion of nitrogen during pyrolysis of antibiotic mycelial fermentation residues using XPS and TG-FTIR-MS technology.

PubMed

Zhu, Xiangdong; Yang, Shijun; Wang, Liang; Liu, Yuchen; Qian, Feng; Yao, Wenqing; Zhang, Shicheng; Chen, Jianmin

2016-04-01

Antibiotic mycelial fermentation residues (AMFRs), which are emerging solid pollutants, have been recognized as hazardous waste in China since 2008. Nitrogen (N), which is an environmental sensitivity element, is largely retained in AMFR samples derived from fermentation substrates. Pyrolysis is a promising technology for the treatment of solid waste. However, the outcomes of N element during the pyrolysis of AMFRs are still unknown. In this study, the conversion of N element during the pyrolysis of AMFRs was tracked using XPS (X-ray photoelectron spectroscopy) and online TG-FTIR-MS (Thermogravimetry-Fourier transform infrared-Mass spectrometry) technology. In the AMFR sample, organic amine-N, pyrrolic-N, protein-N, pyridinic-N, was the main N-containing species. XPS results indicated that pyrrolic-N and pyridinic-N were retained in the AMFR-derived pyrolysis char. More stable species, such as N-oxide and quaternary-N, were also produced in the char. TG-FTIR-MS results indicated that NH3 and HCN were the main gaseous species, and their contents were closely related to the contents of amine-N and protein-N, and pyrrolic-N and pyridinic-N of AMFRs, respectively. Increases in heating rate enhanced the amounts of NH3 and HCN, but had less of an effect on the degradation degree of AMFRs. N-containing organic compounds, including amine-N, nitrile-N and heterocyclic-N, were discerned from the AMFR pyrolysis process. Their release range was extended with increasing of heating rate and carbon content of AMFR sample. This work will help to take appropriate measure to reduce secondary pollution from the treatment of AMFRs. Copyright © 2015 Elsevier Ltd. All rights reserved.

Near-field photothermal microspectroscopy for adult stem-cell identification and characterization.

PubMed

Grude, Olaug; Hammiche, Azzedine; Pollock, Hubert; Bentley, Adam J; Walsh, Michael J; Martin, Francis L; Fullwood, Nigel J

2007-12-01

The identification of stem cells in adult tissue is a challenging problem in biomedicine. Currently, stem cells are identified by individual epitopes, which are generally tissue specific. The discovery of a stem-cell marker common to other adult tissue types could open avenues in the development of therapeutic stem-cell strategies. We report the use of the novel technique of Fourier transform infrared near-field photothermal microspectroscopy (FTIR-PTMS) for the characterization of stem cells, transit amplifying (TA) cells and terminally differentiated (TD) cells in the corneal epithelium. Principal component analysis (PCA) data demonstrate excellent discrimination of cell type by spectra. PCA in combination with linear discriminant analysis (PCA-LDA) shows that FTIR-PTMS very effectively discriminates between the three cell populations. Statistically significant differences above the 99% confidence level between IR spectra from stem cells and TA cells suggest that nucleic acid conformational changes are an important component of the differences between spectral data from the two cell types. FTIR-PTMS is a new addition to existing spectroscopy methods based on the concept of interfacing a conventional FTIR spectrometer with an atomic force microscope equipped with a near-field thermal sensing probe. FTIR-PTMS spectroscopy currently has spatial resolution that is similar to that of diffraction-limited optical detection FTIR spectroscopy techniques, but as a near-field probing technique has considerable potential for further improvement. Our work also suggests that FTIR-PTMS is potentially more sensitive than synchrotron radiation FTIR spectroscopy for some applications. Microspectroscopy techniques like FTIR-PTMS provide information about the entire molecular composition of cells, in contrast to epitope recognition that only considers the presence or absence of individual molecules. Our results with FTIR-PTMS on corneal stem cells are promising for the potential development of an IR spectral fingerprint for stem cells.

The synthesis and the spectroscopic, thermal, and structural properties of the M2[(fumarate)Ni(CN)4]·2(1,4-Dioxane) clathrate (M = Co, Ni, Cd and Hg)

NASA Astrophysics Data System (ADS)

Kartal, Zeki; Yavuz, Abdülkerim

2018-03-01

In this study, the clathrates of fumarate-tetracyanonickel-dioxane, given by the formula M2[(fumarate)Ni(CN)4]·2(1,4-Dioxane) (M = Co, Ni, Cd and Hg), have been obtained for the first time through chemical methods. These clathrates have been characterized by elemental, thermal, FT-IR, and FT-Raman spectroscopies. The parameters of structures of clathrates have been determined by X-ray powder diffraction. The thermal behaviors of these clathrates have been also investigated by thermo-gravimetric analysis (TGA), differential thermal analysis (DTA), and derivative thermal gravimetric analysis (DTG) in the range of 20-900 °C. X-ray powder diffraction data have been recorded at ambient temperature in the 2θ range 5-50°. The FT-IR and FT-Raman spectra of clathrates have been recorded in the region of 4000-400 cm-1 and 4000-100 cm-1, respectively. The results of the spectral and thermal analyses of the newly synthesized clathrates of fumarate-tetracyanonickel-dioxane suggest that these clathrates are new examples of the Hofmann-type dioxane clathrates. In our study, the Hofmann-type dioxane clathrates, which are formed by bounding electrons of oxygen-donor atoms of fumarate ion ligand molecule to transition metal atoms, consist of the corrugated |M-Ni(CN)4|∞ polymeric layers, which are held in parallel through the chain of (-M-fumarate-M-).

Spectroscopic studies of gel grown zinc doped calcium hydrogen phosphate dihydrate crystals

NASA Astrophysics Data System (ADS)

Suryawanshi, V. B.; Chaudhari, R. T.

2018-05-01

The influence of zinc doping on the gel grown calcium hydrogen phosphate dihydrate crystals was studied using the spectroscopic techniques, which included SEM, FTIR and EDAX. It was found that, zinc ions transform the morphology of brushite crystals from rectangular plate shaped crystals to branching microcrystal patterns. However in FT-IR spectroscopy, as compared to undoped brushite crystals few vibrations were shifted to higher value. The observed changes in the vibrations were due to the impact of zinc ions. EDAX techniques is use to determine the percentage composition of elements present in the doped crystals. It revealed that the sample was of a mixed composition.

Non-covalent interactions in 2-methylimidazolium copper(II) complex (MeImH)2[Cu(pfbz)4]: Synthesis, characterization, single crystal X-ray structure and packing analysis

NASA Astrophysics Data System (ADS)

Sharma, Raj Pal; Saini, Anju; Kumar, Santosh; Kumar, Jitendra; Sathishkumar, Ranganathan; Venugopalan, Paloth

2017-01-01

A new anionic copper(II) complex, (MeImH)2 [Cu(pfbz)4] (1) where, MeImH = 2-methylimidazolium and pfbz = pentafluorobenzoate has been isolated by reacting copper(II) sulfate pentahydrate, pentafluorobenzoic acid and 2-methylimidazole in ethanol: water mixture in 1:2:2 molar ratio. This complex 1 has been characterized by elemental analysis, thermogravimetric analysis, spectroscopic techniques (UV-Vis, FT-IR) and conductance measurements. The complex salt crystallizes in monoclinic crystal system with space group C2/c. Single crystal X-ray structure determination revealed the presence of discrete ions: [Cu(pfbz)4]2- anion and two 2-methylimidazolium cation (C4H7N2)+. The crystal lattice is stabilized by strong hydrogen bonding and F⋯F interactions between cationic-anionic and the anionic-anionic moieties respectively, besides π-π interactions.

Characterization of potassium bromide crystals grown in the aqueous solution of picric acid

NASA Astrophysics Data System (ADS)

Maheswari, J. Uma; Krishnan, C.; Kalyanaraman, S.; Selvarajan, P.

2016-12-01

Potassium bromide crystals were grown in the aqueous solution of picric acid by slow evaporation technique at room temperature. X-ray Diffraction (XRD) analysis ensures that the grown sample is in Fm3m space group and FCC structure. Energy Dispersive X-ray Spectroscopy (EDX) reveals the presence of elements in the title compound. UV-Vis-NIR spectrum reveals that the grown sample is a promising nonlinear optical (NLO) material. FTIR analysis confirms the functional groups present in the sample. The thermogravimetric (TG) and differential thermogravimetric (DTA) analyses ensure that the sample material is thermally stable up to 160 °C. The second harmonic efficiency of the sample is 1.3 times greater than that of standard KDP. The mechanical strength of the grown sample is estimated by Vickers microhardness tester. The electrical properties were investigated by impedance analysis and the results of various studies of the grown crystals are discussed.

Analysis of Moisture Content in Beetroot using Fourier Transform Infrared Spectroscopy and by Principal Component Analysis.

PubMed

Nesakumar, Noel; Baskar, Chanthini; Kesavan, Srinivasan; Rayappan, John Bosco Balaguru; Alwarappan, Subbiah

2018-05-22

The moisture content of beetroot varies during long-term cold storage. In this work, we propose a strategy to identify the moisture content and age of beetroot using principal component analysis coupled Fourier transform infrared spectroscopy (FTIR). Frequent FTIR measurements were recorded directly from the beetroot sample surface over a period of 34 days for analysing its moisture content employing attenuated total reflectance in the spectral ranges of 2614-4000 and 1465-1853 cm -1 with a spectral resolution of 8 cm -1 . In order to estimate the transmittance peak height (T p ) and area under the transmittance curve [Formula: see text] over the spectral ranges of 2614-4000 and 1465-1853 cm -1 , Gaussian curve fitting algorithm was performed on FTIR data. Principal component and nonlinear regression analyses were utilized for FTIR data analysis. Score plot over the ranges of 2614-4000 and 1465-1853 cm -1 allowed beetroot quality discrimination. Beetroot quality predictive models were developed by employing biphasic dose response function. Validation experiment results confirmed that the accuracy of the beetroot quality predictive model reached 97.5%. This research work proves that FTIR spectroscopy in combination with principal component analysis and beetroot quality predictive models could serve as an effective tool for discriminating moisture content in fresh, half and completely spoiled stages of beetroot samples and for providing status alerts.

Synthesis, structural, thermal and optical studies of 1-ethyl-2,6-dimethyl-4-hydroxy pyridinium halides.

PubMed

Dhanuskodi, S; Manivannan, S; Kirschbaum, K

2006-05-15

1-Ethyl-2,6-dimethyl-4-hydroxy pyridinium chloride dihydrate and bromide dihydrate salts have been synthesized and their single crystals were grown by the slow evaporation of aqueous solution at 30 degrees C. The grown crystals were characterized by elemental analysis, FT-NMR and FT-IR techniques to confirm the formation of the expected compound. Optical transmittance window in aqueous solution was found to be 275-1100 nm by UV-vis-NIR technique. Thermogravimetric and differential thermal analyses reveal thermal stability and the presence of two water molecules in the crystal lattices. The crystal structure of chloride salt was also determined by X-ray diffraction method.

Laser modification of graphene oxide layers

NASA Astrophysics Data System (ADS)

Malinský, Petr; Macková, Anna; Cutroneo, Mariapompea; Siegel, Jakub; Bohačová, Marie; Klímova, Kateřina; Švorčík, Václav; Sofer, Zdenĕk

2018-01-01

The effect of linearly polarized laser irradiation with various energy densities was successfully used for reduction of graphene oxide (GO). The ion beam analytical methods (RBS, ERDA) were used to follow the elemental composition which is expected as the consequence of GO reduction. The chemical composition analysis was accompanied by structural study showing changed functionalities in the irradiated GO foils using spectroscopy techniques including XPS, FTIR and Raman spectroscopy. The AFM was employed to identify the surface morphology and electric properties evolution were subsequently studied using standard two point method measurement. The used analytical methods report on reduction of irradiated graphene oxide on the surface and the decrease of surface resistivity as a growing function of the laser beam energy density.

Manufacturing of novel low-cost adsorbent: Co-granulation of limestone and coffee waste.

PubMed

Iakovleva, Evgenia; Sillanpää, Mika; Maydannik, Philipp; Liu, Jiang Tao; Allen, Stephen; Albadarin, Ahmad B; Mangwandi, Chirangano

2017-12-01

Limestone and coffee waste were used during the wet co-granulation process for the production of efficient adsorbents to be used in the removal of anionic and cationic dyes. The adsorbents were characterized using different analytical techniques such as XRD, SEM, FTIR, organic elemental analysis, the nitrogen adsorption method, with wettability, strength and adsorption tests. The adsorption capacity of granules was determined by removal of methylene blue (MB) and orange II (OR) from single and mixed solutions. In the mixed solution, co-granules removed 100% of MB and 85% of OR. The equilibria were established after 6 and 480 h for MB and OR, respectively. Copyright © 2017 Elsevier Ltd. All rights reserved.

Synthesis, Spectral investigation (¹H, ¹³C) and Anti-microbial Screening of benzophenone imines.

PubMed

Khosa, Muhammad Kaleem; Jamal, Muhammad Asghar; Saif, Muhammad Jawad; Muneer, Majid; Rehman, Fazalur; Farman, Muhammad; Shoaib, Hafiz Muhammad; Shahid, Muhammad; Hameed, Shabnam

2015-11-01

New series of benzophenone imines with general formula Ph2-C=NR; R = Benzyl, 4-Fluorobenzyl, Naphthyl, Phenyl, 4-Nitrophenyl were synthesized by condensation of dichlorodiphenylmethane and different aromatic primary amines (1:1) Those imines were characterized by different physiochemical and spectroscopic techniques like melting point, elemental analysis, FT-IR, multinuclear NMR (¹H, ¹³C). After characterization, imines were subjected to anti-microbial activities. All compounds showed promising activity against different bacterial strains like Escherichia coli, Bacillussubtilis, Pasturellam ultocida and Staphylococcus aureus as well as fungal strains like Alternata alternaria, Ganoderma lucidium, Penicillium notatum and Trichoderma harzianum using Amoxicillin and Flucanazole as a standard drugs respectively.

Synthesis, characterization, spectroscopic studies and antimicrobial activity of three new Schiff bases derived from Heterocyclic moiety

NASA Astrophysics Data System (ADS)

Mesbah, Mounira; Douadi, Tahar; Sahli, Farida; Issaadi, Saifi; Boukazoula, Soraya; Chafaa, Salah

2018-01-01

Three new Schiff-bases compounds (I-III) were synthesized by a condensation reaction in 1:2 M ratios of 4,4‧-diaminodiphenyl sulfide and pyrrol/thiophene/furan-2-carboxaldehyde in ethanol. The structural determinations of the Schiff-bases were identified with the help of elemental analysis then confirmed by UV-Vis, FT-IR and 1H NMR. The products were obtained in excellent yields. On the other hand, the in vitro antibacterial and antifungal activities of the synthesized compounds were investigated using disc diffusion method. Schiff bases synthesized individually exhibited varying degrees of inhibitory effects on the growth of the tested microbial species.

Extraction and physicochemical characterization of chitin and chitosan from Zophobas morio larvae in varying sodium hydroxide concentration.

PubMed

Soon, Chu Yong; Tee, Yee Bond; Tan, Choon Hui; Rosnita, Abdul Talib; Khalina, Abdan

2018-03-01

Large amount of sodium hydroxide (NaOH) is consumed to remove the protein content in chitin biomass during deproteinization. However, excessive NaOH concentration used might lead to the reduction of cost effectiveness during chitin extraction. Hence, the present study aimed to extract and evaluate the physicochemical properties of chitin and chitosan isolated from superworm (Zophobas morio) larvae using 0.5M-2.0M of NaOH. The extracted chitin and chitosan were subjected to Fourier Transform Infrared Spectroscopy (FT-IR), elemental analysis, Scanning Electron Microscope (SEM), Thermogravimetric Analysis (TGA), Differential Scanning Calorimetry (DSC) and X-ray Diffraction (XRD). The 0.5M NaOH treatment resulted in the highest yield of chitin (5.43%), but produced the lowest yield (65.84%) of chitosan. The extracted chitin samples had relatively high degree of acetylation (DA) (82.39%-101.39%). Both chitin and chitosan showed smooth surface with tiny pores. The extracted chitin samples were confirmed as α-chitin based on the FT-IR and TGA. The chitin samples were amorphous with low degree of crystallinity. From TGA, the Chitosan 3 extracted was partially deacetylated. Both DPPH radical scavenging and ferric-chelating assay showed positive correlation with DD of chitosan isolates. However, the chitosan isolates were not fully dissolved, resulting in lower radical scavenging and ferric-chelating ability compared to commercial chitosan. Copyright © 2017. Published by Elsevier B.V.

Isolation and characterization of lignin from the oak wood bioethanol production residue for adhesives.

PubMed

Lee, Soo Jung; Kim, Hyun Joo; Cho, Eun Jin; Song, Younho; Bae, Hyeun-Jong

2015-01-01

Lignin was isolated from the residue of bioethanol production with oak wood via alkaline and catalyzed organosolv treatments at ambient temperature to improve the purity of lignin for the materials application. The isolated lignins were analyzed for their chemical composition by nitrobenzene oxidation method and their functionality was characterized via wet chemistry method, element analysis, (1)H NMR, GPC and FTIR-ATR. The isolated lignin by acid catalyzed organosolv treatment (Acid-OSL) contained a higher lignin content, aromatic proton, phenolic hydroxyl group and a lower nitrogen content that is more reactive towards chemical modification. The lignin-based adhesives were prepared and the bond strength was measured to evaluate the enhanced reactivity of lignin by the isolation. Two steps of phenolation and methylolation were applied for the modification of the isolated lignins and their tensile strengths were evaluated for the use as an adhesive. The acid catalyzed organosolv lignin-based adhesives had comparable bond strength to phenol-formaldehyde adhesives. The analysis of lignin-based adhesives by FTIR-ATR and TGA showed structural similarity to phenol adhesive. The results demonstrate that the reactivity of lignin was enhanced by isolation from hardwood bioethanol production residues at ambient temperature and it could be used in a value-added application to produce lignin-based adhesives. Copyright © 2014 Elsevier B.V. All rights reserved.

The Use of ATR-FTIR in Conjunction with Thermal Analysis Methods for Efficient Identification of Polymer Samples: A Qualitative Multiinstrument Instrumental Analysis Laboratory Experiment

ERIC Educational Resources Information Center

Dickson-Karn, Nicole M.

2017-01-01

A multi-instrument approach has been applied to the efficient identification of polymers in an upper-division undergraduate instrumental analysis laboratory course. Attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR) is used in conjunction with differential scanning calorimetry (DSC) to identify 18 polymer samples and…

Histopathology mapping of biochemical changes in myocardial infarction by Fourier transform infrared spectral imaging.

PubMed

Yang, Tian T; Weng, Shi F; Zheng, Na; Pan, Qing H; Cao, Hong L; Liu, Liang; Zhang, Hai D; Mu, Da W

2011-04-15

Fourier transform infrared (FTIR) imaging and microspectroscopy have been extensively applied in the identification and investigation of both healthy and diseased tissues. FTIR imaging can be used to determine the biodistribution of several molecules of interest (carbohydrates, lipids, proteins) for tissue analysis, without the need for prior staining of these tissues. Molecular structure data, such as protein secondary structure and collagen triple helix exhibits, can also be obtained from the same analysis. Thus, several histopathological lesions, for example myocardial infarction, can be identified from FTIR-analyzed tissue images, the latter which can allow for more accurate discrimination between healthy tissues and pathological lesions. Accordingly, we propose FTIR imaging as a new tool integrating both molecular and histopathological assessment to investigate the degree of pathological changes in tissues. In this study, myocardial infarction is presented as an illustrative example of the wide potential of FTIR imaging for biomedical applications. Copyright © 2010 Elsevier Ireland Ltd. All rights reserved.

Anti-inflammatory drugs interacting with Zn (II) metal ion based on thiocyanate and azide ligands: synthesis, spectroscopic studies, DFT calculations and antibacterial assays.

PubMed

Chiniforoshan, Hossein; Tabrizi, Leila; Hadizade, Morteza; Sabzalian, Mohammad R; Chermahini, Alireza Najafi; Rezapour, Mehdi

2014-07-15

Zinc (II) complexes with non-steroidal anti-inflammatory drugs (NSAIDs) naproxen (nap) and ibuprofen (ibu) were synthesized in the presence of nitrogen donor ligands (thiocyanate or azide). The complexes were characterized by elemental analysis, FT-IR, (1)H NMR and UV-Vis spectroscopes. The binding modes of the ligands in complexes were established by means of molecular modeling of the complexes, and calculation of their IR, NMR and absorption spectra at DFT (TDDFT)/B3LYP level were studied. The experimental and calculated data verified monodentate binding through the carboxylic oxygen atoms of anti-inflammatory drugs in the zinc complexes. The calculated (1)H, FT-IR and UV-Vis data are in better agreement with the experimental results, and confirm the predicted tetrahedral structures for the Zn (II) complexes. In addition to DFT calculations of complexes, natural bond orbital (NBO) was performed at B3LYP/6-31+G(d,p) level of theory. Biological studies showed the antibacterial activity of zinc complexes against Gram-positive and Gram-negative bacterial strains. Copyright © 2014 Elsevier B.V. All rights reserved.

Controlling of free radical copolymerization of styrene and maleic anhydride via RAFT process for the preparation of acetaminophen drug conjugates

NASA Astrophysics Data System (ADS)

Sütekin, S. Duygu; Atıcı, Ayşe Bakar; Güven, Olgun; Hoffman, Allan S.

2018-07-01

The presence of maleic anhydride moiety in styrene-maleic anhydride (SMA) copolymer makes it a versatile substrate for conjugation of drugs. In this study biocompatible styrene-maleic anhydride (SMA) copolymer with alternating structure was synthesized by gamma irradiation at room temperature in the presence of 2-phenyl-2-propyl benzodithioate (PPB). The poly(styrene-alt-maleic anhydride) (poly(St-alt-MA)) with narrow molecular weight distribution (Đ: 1.1-1.3) was prepared by reversible addition-fragmentation chain transfer (RAFT) polymerization. The synthesized poly(St-alt-MA) structure was characterized by ATR-FTIR spectroscopy, elemental analysis and 1H NMR spectroscopy and molecular weight and dispersity were determined by size exclusion chromatography (SEC). SMA copolymers were further conjugated with acetaminophen via ester linkage and FT-IR, 1H NMR investigation indicated that the acetaminophen was attached to poly(St-alt-MA). Drug release profile of the polymer-drug conjugate was followed by high performance liquid chromatography (HPLC). The drug-conjugate system was found to follow first order release kinetics with Hixson-Crowell model while drug release mechanism was found as non-Fickian diffusion after testing various kinetic models.

Star-shaped azomethines based on tris(2-aminoethyl)amine. Characterization, thermal and optical study.

PubMed

Iwan, Agnieszka; Janeczek, Henryk; Kaczmarczyk, Bozena; Jarzabek, Bozena; Sobota, Michal; Rannou, Patrice

2010-02-01

The synthesis and detailed (physico)-chemical ((1)H/(13)C NMR, FTIR, UV-vis and elemental analysis) characterizations of new star-shaped compounds based on tris(2-aminoethyl)amine, including in their structure an azomethine function (HCN-) and alkoxysemiperfluorinated (-O-(CH(2))(3)-(CF(2))(7)-CF(3)), octadecyloxy aliphatic (-O-(CH(2))(17)-CH(3)) chain or two phenyl rings (-Ph-Ph-) as a terminal group, were reported. The mesomorphic behavior was investigated by means of differential scanning calorimetry (DSC), polarized optical microscopy (POM) and additionally by FTIR(T) and UV-vis(T) spectroscopy. Wide-angle X-ray diffraction (WAXD) technique was used to probe the structural properties of the azomethines. Moreover, the azomethine A1 was electro-spun to prepare fibers with poly(methyl methacrylate) (PMMA) and investigated by DSC and POM. Additionally, a film of the A1 with PMMA was cast from chloroform and the thermal properties of the film were compared with the thermal properties of the fiber and powder. It was showed that terminal groups dramatically influence the thermal and optical properties of the star-shaped azomethines. Copyright (c) 2009 Elsevier B.V. All rights reserved.

Structural characterization and chemical classification of some bryophytes found in Latvia.

PubMed

Maksimova, Viktorija; Klavina, Laura; Bikovens, Oskars; Zicmanis, Andris; Purmalis, Oskars

2013-07-01

Bryophytes are the second largest taxonomic group in the plant kingdom; yet, studies conducted to better understand their chemical composition are rare. The aim of this study was to characterize the chemical composition of bryophytes common in Northern Europe by using elemental, spectral, and non-destructive analytical methods, such as Fourier transform IR spectrometry (FT-IR), solid-phase (13) C-NMR spectrometry, and pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS), for the purpose of investigating their chemotaxonomic relationships on the basis of chemical-composition data. The results of all these analyses showed that bryophytes consist mainly of carbohydrates. Judging by FT-IR spectra, the OH groups in combination of CO groups were the most abundant groups. The (13) C-NMR spectra provided information on the presence of such compounds as phenolics and lipids. It was found that the amount of phenolic compounds in bryophytes is relatively small. This finding definitely confirmed the absence of lignin in the studied bryophytes. Cluster analysis was used to better understand differences in the chemical composition of bryophyte samples and to evaluate possible usage of these methods in the chemotaxonomy of bryophytes. Copyright © 2013 Verlag Helvetica Chimica Acta AG, Zürich.

Influence of Pyrolysis Temperature on Physico-Chemical Properties of Corn Stover (Zea mays L.) Biochar and Feasibility for Carbon Capture and Energy Balance

PubMed Central

Rafiq, Muhammad Khalid; Bachmann, Robert Thomas; Rafiq, Muhammad Tariq; Shang, Zhanhuan; Joseph, Stephen; Long, Ruijun

2016-01-01

This study examined the influence of pyrolysis temperature on biochar characteristics and evaluated its suitability for carbon capture and energy production. Biochar was produced from corn stover using slow pyrolysis at 300, 400 and 500°C and 2 hrs holding time. The experimental biochars were characterized by elemental analysis, BET, FTIR, TGA/DTA, NMR (C-13). Higher heating value (HHV) of feedstock and biochars was measured using bomb calorimeter. Results show that carbon content of corn stover biochar increased from 45.5% to 64.5%, with increasing pyrolysis temperatures. A decrease in H:C and O:C ratios as well as volatile matter, coupled with increase in the concentration of aromatic carbon in the biochar as determined by FTIR and NMR (C-13) demonstrates a higher biochar carbon stability at 500°C. It was estimated that corn stover pyrolysed at 500°C could provide of 10.12 MJ/kg thermal energy. Pyrolysis is therefore a potential technology with its carbon-negative, energy positive and soil amendment benefits thus creating win- win scenario. PMID:27327870

Synthesis, characterization and visible-light driven photocatalysis by differently structured CdS/ZnS sandwich and core-shell nanocomposites

NASA Astrophysics Data System (ADS)

Qutub, Nida; Pirzada, Bilal Masood; Umar, Khalid; Mehraj, Owais; Muneer, M.; Sabir, Suhail

2015-11-01

CdS/ZnS sandwich and core-shell nanocomposites were synthesized by a simple and modified Chemical Precipitation method under ambient conditions. The synthesized composites were characterized by XRD, SEM, TEM, EDAX and FTIR. Optical properties were analyzed by UV-vis. Spectroscopy and the photoluminescence study was done to monitor the recombination of photo-generated charge-carriers. Thermal stability of the synthesized composites was analyzed by Thermal Gravimetric Analysis (TGA). XRD revealed the formation of nanocomposites as mixed diffraction peaks were observed in the XRD pattern. SEM and TEM showed the morphology of the nanocomposites particles and their fine particle size. EDAX revealed the appropriate molar ratios exhibited by the constituent elements in the composites and FTIR gave some characteristic peaks which indicated the formation of CdS/ZnS nanocomposites. Electrochemical Impedance Spectroscopy was done to study charge transfer properties along the nanocomposites. Photocatalytic properties of the synthesized composites were monitored by the photocatalytic kinetic study of Acid Blue dye and p-chlorophenol under visible light irradiation. Results revealed the formation of stable core-shell nanocomposites and their efficient photocatalytic properties.

Preparation and spectroscopic characterization of two HoCl 3-galactitol complexes and one ErCl 3-galactitol complex

NASA Astrophysics Data System (ADS)

Hua, Xiaohui; Pan, Qinghua; Yu, Lei; Xue, Junhui; Yang, Limin; Xu, Yizhuang; Zhao, Guozhong; Li, Weihong; Wang, Zheming; Wu, Jinguang; Liu, Kexin; Chen, Jia'er

2011-07-01

The interactions between metal ions and hydroxyl groups of carbohydrates are important for their possible biological activities. Here two HoCl 3-galactitol complexes ([Ho(galac)(H 2O) 3)]Cl 3·0.5galac) (HoG(I)) and ([Ho 2(galac)(H 2O) 12)]Cl 6·2H 2O) (HoG(II))) and one ErCl 3-galactitol complex ([Er(galac)(H 2O) 3)]Cl 3·0.5galac)(ErG)) were prepared and characterized. The possible structures of HoG(I) and ErG were deduced from FTIR, elemental analysis, ESI-MS, FIR, THz and TGA results. It is suggested that Ho 3+ or Er 3+ is 9-coordinated with six hydroxyl groups from two galactitol molecules and three water molecules, and another galactitol molecule is hydrogen-bonded in HoG(I) and ErG and the ratio of metal to ligand is 1:1.5. The structure of HoG(II) was determined by FTIR and X-ray diffraction analyses. The results demonstrate that lanthanide ions with galactitol may form two compounds in a system and different topological structures can be obtained.

Installation of a reactive site for covalent wiring onto an intrinsically conductive poly(ionic liquid)

DOE PAGES

Brombosz, Scott M.; Lee, Sungwon; Firestone, Millicent A.

2014-11-04

We describe post-polymerization radical bromination of a nanostructured poly(ionic liquid) that selectively introduces a reactive bromo-group onto the polyalkylthiophene backbone. Raman and FT-IR spectroscopy proves that the bromine is successfully introduced at the 3-methyl position of the thiophene and that the molecular structure of the polymer remains largely intact with only minimal chain scission detected. FT-IR and Vis-NIR spectroscopy indicates that incorporation of the bromine induces twisting (loss of co-planarity) of the polythiophene backbone. WAXS confirms retention of an ordered lamellar structure with minor lattice spacing contraction. Cyclic voltammetry confirms spectroscopic findings that the bromination reaction yields a stable p-dopedmore » polymer. The installed bromine is susceptible to nucleophilic displacement permitting the covalent attachment of other functional molecules, such as a dialkylphosphonate. Elemental analysis of such a transformation established that 100 % functionalization can be achieved. These results collectively demonstrate that post-modification of a π-conjugated polymer can be used to both tune electronic and photonic properties, as well as install a chemoselective attachment point for the covalent wiring of other molecules.« less

Synthesis, characterization and antimicrobial activity of dextran sulphate stabilized silver nanoparticles

NASA Astrophysics Data System (ADS)

Cakić, Milorad; Glišić, Slobodan; Nikolić, Goran; Nikolić, Goran M.; Cakić, Katarina; Cvetinov, Miroslav

2016-04-01

Dextran sulphate stabilized silver nanoparticles (AgNPs - DS) were synthesized from aqueous solution of silver nitrate (AgNO3) and dextran sulphate sodium salt (DS). The characterization of AgNPs - DS was performed by ultraviolet-visible spectroscopy (UV-VIS), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and antimicrobial activity. The formation of AgNPs - DS was monitored by colour changes of the reaction mixture from yellowish to brown and by measuring the surface plasmon resonance absorption peak in UV-VIS spectra at 420 nm. The SEM analysis was used for size and shape determination of AgNPs - DS. The presence of elemental silver and its crystalline structure in AgNPs - DS were confirmed by EDX and XRD analyses. The possible functional groups of DS responsible for the reduction and stabilization of AgNPs were determinated by FTIR spectroscopy. The AgNPs - DS showed strong antibacterial activity against Staphylococcus aureus ATCC 25923, Bacillus cereus ATCC 11778, Bacillus luteus in haus strain, Bacillus subtilis ATTC 6633, Listeria monocytogenes ATCC 15313, Escherichia coli ATTC 25922, Pseudomonas aeruginosa ATTC 27853, Klebsiella pneumoniae ATTC 700603, Proteus vulgaris ATTC 8427, and antifungal activity against Candida albicans ATTC 2091.

Off-line real-time FTIR analysis of a process step in imipenem production

NASA Astrophysics Data System (ADS)

Boaz, Jhansi R.; Thomas, Scott M.; Meyerhoffer, Steven M.; Staskiewicz, Steven J.; Lynch, Joseph E.; Egan, Richard S.; Ellison, Dean K.

1992-08-01

We have developed an FT-IR method, using a Spectra-Tech Monit-IR 400 systems, to monitor off-line the completion of a reaction in real-time. The reaction is moisture-sensitive and analysis by more conventional methods (normal-phase HPLC) is difficult to reproduce. The FT-IR method is based on the shift of a diazo band when a conjugated beta-diketone is transformed into a silyl enol ether during the reaction. The reaction mixture is examined directly by IR and does not require sample workup. Data acquisition time is less than one minute. The method has been validated for specificity, precision and accuracy. The results obtained by the FT-IR method for known mixtures and in-process samples compare favorably with those from a normal-phase HPLC method.

Rietveld refinement and FTIR analysis of bulk ceramic Co3-xMnxO4 compositions

NASA Astrophysics Data System (ADS)

Meena, P. L.; Kumar, Ravi; Sreenivas, K.

2013-02-01

Co3-xMnxO4 (x = 0.0, 0.6, 1.2) prepared by solid state reaction method and characterized by powder X-ray diffraction (XRD) and Fourier transform infrared (FTIR). Lattice parameters (a), oxygen parameter (u), and ionic radii of cations have been determined through Rietveld analysis. Both a and u parameters are related to expansion of octahedral site as Mn content in Co3O4. Analysis of XRD data show that Mn (x ≤ 1.2) is accommodated at the octahedral site, while retaining the cubic spinel structure. FTIR results also confirm the same and signify strong interactions due to overlapping of Co and Mn octahedra.

Differentiation of aflatoxigenic and non-aflatoxigenic strains of Aspergilli by FT-IR spectroscopy.

PubMed

Atkinson, Curtis; Pechanova, Olga; Sparks, Darrell L; Brown, Ashli; Rodriguez, Jose M

2014-01-01

Fourier transform infrared spectroscopy (FT-IR) is a well-established and widely accepted methodology to identify and differentiate diverse microbial species. In this study, FT-IR was used to differentiate 20 strains of ubiquitous and agronomically important phytopathogens of Aspergillus flavus and Aspergillus parasiticus. By analyzing their spectral profiles via principal component and cluster analysis, differentiation was achieved between the aflatoxin-producing and nonproducing strains of both fungal species. This study thus indicates that FT-IR coupled to multivariate statistics can rapidly differentiate strains of Aspergilli based on their toxigenicity.

Synthesis, structure and magnetic property of a two-dimensional coordination polymer decorated with sine wave-like 1D double chain

NASA Astrophysics Data System (ADS)

Yao, Xiao-Qiang; Li, Dan-Yang; Xiao, Guo-Bin; Ma, Heng-Chang; Lei, Zi-Qiang; Liu, Jia-Cheng

2018-04-01

A new compound, {[Co(BPFI)(NDC)]H2O·0.5DMF}n (1) has been synthesized under hydrothermal condition by the self-assembly of V-shaped N-containing rigid ligand BPFI with Co(II) ions in the presence of H2NDC acid, where BPFI = 2,8-di(1H-imidazole-1-yl)dibenzo[b,d]furan, H2NDC = naphthalene-1,4-dicarboxylic acid. Compound 1 was characterized by elemental analysis, single crystal X-ray diffraction, FT-IR spectroscopy and UV-visible spectra. Structural analysis reveals that compound 1 is a unique dinuclear Co-based 2D (4,4) layer structure decorated with parallel double chains. In addition, magnetic study reveals the existence of antiferromagnetic coupling interactions between the Co(II) ions within the dinuclear unit of 1.

The effect of the distance between acidic site and basic site immobilized on mesoporous solid on the activity in catalyzing aldol condensation

NASA Astrophysics Data System (ADS)

Yu, Xiaofang; Yu, Xiaobo; Wu, Shujie; Liu, Bo; Liu, Heng; Guan, Jingqi; Kan, Qiubin

2011-02-01

Acid-base bifunctional heterogeneous catalysts containing carboxylic and amine groups, which were immobilized at defined distance from one another on the mesoporous solid were synthesized by immobilizing lysine onto carboxyl-SBA-15. The obtained materials were characterized by X-ray diffraction (XRD), N 2 adsorption, Fourier-transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), scanning electron micrographs (SEM), transmission electron micrographs (TEM), elemental analysis, and back titration. Proximal-C-A-SBA-15 with a proximal acid-base distance was more active than maximum-C-A-SBA-15 with a maximum acid-base distance in aldol condensation reaction between acetone and various aldehydes. It appears that the distance between acidic site and basic site immobilized on mesoporous solid should be an essential factor for catalysis optimization.

Lipase Immobilization on Silica Xerogel Treated with Protic Ionic Liquid and its Application in Biodiesel Production from Different Oils.

PubMed

Carvalho, Nayára B; Vidal, Bruna T; Barbosa, Anderson S; Pereira, Matheus M; Mattedi, Silvana; Freitas, Lisiane Dos S; Lima, Álvaro S; Soares, Cleide M F

2018-06-21

Treated silica xerogel with protic ionic liquid (PIL) and bifunctional agents (glutaraldehyde and epichlorohydrin) is a novel support strategy used in the effective immobilization of lipase from Burkholderia cepacia (LBC) by covalent binding. As biocatalysts with the highest activity recovery yields, LBC immobilized by covalent binding with epichlorohydrin without (203%) and with PIL (250%), was assessed by the following the hydrolysis reaction of olive oil and characterized biochemically (Michaelis⁻Menten constant, optimum pH and temperature, and operational stability). Further, the potential transesterification activity for three substrates: sunflower, soybean, and colza oils, was also determined, achieving a conversion of ethyl esters between 70 and 98%. The supports and the immobilized lipase systems were characterized using Fourier transform infrared spectra (FTIR), scanning electron microscopy (SEM), elemental analysis, and thermogravimetric (TG) analysis.

Physicochemical analysis of urinary stones from Dharmapuri district

NASA Astrophysics Data System (ADS)

Aslin Shamema, A.; Thanigai Arul, K.; Senthil Kumar, R.; Narayana Kalkura, S.

2015-01-01

Nephrolithiasis is a common disease caused by the multifactorial components such as geographical location, bacterial infection, low urine volume, and low intake of water. This disease induces severe metabolic abnormalities in the human body. As the prevalence of this disease was high in Dharmapuri district located in Tamil Nadu, urinary stones removed from the patients pertaining to this district were collected and to identify the toxic elements present in the stones. The presence of functional groups and phases of the stones were analyzed using X-ray diffraction (XRD), Fourier transform Raman spectroscopy and Fourier transform infrared spectroscopy (FT-IR). The majority of stones were found to be calcium oxalate monohydrate (COM) and mixed stones having minor existence of struvite and uric acid. Hexagonal shaped COM crystals, needle shaped uric acid crystals and layered arrangement of struvite crystals in the core region were revealed by Scanning Electron Microscopy (SEM). Thermo Gravimetric Analysis (TGA) was used to determine the thermal stability and the hardness of the stone which was measured using Vickers hardness (HV). The presence of toxic elements in stones such as zirconium and mercury was identified using Energy Dispersive X-ray Spectroscopy (EDS). The EDS analysis showed higher concentration of zirconium in the core region compared to the periphery. The percentage of zirconium was relatively high compared to other toxic elements in the stones. The Vickers hardness results indicated that high HV values in the core region than the periphery and this might be due to the presence of zirconium.

The Synthesis of Silicon Carbide in Rhombohedral Form with Different Chemicals

NASA Astrophysics Data System (ADS)

KARİPER, İ. AFŞIN

2017-06-01

This study describes the attempt at producing silicon carbide using a simpler and less costly method. Within the study, XRD, EDX, and FTIR analyses were performed to determine the structural properties of the product, and SEM analyses were used to identify its surface properties. The characteristics such as porosity and surface area were determined through BET analysis. The starting reagents were compared with the product using FTIR analysis, whereas the product was compared with a sample of SiC procured from a supplier who manufactures high-purity products through BET analysis. In EDX analysis, approximately 72 pct Si and 28 pct C were identified. The vibrational peaks of the synthesized product (characteristics Si-C bonds) were observed at around 1076 cm-1 (FTIR analysis). At the same time, the outcomes were compared with major publications in the literature.

Analysis of Resistant Starches in Rat Cecal Contents Using Fourier Transform Infrared Photoacoustic Spectroscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Anderson, Timothy J.; Ai, Yongfeng; Jones, Roger W.

Fourier transform infrared photoacoustic spectroscopy (FTIR-PAS) qualitatively and quantitatively measured resistant starch (RS) in rat cecal contents. Fisher 344 rats were fed diets of 55% (w/w, dry basis) starch for 8 weeks. Cecal contents were collected from sacrificed rats. A corn starch control was compared against three RS diets. The RS diets were high-amylose corn starch (HA7), HA7 chemically modified with octenyl succinic anhydride, and stearic-acid-complexed HA7 starch. To calibrate the FTIR-PAS analysis, samples from each diet were analyzed using an enzymatic assay. A partial least-squares cross-validation plot generated from the enzymatic assay and FTIR-PAS spectral results for starch fitmore » the ideal curve with a R2 of 0.997. A principal component analysis plot of components 1 and 2 showed that spectra from diets clustered significantly from each other. This study clearly showed that FTIR-PAS can accurately quantify starch content and identify the form of starch in complex matrices.« less

Classification of java tea (Orthosiphon aristatus) quality using FTIR spectroscopy and chemometrics

NASA Astrophysics Data System (ADS)

Heryanto, R.; Pradono, D. I.; Marlina, E.; Darusman, L. K.

2017-05-01

Java tea (Orthosiphon aristatus) is a plant that widely used as a medicinal herb in Indonesia. Its quality is varying depends on various factors, such as cultivating area, climate and harvesting time. This study aimed to investigate the effectiveness of FTIR spectroscopy coupled with chemometrics for discriminating the quality of java tea from different cultivating area. FTIR spectra of ethanolic extracts were collected from five different regions of origin of java tea. Prior to chemometrics evaluation, spectra were pre-processed by using baselining, normalization and derivatization. Principal Components Analysis (PCA) was used to reduce the spectra to two PCs, which explained 73% of the total variance. Score plot of two PCs showed groupings of the samples according to their regions of origin. Furthermore, Partial Least Squares-Discriminant Analysis (PLSDA) was applied to the pre-processed data. The approach produced an external validation success rate of 100%. This study shows that FTIR analysis and chemometrics has discriminatory power to classify java tea based on its quality related to the region of origin.

Enhanced detectability of fluorinated derivatives of N,N-dialkylamino alcohols and precursors of nitrogen mustards by gas chromatography coupled to Fourier transform infrared spectroscopy analysis for verification of chemical weapons convention.

PubMed

Garg, Prabhat; Purohit, Ajay; Tak, Vijay K; Dubey, D K

2009-11-06

N,N-Dialkylamino alcohols, N-methyldiethanolamine, N-ethyldiethanolamine and triethanolamine are the precursors of VX type nerve agents and three different nitrogen mustards respectively. Their detection and identification is of paramount importance for verification analysis of chemical weapons convention. GC-FTIR is used as complimentary technique to GC-MS analysis for identification of these analytes. One constraint of GC-FTIR, its low sensitivity, was overcome by converting the analytes to their fluorinated derivatives. Owing to high absorptivity in IR region, these derivatives facilitated their detection by GC-FTIR analysis. Derivatizing reagents having trimethylsilyl, trifluoroacyl and heptafluorobutyryl groups on imidazole moiety were screened. Derivatives formed there were analyzed by GC-FTIR quantitatively. Of these reagents studied, heptafluorobutyrylimidazole (HFBI) produced the greatest increase in sensitivity by GC-FTIR detection. 60-125 folds of sensitivity enhancement were observed for the analytes by HFBI derivatization. Absorbance due to various functional groups responsible for enhanced sensitivity were compared by determining their corresponding relative molar extinction coefficients ( [Formula: see text] ) considering uniform optical path length. The RSDs for intraday repeatability and interday reproducibility for various derivatives were 0.2-1.1% and 0.3-1.8%. Limit of detection (LOD) was achieved up to 10-15ng and applicability of the method was tested with unknown samples obtained in international proficiency tests.

Human papillomavirus detection using PCR and ATR-FTIR for cervical cancer screening

NASA Astrophysics Data System (ADS)

Rymsza, Taciana; Ribeiro, Eliane Aline; de Carvalho, Luis Felipe das Chagas e. Silva; Bhattacharjee, Tanmoy; de Azevedo Canevari, Renata

2018-05-01

The human papillomavirus (HPV) genital infection is considered one of the most common sexually transmitted diseases worldwide, and has been associated with cervical cancer. The objective of this study was to investigate the efficacy of the diagnostic methods: polymerase chain reaction (PCR) and Fourier transform infrared (FTIR) equipped with an ATR (Attenuated Total Reflectance) unit (Pike Tech) spectroscopy, to diagnose HPV infection in women undergoing gynecological examination. Seventeen patients (41.46%) of the 41 patients analyzed were diagnosed with exophytic/condyloma acuminate lesions by clinical analysis, 29 patients (70.7%) (G1 group) of the 41 patients, showed positive result for HPV cell injury by oncotic colpocitology and 12 patients (29.3%) (G2 group), presented negative result for cellular lesion and absence of clinical HPV lesion. Four samples were obtained per patient, which were submitted oncotic colpocitology analysis (Papanicolau staining, two samples), PCR (one sample) and ATR-FTIR analysis (one sample). L1 gene was amplified by PCR technique with specific GP5+/GP6+ and MY09/MY11 primers. PCR results were uniformly positive for presence of HPV in all analyzed samples. Multivariate analysis of ATR-FTIR spectra suggests no significant biochemical changes between groups and no clustering formed, concurring with results of PCR. This study suggests that PCR and ATR-FTIR are highly sensitive technique for HPV detection.

Human papillomavirus detection using PCR and ATR-FTIR for cervical cancer screening.

PubMed

Rymsza, Taciana; Ribeiro, Eliane Aline; de Carvalho, Luis Felipe das Chagas E Silva; Bhattacharjee, Tanmoy; de Azevedo Canevari, Renata

2018-05-05

The human papillomavirus (HPV) genital infection is considered one of the most common sexually transmitted diseases worldwide, and has been associated with cervical cancer. The objective of this study was to investigate the efficacy of the diagnostic methods: polymerase chain reaction (PCR) and Fourier transform infrared (FTIR) equipped with an ATR (Attenuated Total Reflectance) unit (Pike Tech) spectroscopy, to diagnose HPV infection in women undergoing gynecological examination. Seventeen patients (41.46%) of the 41 patients analyzed were diagnosed with exophytic/condyloma acuminate lesions by clinical analysis, 29 patients (70.7%) (G1 group) of the 41 patients, showed positive result for HPV cell injury by oncotic colpocitology and 12 patients (29.3%) (G2 group), presented negative result for cellular lesion and absence of clinical HPV lesion. Four samples were obtained per patient, which were submitted oncotic colpocitology analysis (Papanicolau staining, two samples), PCR (one sample) and ATR-FTIR analysis (one sample). L1 gene was amplified by PCR technique with specific GP5+/GP6+ and MY09/MY11 primers. PCR results were uniformly positive for presence of HPV in all analyzed samples. Multivariate analysis of ATR-FTIR spectra suggests no significant biochemical changes between groups and no clustering formed, concurring with results of PCR. This study suggests that PCR and ATR-FTIR are highly sensitive technique for HPV detection. Copyright © 2018 Elsevier B.V. All rights reserved.

FT-IR spectroscopy characterization of schwannoma: a case study

NASA Astrophysics Data System (ADS)

Ferreira, Isabelle; Neto, Lazaro P. M.; das Chagas, Maurilio José; Carvalho, Luís. Felipe C. S.; dos Santos, Laurita; Ribas, Marcelo; Loddi, Vinicius; Martin, Airton A.

2016-03-01

Schwannoma are rare benign neural neoplasia. The clinical diagnosis could be improved if novel optical techniques are performed. Among these techniques, FT-IR is one of the currently techniques which has been applied for samples discrimination using biochemical information with minimum sample preparation. In this work, we report a case of a schwannoma in the cervical region. A histological examination described a benign process. An immunohistochemically examination demonstrated positivity to anti-S100 protein antibody, indicating a diagnosis of schwannoma. The aim of this analysis was to characterize FT-IR spectrum of the neoplastic and normal tissue in the fingerprint (1000-1800 cm-1) and high wavenumber region (2800-3600 cm-1). The IR spectra were collect from tumor tissue and normal nerve samples by a FT-IR spectrophotometer (Spotlight Perkin Elmer 400, USA) with 64 scans, and resolution of 4 cm-1. A total of twenty spectra were recorded (10 from schwannoma and 10 from nerve). Multivariate Analysis was used to classify the data. Through average and standard deviation analysis we observed that the main spectral change occurs at ≍1600 cm-1 (amide I) and ≍1400 cm-1 (amide III) in the fingerprint region, and in CH2/CH3 protein-lipids and OH-water vibrations for the high wavenumber region. In conclusion, FT-IR could be used as a technique for schwannoma analysis helping to establish specific diagnostic.

Characterization of mannitol in Curvularia protuberata hyphae by FTIR and Raman spectromicroscopy.

PubMed

Isenor, Merrill; Kaminskyj, Susan G W; Rodriguez, Russell J; Redman, Regina S; Gough, Kathleen M

2010-12-01

FTIR and Raman spectromicroscopy were used to characterize the composition of Curvularia protuberata hyphae, and to compare a strain isolated from plants inhabiting geothermal soils with a non-geothermal isolate. Thermal IR source images of hyphae have been acquired with a 64 × 64 element focal plane array detector; single point IR spectra have been obtained with synchrotron source light. In some C. protuberata hyphae, we have discovered the spectral signature of crystalline mannitol, a fungal polyol with complex protective roles. With FTIR-FPA imaging, we have determined that the protein content in cells remains fairly constant throughout the length of a hypha, whereas the mannitol is found at discrete, irregular locations. This is the first direct observation of mannitol in intact fungal hyphae. Since the concentration of mannitol in cells varies with respect to position and is not present in all hyphae, this discovery may be related to habitat adaptation, fungal structure and growth stages.

Characterization of mannitol in Curvularia protuberata hyphae by FTIR and Raman spectromicroscopy

USGS Publications Warehouse

Isenor, M.; Kaminskyj, S.G.W.; Rodriguez, R.J.; Redman, R.S.; Gough, K.M.

2010-01-01

FTIR and Raman spectromicroscopy were used to characterize the composition of Curvularia protuberata hyphae, and to compare a strain isolated from plants inhabiting geothermal soils with a non-geothermal isolate. Thermal IR source images of hyphae have been acquired with a 64 ?? 64 element focal plane array detector; single point IR spectra have been obtained with synchrotron source light. In some C. protuberata hyphae, we have discovered the spectral signature of crystalline mannitol, a fungal polyol with complex protective roles. With FTIR-FPA imaging, we have determined that the protein content in cells remains fairly constant throughout the length of a hypha, whereas the mannitol is found at discrete, irregular locations. This is the first direct observation of mannitol in intact fungal hyphae. Since the concentration of mannitol in cells varies with respect to position and is not present in all hyphae, this discovery may be related to habitat adaptation, fungal structure and growth stages. ?? 2010 The Royal Society of Chemistry.

Characterization of mannitol in Curvularia protuberata hyphae by FTIR and Raman spectromicroscopy

USGS Publications Warehouse

Rodriguez, Russell J.; Isenor, Merrill; Kaminsky, Susan G.W.; Redman, S.; Gough, Kathleen M.

2010-01-01

FTIR and Raman spectromicroscopy were used to characterize the composition of Curvularia protuberata hyphae, and to compare a strain isolated from plants inhabiting geothermal soils with a non-geothermal isolate. Thermal IR source images of hyphae have been acquired with a 64 × 64 element focal plane array detector; single point IR spectra have been obtained with synchrotron source light. In some C. protuberata hyphae, we have discovered the spectral signature of crystalline mannitol, a fungal polyol with complex protective roles. With FTIR-FPA imaging, we have determined that the protein content in cells remains fairly constant throughout the length of a hypha, whereas the mannitol is found at discrete, irregular locations. This is the first direct observation of mannitol in intact fungal hyphae. Since the concentration of mannitol in cells varies with respect to position and is not present in all hyphae, this discovery may be related to habitat adaptation, fungal structure and growth stages.

3D FT-IR imaging spectroscopy of phase-separation in a poly(3-hydroxybutyrate)/poly(L-lactic acid) blend

Treesearch

Miriam Unger; Julia Sedlmair; Heinz W. Siesler; Carol Hirschmugl; Barbara Illman

2014-01-01

In the present study, 3D FT-IR spectroscopic imaging measurements were applied to study the phase separation of a poly(3-hydroxybutyrate) (PHB)/poly(L-lactic acid) (PLA) (50:50 wt.%) polymer blend film. While in 2D projection imaging the z-dependent information is overlapped, thereby complicating the analysis, FT-IR spectro-micro-tomography,...

Synthesis, physicochemical characterization, DFT calculation and biological activities of Fe(III) and Co(II)-omeprazole complexes. Potential application in the Helicobacter pylori eradication

NASA Astrophysics Data System (ADS)

Russo, Marcos G.; Vega Hissi, Esteban G.; Rizzi, Alberto C.; Brondino, Carlos D.; Salinas Ibañez, Ángel G.; Vega, Alba E.; Silva, Humberto J.; Mercader, Roberto; Narda, Griselda E.

2014-03-01

The reaction between the antiulcer agent omeprazole (OMZ) with Fe(III) and Co(II) ions was studied, observing a high ability to form metal complexes. The isolated microcrystalline solid complexes were characterized by elemental analysis, X-ray powder diffraction (XRPD), Scanning Electron Microscopy (SEM), magnetic measurements, thermal study, FTIR, UV-Visible, Mössbauer, electronic paramagnetic resonance (EPR), and DFT calculations. The metal-ligand ratio for both complexes was 1:2 determined by elemental and thermal analysis. FTIR spectroscopy showed that OMZ acts as a neutral bidentate ligand through the pyridinic nitrogen of the benzimidazole ring and the oxygen atom of the sulfoxide group, forming a five-membered ring chelate. Electronic, Mössbauer, and EPR spectra together with magnetic measurements indicate a distorted octahedral geometry around the metal ions, where the coordination sphere is completed by two water molecules. SEM and XRPD were used to characterize the morphology and the crystal nature of the complexes. The most favorable conformation for the Fe(III)-OMZ and Co(II)-OMZ complexes was obtained by DFT calculations by using B3LYP/6-31G(d)&LanL2DZ//B3LYP/3-21G(d)&LanL2DZ basis set. Studies of solubility along with the antibacterial activity against Helicobacter pylori for OMZ and its Co(II) and Fe(III) complexes are also reported. Free OMZ and both metal complexes showed antibacterial activity against H. pylori. Co(II)-OMZ presented a minimal inhibitory concentration ˜32 times lower than that of OMZ and ˜65 lower than Fe(III)-OMZ, revealing its promising potential use for the treatment of gastric pathologies associated with the Gram negative bacteria. The morphological changes observed in the cell membrane of the bacteria after the incubation with the metal-complexes were also analyzed by SEM microscopy. The antimicrobial activity of the complexes was proved by the viability test.

Polyethylene-glycol-doped polypyrrole increases the rate performance of the cathode in lithium-sulfur batteries.

PubMed

Wu, Feng; Chen, Junzheng; Li, Li; Zhao, Teng; Liu, Zhen; Chen, Renjie

2013-08-01

Polypyrrole-polyethylene glycol (PPy/PEG)-modified sulfur/aligned carbon nanotubes (PPy/PEG-S/A-CNTs) were synthesized by using an in situ polymerization method. The ratio of PPy to PEG equaled 31.7:1 after polymerization, and the PEG served as a cation dopant in the polymerization and electrochemical reactions. Elemental analysis, FTIR, Raman spectroscopy, XRD, and electrochemical methods were performed to measure the physicochemical properties of the composite. Elemental analysis demonstrated that the sulfur, PPy, PEG, A-CNT, and chloride content in the synthesized material was 64.6%, 22.1%, 0.7%, 12.1%, and 0.5%, respectively. The thickness of the polymer shell was about 15-25 nm, and FTIR confirmed the successful PPy/PEG synthesis. The cathode exhibited a high initial specific capacity of 1355 mAh g(-1) , and a sulfur usage of 81.1%. The reversible capacity of 924 mAh g(-1) was obtained after 100 cycles, showing a remarkably improved cyclability compared to equivalent systems without PEG doping and without any coatings. PPy/PEG provided an effective electronically conductive network and a stable interface structure for the cathode. Rate performance of the PPy/PEG- S/A-CNT composite was more than double that of the unmodified S/A-CNTs. Remarkably, the battery could work at a very high current density of 8 A g(-1) and reached an initial capacity of 542 mAh g(-1) ; it also retained a capacity of 480 mAh g(-1) after 100 cycles. The addition of PEG as a dopant in the PPy shell contributed to this prominent rate improvement. Lithium ions and electrons were available everywhere on the surfaces of the particles, and thus could greatly improve the electrochemical reaction; PEG is a well-known solvent for lithium salts and a very good lithium-ion catcher. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Dimethylaminodiethylenetriamine Derivatives of Fluorescence Chemosenso for Detection of Zn2+ In Aqueous Solution

NASA Astrophysics Data System (ADS)

Adnan, S. N. A. M.; Hasan, S.; Zakaria, S.; Yusof, Y. M.

2017-02-01

Fluorescent chemosensors for the detection and measurement of metal ions, especially for cations environmental interest such as Fe3+, Co2+, Mn2+, Cu2+, and Zn2+ are actively investigated because it shows simplicity, high sensitivity and fast response. New benzenyl derivative bearing pyridine group has been synthesized and studied as fluorescent chemosensor for Zn2+ ion. Chemosensor N-{2-[(4-Dimethylamino-benzylidene)-amino]-ethyl}-N’-pyridin-2-ylmethylene-ethane-1,2-diamine was synthesized by condensation of p-dimethylaminobenzaldehyde, diethylenetriamine and o-pyridinecarbaldehyde and characterized by FT-IR, 1H-NMR and elemental analysis (CHN). FT-IR showed the appearance of peak azomethine (C=NH) at 1639.46 cm-1, pyridine (C-N) at 1591 cm-1and disappearance of NH2 peak at 3278.78 cm-1 after the condensation reaction in between aldehyde and amine. 1H-NMR signal at 8.19 ppm, 3.12 ppm and 8.08 ppm was assigned to C=NH, N(CH3)2 and C-N respectively, confirmed the formation of N-{2-[(4-Dimethylamino-benzylidene)-amino]-ethyl}-N’-pyridin-2-ylmethylene-ethane-1,2-diamine. The elemental analysis was found closed to the theoretical value and the percent composition of A is 91.82%. Sensor A exhibits high selectivity and sensitivity towards Zn2+. Other metal ions such Cu2+, Fe3+, Co2+ and Ni2+ had no such significant effect on the fluorescence. The detection limit of N-{2-[(4-Dimethylamino-benzylidene)-amino]-ethyl}-N’-pyridin-2-ylmethylene-ethane-1,2-diamine for Zn2+ was 3.5 x 10-5 M. M. This sensor exhibits a very good fluorescence sensing ability to Zn2+ over a wide range of pH. Therefore it is capable of being a practical system for the monitoring of Zn2+ concentrations in real water sample.

Satellite Characterization of Biomass Burning: Fourier Transform Infrared Spectroscopy (FTIR) and Scanning Electron Microscope Study of Combustion Experiments

NASA Astrophysics Data System (ADS)

Padilla, D.; Steiner, J. C.

2005-12-01

Fourier Transform Infrared (FTIR) examination of the combustion products of selected forest materials using a meeker burner flame at temperatures up to 500 degrees Celsius produces a cluster of broad distinct peaks throughout the 400 to 4000 cm-1 wavenumber interval. Distinct bands bracketed by wavenumbers 400-700, 1500-1700, 2200-2400 and 3300-3600 cm-1 show variable intensity with an average difference between the least absorbing and most strongly absorbing species of approximately fifty percent. Given that spectral band differences of ten percent are within the range of modern satellite spectrometers, these band differences are of potential value for discriminating between fires that are impacting a range of vegetation types. Corresponding scanning electron microscope and energy dispersive micro-chemical (SEM/ED) analysis establishes that the evolved soot particles exhibit a characteristic rounded morphology, are carbon rich and host a wide range of adsorbed elements, including calcium, aluminum, potassium, silicon, sulfur and trace nitrogen. Combustion experiments involving leaves and branches as a subset of the biomass experiments at 200-500 degrees Celsius yield a similar broad background, but with peak shifts for maxima residing at less than 1700 cm-1. Additional peaks appear in the ranges 1438-1444, 875 and 713 cm-1. These peak are of potential use for discriminating between hot and smoldering fires, and between soot and smoke yields from green woods and whole-wood or lumber. The spectral shifts noted for low temperature smoldering conditions are in the vicinity of those cited for green vegetation and may not be resolved by present satellite platforms. Nevertheless, the experimental peak data set is of potential use for discriminating between a conflagration or accentuated fire and one characterized by smoldering at low temperature. SEM/ED analysis of the combusted leaf, branch, bark and various crown assemblages yields comparable morphological and geochemical signatures although potassium and light elements are slightly concentrated in effluent from the leafy matrix.

A data-driven approach for the study of coagulation phenomena in waste lubricant oils and its relevance in alkaline regeneration treatments.

PubMed

Pinheiro, C T; Ascensão, V R; Reis, M S; Quina, M J; Gando-Ferreira, L M

2017-12-01

Coagulation phenomena can occur in certain types of waste lubricant oils (WLO) during regeneration processes involving alkaline treatments, causing plant shutdowns. In this context, this study addresses the nature of the compounds responsible for the coagulation phenomena after the alkaline treatment. For such, an empirical test was developed to assess the coagulation behaviour of WLO, consisting in the addition of KOH to the WLO followed by heating under stirring conditions. This test was performed on 133 samples and four coagulation classes were identified: A; B1; B2 and C. Moreover, a physicochemical characterization of WLO was carried out regarding viscosity at 40°C, saponification number (SN), total acid number (TAN), surface tension, water content, elemental analysis and functional groups (FTIR). 56 samples of fresh lubricant oils for different applications were also characterized and their properties assessed and compared. Multivariate methods were applied to WLO to discriminate among coagulation classes based on FTIR spectra. It was found that coagulation classes A and B1 exhibit statistically similar patterns for all properties determined. Spectral discriminating analysis did not reveal discriminant peaks for class B1 samples, and the presence of specific additives was pointed as the possible factor underlying the increase in viscosity in this oils. Class B2 presents the absence of additives and oxidation products as differentiating features. In addition, B2 samples showed lower TAN SN, and lower concentration of some elements. Lubricants from gear or hydraulic applications can give rise to this class of WLO. Oils of Class C are mainly composed by synthetic ester type base oils, which hamper regeneration processes using alkaline pretreatments. In future studies, WLO type A and B1 can be classified as a single class. The coagulation phenomena classification becomes A - negative, B - precipitate formation and C - positive. Copyright © 2017 Elsevier B.V. All rights reserved.

Infrared spectroscopy as a tool to characterise starch ordered structure--a joint FTIR-ATR, NMR, XRD and DSC study.

PubMed

Warren, Frederick J; Gidley, Michael J; Flanagan, Bernadine M

2016-03-30

Starch has a heterogeneous, semi-crystalline granular structure and the degree of ordered structure can affect its behaviour in foods and bioplastics. A range of methodologies are employed to study starch structure; differential scanning calorimetry, (13)C nuclear magnetic resonance, X-ray diffraction and Fourier transform infrared spectroscopy (FTIR). Despite the appeal of FTIR as a rapid, non-destructive methodology, there is currently no systematically defined quantitative relationship between FTIR spectral features and other starch structural measures. Here, we subject 61 starch samples to structural analysis, and systematically correlate FTIR spectra with other measures of starch structure. A hydration dependent peak position shift in the FTIR spectra of starch is observed, resulting from increased molecular order, but with complex, non-linear behaviour. We demonstrate that FTIR is a tool that can quantitatively probe short range interactions in starch structure. However, the assumptions of linear relationships between starch ordered structure and peak ratios are overly simplistic. Copyright © 2015 Elsevier Ltd. All rights reserved.

Synthesis, characterization, electrical conductivity and luminescence properties of two copper(II) complexes with tridentate N2O chelating ligands containing imine bond

NASA Astrophysics Data System (ADS)

Gönül, İlyas; Ay, Burak; Karaca, Serkan; Şahin, Onur; Serin, Selahattin

2018-03-01

In the present study, we describe the synthesis and characterization of two tridentate N2O donor ligands, namely, (E)-2-(((2-(diethylamino)ethyl)imino)methyl)-6-methoxyphenol (HL1) and (E)-2-(((2-(diethylamino)ethyl)imino)methyl)-6-ethoxyphenol (HL2), and their copper(II) complexes, [Cu(L1)(CH3COO)] (1), [Cu(L2)(CH3COO)] (2). They have been synthesized under conventional methods and characterized by elemental analysis, FTIR, 1H and 13C NMR, ICP-OES, TGA and GC/MS analysis. For the morphological analysis field emission scanning electron microscopy (FESEM) was used. The geometry of the copper(II) complexes was determined by single crystal X-ray diffraction analysis. The copper(II) ions are in distorted square-pyramidal coordination environments. Complexes crystallize in monoclinic space group, P21/c. The electrical conductivity and luminescence properties of 1-2 have been investigated.

Characterization of milled solid residue from cypress liquefaction in sub- and super ethanol.

PubMed

Liu, Hua-Min; Liu, Yu-Lan

2014-01-01

Cypress liquefaction in sub- and super ethanol was carried out in an autoclave at various temperatures. Milled solid residue (MSR) was isolated from solid residue remaining from the liquefaction process, and its chemical characteristics was comparatively investigated with milled wood lignin (MWL) of cypress by sugar analysis, elemental analysis, FT-IR analysis, gel permeation chromatography, and NMR analysis. Results showed that there were two reactions (de-polymerization and re-polymerization) during the cypress liquefaction in sub- and super ethanol and the re-polymerization reactions were the main reaction at 220-260°C. Considering the stability of side-chain, the stability of lignin side-chain in cypress during liquefaction process in ethanol could be sequenced as follows: β-5>β-β'>β-O-4'. The MSR were mainly from the decomposition and re-polymerization of lignin. This study suggests that characterization of MSR provides a promising method to investigate the mechanisms of cypress liquefaction in ethanol. Crown Copyright © 2013. Published by Elsevier Ltd. All rights reserved.

Induced secondary structure and polymorphism in an intrinsically disordered structural linker of the CNS: solid-state NMR and FTIR spectroscopy of myelin basic protein bound to actin.

PubMed

Ahmed, Mumdooh A M; Bamm, Vladimir V; Shi, Lichi; Steiner-Mosonyi, Marta; Dawson, John F; Brown, Leonid; Harauz, George; Ladizhansky, Vladimir

2009-01-01

The 18.5 kDa isoform of myelin basic protein (MBP) is a peripheral membrane protein that maintains the structural integrity of the myelin sheath of the central nervous system by conjoining the cytoplasmic leaflets of oligodendrocytes and by linking the myelin membrane to the underlying cytoskeleton whose assembly it strongly promotes. It is a multifunctional, intrinsically disordered protein that behaves primarily as a structural stabilizer, but with elements of a transient or induced secondary structure that represent binding sites for calmodulin or SH3-domain-containing proteins, inter alia. In this study we used solid-state NMR (SSNMR) and Fourier transform infrared (FTIR) spectroscopy to study the conformation of 18.5 kDa MBP in association with actin microfilaments and bundles. FTIR spectroscopy of fully (13)C,(15)N-labeled MBP complexed with unlabeled F-actin showed induced folding of both protein partners, viz., some increase in beta-sheet content in actin, and increases in both alpha-helix and beta-sheet content in MBP, albeit with considerable extended structure remaining. Solid-state NMR spectroscopy revealed that MBP in MBP-actin assemblies is structurally heterogeneous but gains ordered secondary structure elements (both alpha-helical and beta-sheet), particularly in the terminal fragments and in a central immunodominant epitope. The overall conformational polymorphism of MBP is consistent with its in vivo roles as both a linker (membranes and cytoskeleton) and a putative signaling hub.

Taxon-specific responses of Southern Ocean diatoms to Fe enrichment revealed by synchrotron radiation FTIR microspectroscopy

NASA Astrophysics Data System (ADS)

Sackett, O.; Armand, L.; Beardall, J.; Hill, R.; Doblin, M.; Connelly, C.; Howes, J.; Stuart, B.; Ralph, P.; Heraud, P.

2014-05-01

Photosynthesis by marine diatoms contributes substantially to global biogeochemical cycling and ecosystem productivity. It is widely accepted that diatoms are extremely sensitive to changes in Fe availability, with numerous in situ experiments demonstrating rapid growth and increased export of elements (e.g. C, Si and Fe) from surface waters as a result of Fe addition. Less is known about the effects of Fe enrichment on the phenotypes of diatoms, such as associated changes in nutritional value, furthermore data on taxon-specific responses is almost non-existent. Enhanced supply of nutrient-rich waters along the coast of the subantarctic Kerguelen Island provide a valuable opportunity to examine the responses of phytoplankton to natural Fe enrichment. Here we demonstrate the use of synchrotron radiation Fourier Transform Infrared (SR-FTIR) microspectroscopy to analyse changes in the macromolecular composition of diatoms collected along the coast and plateau of Kerguelen Island, Southern Ocean. SR-FTIR microspectroscopy enabled the analysis of individual diatom cells from mixed communities of field-collected samples, thereby providing insight into in situ taxon-specific responses in relation to changes in Fe availability. Phenotypic responses were taxon-specific in terms of intraspecific variability and changes in proteins, amino acids, phosphorylated molecules, silicate and carbohydrates. In contrast to some previous studies, silicate levels increased under Fe enrichment, in conjunction with increases in carbohydrate stores. The highly abundant taxon Fragilariopsis kerguelensis displayed a higher level of phenotypic plasticity than Pseudo-nitzschia spp., while analysis of the data pooled across all measured taxa showed different patterns in macromolecular composition compared to those for individual taxon. This study demonstrates that taxon-specific responses to Fe enrichment may not always be accurately reflected by bulk community measurements, highlighting the need for further research into taxon-specific phenotypic responses of phytoplankton to environmental change.

Taxon-specific responses of Southern Ocean diatoms to Fe enrichment revealed by synchrotron radiation FTIR microspectroscopy

NASA Astrophysics Data System (ADS)

Sackett, O.; Armand, L.; Beardall, J.; Hill, R.; Doblin, M.; Connelly, C.; Howes, J.; Stuart, B.; Ralph, P.; Heraud, P.

2014-10-01

Photosynthesis by marine diatoms contributes substantially to global biogeochemical cycling and ecosystem productivity. It is widely accepted that diatoms are extremely sensitive to changes in Fe availability, with numerous in situ experiments demonstrating rapid growth and increased export of elements (e.g. C, Si and Fe) from surface waters as a result of Fe addition. Less is known about the effects of Fe enrichment on the phenotypes of diatoms, such as associated changes in nutritional value - furthermore, data on taxon-specific responses are almost non-existent. Enhanced supply of nutrient-rich waters along the coast of the subantarctic Kerguelen Island provide a valuable opportunity to examine the responses of phytoplankton to natural Fe enrichment. Here we demonstrate the use of synchrotron radiation Fourier Transform Infrared (SR-FTIR) microspectroscopy to analyse changes in the macromolecular composition of diatoms collected along the coast and plateau of Kerguelen Island, Southern Ocean. SR-FTIR microspectroscopy enabled the analysis of individual diatom cells from mixed communities of field-collected samples, thereby providing insight into in situ taxon-specific responses in relation to changes in Fe availability. Phenotypic responses were taxon-specific in terms of intraspecific variability and changes in proteins, amino acids, phosphorylated molecules, silicate/silicic acid and carbohydrates. In contrast to some previous studies, silicate/silicic acid levels increased under Fe enrichment, in conjunction with increases in carbohydrate stores. The highly abundant taxon Fragilariopsis kerguelensis displayed a higher level of phenotypic plasticity than Pseudo-nitzschia spp., while analysis of the data pooled across all measured taxa showed different patterns in macromolecular composition compared to those for individual taxon. This study demonstrates that taxon-specific responses to Fe enrichment may not always be accurately reflected by bulk community measurements, highlighting the need for further research into taxon-specific phenotypic responses of phytoplankton to environmental change.

Fourier Transform Infrared Spectroscopy as a Tool in Analysis of Proteus mirabilis Endotoxins.

PubMed

Żarnowiec, Paulina; Czerwonka, Grzegorz; Kaca, Wiesław

2017-01-01

Fourier transform infrared spectroscopy (FT-IR) was used to scan whole bacterial cells as well as lipopolysaccharides (LPSs, endotoxins) isolated from them. Proteus mirabilis cells, with chemically defined LPSs, served as a model for the ATR FT-IR method. The paper focuses on three steps of infrared spectroscopy: (1) sample preparation, (2) IR scanning, and (3) multivariate analysis of IR data (principal component analysis, PCA).

The function of prehistoric lithic tools: a combined study of use-wear analysis and FTIR microspectroscopy.

PubMed

Nunziante Cesaro, Stella; Lemorini, Cristina

2012-02-01

The application of combined use-wear analysis and FTIR micro spectroscopy for the investigation of the flint and obsidian tools from the archaeological sites of Masseria Candelaro (Foggia, Italy) and Sant'Anna di Oria (Brindisi, Italy) aiming to clarify their functional use is described. The tools excavated in the former site showed in a very high percentage spectroscopically detectable residues on their working edges. The identification of micro deposits is based on comparison with a great number of replicas studied in the same experimental conditions. FTIR data confirmed in almost all cases the use-wear analysis suggestions and added details about the material processed and about the working procedures. Copyright © 2011 Elsevier B.V. All rights reserved.

Flame retardant finishing of cotton fabric based on synergistic compounds containing boron and nitrogen.

PubMed

Xie, Kongliang; Gao, Aiqin; Zhang, Yongsheng

2013-10-15

Boric acid and compound containing nitrogen, 2,4,6-tri[(2-hydroxy-3-trimethyl-ammonium)propyl]-1,3,5-triazine chloride (Tri-HTAC) were used to finish cotton fabric. The flame retardant properties of the finished cotton fabrics and the synergetic effects of boron and nitrogen elements were investigated and evaluated by limited oxygen index (LOI) method. The mechanism of cross-linking reaction among cotton fiber, Tri-HTAC, and boric acid was discussed by FTIR and element analysis. The thermal stability and surface morphology of the finished cotton fabrics were investigated by thermogravimetric analysis (TGA) and scanning electron microscope (SEM), respectively. The finishing system of the mixture containing boron and nitrogen showed excellent synergistic flame retardancy for cotton fabric. The cotton fabric finished with mixture system had excellent flame retardancy. The LOI value of the treated cotton fabric increased over 27.5. Tri-HTAC could form covalent bonds with cellulose fiber and boric acid. The flame retardant cotton fabric showed a slight decrease in tensile strength and whiteness. The surface morphology of flame retardant cotton fiber was smooth. Copyright © 2013 Elsevier Ltd. All rights reserved.

Microwave combustion synthesis of Co1-xZnxFe2O4 (0⩽x⩽0.5): Structural, magnetic, optical and vibrational spectroscopic studies.

PubMed

Sundararajan, M; Kennedy, L John; Vijaya, J Judith; Aruldoss, Udaya

2015-04-05

Nanostructured pure and zinc doped cobalt ferrites (Co1-xZnxFe2O4 where x fraction ranging from 0 to 0.5) were prepared by microwave combustion method employing urea as a fuel. The nanostructured samples were characterized by using various instrumental techniques such as X-ray powder diffractometry, high resolution scanning electron microscopy, energy dispersive X-ray analysis, UV-visible diffuse reflectance spectroscopy, photoluminescence spectroscopy and Fourier transformed infrared (FT-IR) spectroscopy. Vibrating sample magnetometry at room temperature was recorded to study the magnetic behavior of the samples. X-ray analysis and the FT-IR spectroscopy revealed the formation of cobalt ferrite cubic spinel-type structure. The average crystallite sizes for the samples were in the range of 3.07-11.30 nm. The direct band gap (Eg) was estimated using Kubelka-Munk method and is obtained from the UV-vis spectra. The band gap value decreased with an increase in zinc fraction (2.56-2.17 eV). The violet and green emission observed in the photoluminescence spectra revealed that cobalt ferrites are governed by defect controlled processes. The elemental analysis of zinc doped cobalt ferrites were obtained from energy dispersive X-ray (EDX) analysis. From the magnetic measurements, it is observed that cobalt ferrite and zinc doped cobalt ferrite systems fall under the soft ferrite category. The saturation magnetization (Ms) value of undoped cobalt ferrite is 14.26 emu/g, and it has reached a maximum of 29.61 emu/g for Co0.7Zn0.3Fe2O4. Copyright © 2014 Elsevier B.V. All rights reserved.

DFT calculations on molecular structure, spectral analysis, multiple interactions, reactivity, NLO property and molecular docking study of flavanol-2,4-dinitrophenylhydrazone

NASA Astrophysics Data System (ADS)

Singh, Ravindra Kumar; Singh, Ashok Kumar

2017-02-01

A new flavanol-2,4-dinitrophenylhydrazone (FDNP) was synthesized and its structure was confirmed by FT-IR, FT-Raman, 1H NMR, mass spectrometry and elemental analysis. All quantum chemical calculations were carried out at level of density functional theory (DFT) with B3LYP functional using 6-311++ G (d,p) basis atomic set. UV-Vis absorption spectra for the singlet-singlet transition computed for fully optimized ground state geometry using Time-Dependent-Density Functional Theory (TD-DFT) with CAM-B3LYP functional was found to be in consistent with that of experimental findings. Analysis of vibrational (FT-IR and FT-Raman) spectrum and their assignments has been done by computing Potential Energy Distribution (PED) using Gar2ped. HOMO-LUMO analysis was performed and reactivity descriptors were calculated. Calculated global electrophilicity index (ω = 7.986 eV) shows molecule to be a strong electrophile. 1H NMR chemical shift calculated with the help of gauge-including atomic orbital (GIAO) approach shows agreement with experimental data. Various intramolecular interactions were analysed by AIM approach. DFT computed total first static hyperpolarizability (β0 = 189.03 × 10-30 esu) indicates that title molecule can be used as attractive future NLO material. Solvent induced effects on the NLO properties studied by using self-consistent reaction field (SCRF) method shows that β0 value increases with increase in solvent polarity. To study the thermal behaviour of title molecule, thermodynamic properties such as heat capacity, entropy and enthalpy change at various temperatures have been calculated and reported. Molecular docking results suggests title molecule to be a potential kinase inhibitor and might be used in future for designing of new anticancer drug.

Synthesis, characterization and relativistic DFT studies of fac-Re(CO)3(isonicotinic acid)2Cl complex

NASA Astrophysics Data System (ADS)

Zúñiga, César; Oyarzún, Diego P.; Martin-Transaco, Rudy; Yáñez-S, Mauricio; Tello, Alejandra; Fuentealba, Mauricio; Cantero-López, Plinio; Arratia-Pérez, Ramiro

2017-11-01

In this work, new fac-Re(CO)3(PyCOOH)2Cl from isonicotinic acid ligand has been prepared. The complex was characterized by structural (single-crystal X-ray diffraction), elemental analysis and spectroscopic (FTIR, NMR, UV-vis spectroscopy) methods. DFT and TDDFT calculations were performed to obtain the electronic transitions involved in their UV-Vis spectrum. The excitation energies agree with the experimental results. The TDDFT calculations suggest that experimental mixed absorption bands at 270 and 314 nm could be assigned to (MLCT-LLCT)/MLCT transitions. Natural Bond Orbitals (NBO) approach has enabled studying the effects of bonding interactions. E(2) energies confirm the occurrence of ICT (Intra-molecular Charge Transfer) within the molecule.

Preparation, Characterization, and Antimicrobial Activities of Bimetallic Complexes of Sarcosine with Zn(II) and Sn(IV)

PubMed Central

Arafat, Yasir; Ali, Saqib; Shahzadi, Saira; Shahid, Muhammad

2013-01-01

Heterobimetallic complexes of Zn(II) and Sn(IV) with sarcosine have been synthesized at room temperature under stirring conditions by the reaction of sarcosine and zinc acetate in 2 : 1 molar ratio followed by the stepwise addition of CS2 and organotin(IV) halides, where R = Me, n-Bu, and Ph. The complexes were characterized by elemental analysis, FT-IR and NMR (1H, 13C) spectroscopy. IR data showed that the ligand acts in a bidentate manner. NMR data revealed the four coordinate geometry in solution state. In vitro antimicrobial activities data showed that complexes (3) and (4) were effective against bacterial and fungal strains with few exceptions. PMID:24235910

Size controlled biogenic silver nanoparticles as antibacterial agent against isolates from HIV infected patients

NASA Astrophysics Data System (ADS)

Suganya, K. S. Uma; Govindaraju, K.; Kumar, V. Ganesh; Dhas, T. Stalin; Karthick, V.; Singaravelu, G.; Elanchezhiyan, M.

2015-06-01

Silver nanoparticles (AgNPs) are synthesized using biological sources due to its high specificity in biomedical applications. Herein, we report the size and shape controlled synthesis of AgNPs using the aqueous extract of blue green alga, Spirulina platensis. Size, shape and elemental composition of AgNPs were characterized using UV-vis spectroscopy, Fluorescence spectroscopy, FT-IR (Fourier Transform-Infrared Spectroscopy), FT-RS (Fourier Transform-Raman Spectroscopy), SEM-EDAX (Scanning Electron Microscopy-Energy Dispersive X-ray analysis) and HR-TEM (High Resolution Transmission Electron Microscopy). AgNPs were stable, well defined and monodispersed (spherical) with an average size of 6 nm. The synthesized AgNPs were tested for its antibacterial potency against isolates obtained from HIV patients.

Synthesis and characterization of a novel potato starch derivative with cationic acetylcholine groups.

PubMed

Zhang, Bing; Ni, Boli; Lü, Shaoyu; Cui, Dapeng; Liu, Mingzhu; Gong, Honghong; Han, Fei

2012-04-01

A novel substance, cationic acetylcholine potato starch (CAPS), was developed for the first time. The synthesis process had three steps: first, carboxymethyl potato starch (CMPS) was synthesized under sodium hydroxide alkaline condition and in isopropyl alcohol organic media; second, bromocholine chloride (BCC) was synthesized with sulphuric acid as a catalytic agent; finally, CAPS was synthesized by the reaction of CMPS with BCC in N,N'-dimethylformamide (DMF). The degree of substitution (DS) of CAPS was determined by ammonia gas-sensing electrode and elemental analysis. CAPS was characterized by Fourier transformed infrared (FTIR) and near infrared (FTNIR) spectroscopy, scanning electron microscopy (SEM), X-ray diffraction (XRD) and differential scanning calorimetry (DSC). Copyright © 2012 Elsevier B.V. All rights reserved.

Synthesis Characterization and DNA Interaction Studies of a New Zn(II) Complex Containing Different Dinitrogen Aromatic Ligands

PubMed Central

Shahabadi, Nahid; Mohammadi, Somaye

2012-01-01

A mononuclear complex of Zn(II), [Zn(DIP)2 (DMP)] (NO3)2 ·2H2O in which DIP is 4,7-diphenyl-1,10-phenanthroline and DMP is 4,4′-dimethyl-2,2′-bipyridine has been prepared and characterized by 1HNMR spectroscopy, FT-IR, UV-Vis and elemental analysis techniques. DNA-binding properties of the complex were studied using UV-vis spectra, circular dichroism (CD) spectra, fluorescence, cyclic voltammetry (CV), and viscosity measurements. The results indicate that this zinc(II) complex can intercalate into the stacked base pairs of DNA and compete with the strong intercalator ethidium bromide for the intercalative binding sites. PMID:22956919

Synthesis, spectral and thermal studies of the newly hydrogen bonded charge transfer complex of o-phenylenediamine with π acceptor picric acid

NASA Astrophysics Data System (ADS)

Khan, Ishaat M.; Ahmad, Afaq

2010-10-01

Newly proton or charge transfer complex [(OPDH) +(PA) -] was synthesized by the reaction of the donor, o-phenylenediamine (OPD) with acceptor, 2,4,6-trinitrophenol (PAH). The chemical reaction has occurred via strong hydrogen bonding followed by migration of proton from acceptor to donor. UV-vis, 1H NMR and FTIR spectra, in addition to the thermal and elemental analysis were used to confirm the proposed occurrence of the chemical reaction and to investigate the newly synthesized solid CT complex. The stoichiometry of the CT complex was found to be 1:1. The formation constant and molar extinction coefficient of the CT complex were evaluated by the Benesi-Hildebrand equation.

Heteroleptic Palladium(II) dithiocarbamates: Synthesis, characterization and in vitro biological screening

NASA Astrophysics Data System (ADS)

Khan, Shahan Zeb; Zia-ur-Rehman; Amir, Muhammad Kashif; Ullah, Imdad; Akhter, M. S.; Bélanger-Gariepy, Francine

2018-03-01

Two new heteroleptic Pd(II) complexes of sodium 4-(2-pyrimidyl)piperazine-1-carbodithioate with tris-p-flourophenylphosphine (1) and tris-p-chlorophenylphosphine (2) were prepared and characterized by elemental analysis, FT-IR, multinuclear NMR {1H, 13C and 31P} and single-crystal X-ray diffraction measurement. In both complexes, Pd exhibit pseudo square planner geometry mediated by SS chelate, P and Cl. In vitro cytotoxicity against five different cancer cell lines using staurosporine as a standard revealed 1 to be more cytotoxic than 2, though both complexes are more active than cisplatin. Subsequent DNA binding studies revealed that non-covalent complex-DNA interaction may be the reason for arresting cancer cell growth. Furthermore, 1 and 2 are potent antioxidant agents.

Synthesis, spectral features and biological activity of some novel hetarylazo dyes derived from 6-amino-1,3-dimethyluracil

NASA Astrophysics Data System (ADS)

Yousefi, Hessamoddin; Yahyazadeh, Asieh; Yazdanbakhsh, Mohammad Reza; Rassa, Mehdi; Moradi-e-Rufchahi, Enayat O.'llah

2012-05-01

A series of hetarylazoaminouracil dyes were prepared by coupling of 6-amino-1,3-dimethyluracil with eight diazotized heterocyclic amines in nitrosyl sulphuric acid. The prepared azo dyes were characterized by UV-Vis, FT-IR, 13C NMR, 1H NMR spectroscopic techniques and elemental analysis. The solvatochromism of dyes was evaluated with respect to wavelength of maximum absorption (λmax) in seven solvents with different polarities: acetic acid, methanol, water, chloroform, acetonitrile, dimethyl sulfoxide and dimethyl formamide. The effects of acid, base and concentration of the dye on the visible absorption spectra were also reported. In addition, the antimicrobial activity of the synthesized dyes was evaluated on Escherichia coli, Bacillus subtilis, Micrococcus leuteus and Pseudomonas aeruginosa.

Discrimination of cultivation ages and cultivars of ginseng leaves using Fourier transform infrared spectroscopy combined with multivariate analysis

PubMed Central

Kwon, Yong-Kook; Ahn, Myung Suk; Park, Jong Suk; Liu, Jang Ryol; In, Dong Su; Min, Byung Whan; Kim, Suk Weon

2013-01-01

To determine whether Fourier transform (FT)-IR spectral analysis combined with multivariate analysis of whole-cell extracts from ginseng leaves can be applied as a high-throughput discrimination system of cultivation ages and cultivars, a total of total 480 leaf samples belonging to 12 categories corresponding to four different cultivars (Yunpung, Kumpung, Chunpung, and an open-pollinated variety) and three different cultivation ages (1 yr, 2 yr, and 3 yr) were subjected to FT-IR. The spectral data were analyzed by principal component analysis and partial least squares-discriminant analysis. A dendrogram based on hierarchical clustering analysis of the FT-IR spectral data on ginseng leaves showed that leaf samples were initially segregated into three groups in a cultivation age-dependent manner. Then, within the same cultivation age group, leaf samples were clustered into four subgroups in a cultivar-dependent manner. The overall prediction accuracy for discrimination of cultivars and cultivation ages was 94.8% in a cross-validation test. These results clearly show that the FT-IR spectra combined with multivariate analysis from ginseng leaves can be applied as an alternative tool for discriminating of ginseng cultivars and cultivation ages. Therefore, we suggest that this result could be used as a rapid and reliable F1 hybrid seed-screening tool for accelerating the conventional breeding of ginseng. PMID:24558311

Interpreting the results of chemical stone analysis in the era of modern stone analysis techniques

PubMed Central

Gilad, Ron; Williams, James C.; Usman, Kalba D.; Holland, Ronen; Golan, Shay; Ruth, Tor; Lifshitz, David

2017-01-01

Introduction and Objective Stone analysis should be performed in all first-time stone formers. The preferred analytical procedures are Fourier-transform infrared spectroscopy (FT-IR) or X-ray diffraction (XRD). However, due to limited resources, chemical analysis (CA) is still in use throughout the world. The aim of the study was to compare FT-IR and CA in well matched stone specimens and characterize the pros and cons of CA. Methods In a prospective bi-center study, urinary stones were retrieved from 60 consecutive endoscopic procedures. In order to assure that identical stone samples were sent for analyses, the samples were analyzed initially by micro-computed tomography to assess uniformity of each specimen before submitted for FTIR and CA. Results Overall, the results of CA did not match with the FTIR results in 56% of the cases. In 16% of the cases CA missed the major stone component and in 40% the minor stone component. 37 of the 60 specimens contained CaOx as major component by FTIR, and CA reported major CaOx in 47/60, resulting in high sensitivity, but very poor specificity. CA was relatively accurate for UA and cystine. CA missed struvite and calcium phosphate as a major component in all cases. In mixed stones the sensitivity of CA for the minor component was poor, generally less than 50%. Conclusions Urinary stone analysis using CA provides only limited data that should be interpreted carefully. Urinary stone analysis using CA is likely to result in clinically significant errors in its assessment of stone composition. Although the monetary costs of CA are relatively modest, this method does not provide the level of analytical specificity required for proper management of patients with metabolic stones. PMID:26956131

Quantification of material state using reflectance FTIR spectroscopy

NASA Astrophysics Data System (ADS)

Criner, Amanda K.; Henry, Christine; Imel, Megan; King, Derek

2018-04-01

A common, frequently violated, assumption implicit in many data analysis techniques is that data is of the same quality across observations. The effect of this assumption is discussed and demonstrated in the example of FTIR of CMCs. An alternative analysis, which incorporates the variation in the quality of the data, is presented. A comparison between the analyses is used to demonstrate this difference.

Combined use of infrared and hard X-ray microprobes for spectroscopy-based neuroanatomy

NASA Astrophysics Data System (ADS)

Surowka, A. D.; Ziomber, A.; Czyzycki, M.; Migliori, A.; Pieklo, L.; Kasper, K.; Szczerbowska-Boruchowska, M.

2018-05-01

Understanding the pathological triggers that affect the structural and physiological integrity of biochemical milieu of neurons is crucial to extend our knowledge on brain disorders, that are in many circumstances hardly treatable. Over recently, by using sophisticated hyperspectral micro-imaging modalities, it has been placed within our reach to get an insight into high fidelity histological details along with corresponding biochemical information in a label-free fashion, without using any additional chemical fixatives. However, in order to push forwards extensive application of these methods in the clinical arena, it is viable to make further iterations in novel data analysis protocols in order to boost their sensitivity. Therefore, in our study we proposed a new combined approach utilizing both benchtop Fourier transform infrared (FTIR) and synchrotron X-ray fluorescence (SR-XRF) micro-spectroscopies coupled with multivariate data clustering using the K-means algorithm for combined molecular and elemental micro-imaging, so that these complimentary analytical tools could be used for delineating between various brain structures based on their biochemical composition. By utilizing mid-IR transmission FTIR experiments, the biochemical composition in terms of lipids, proteins and phosphodiesters became accessible. In turn, the SR-XRF experiment was carried out at the advanced IAEA X-ray spectrometry station at Elettra Sincrotrone Trieste. By measuring in vacuum and by using the primary exciting X-ray beam, monochromatized to 10.5 keV, we took advantage of accessing the characteristic X-ray lines of a variety of elements ranging from carbon to zinc. Herein, we can report that the developed methodology has high specificity for label-free discriminating between lipid- and protein-rich brain tissue areas.

Induced wettability and surface-volume correlation of composition for bovine bone derived hydroxyapatite particles

NASA Astrophysics Data System (ADS)

Maidaniuc, Andreea; Miculescu, Florin; Voicu, Stefan Ioan; Andronescu, Corina; Miculescu, Marian; Matei, Ecaterina; Mocanu, Aura Catalina; Pencea, Ion; Csaki, Ioana; Machedon-Pisu, Teodor; Ciocan, Lucian Toma

2018-04-01

Hydroxyapatite powders characteristics need to be determined both for quality control purposes and for a proper control of microstructural features of bone reconstruction products. This study combines bulk morphological and compositional analysis methods (XRF, SEM-EDS, FT-IR) with surface-related methods (XPS, contact angle measurements) in order to correlate the characteristics of hydroxyapatite powders derived from bovine bone for its use in medical applications. An experimental approach for correlating the surface and volume composition was designed based on the analysis depth of each spectral method involved in the study. Next, the influences of powder particle size and forming method on the contact angle between water drops and ceramic surface were evaluated for identifying suitable strategies of tuning hydroxyapatite's wettability. The results revealed a preferential arrangement of chemical elements at the surface of hydroxyapatite particles which could induce a favourable material behaviour in terms of sinterability and biological performance.

Immobilization Effect of Morphological, Thermal and Optical Properties in Biotemplate on Zinc Oxide Nanocomposite from Chitosan

NASA Astrophysics Data System (ADS)

Karpuraranjith, M.; Thambidurai, S.

Biotemplate-based zinc oxide nanocomposite was effectively prepared via simple chemical precipitation route. The functional groups of amino (-NH2), hydroxyl (-OH) and O-Zn-O were confirmed and characterized by FTIR spectroscopy. The structural and morphological properties were confirmed by XRD, UV-Vis DRS, HR-SEM and TEM analyses. The elemental composition of carbon, nitrogen, zinc and oxygen was confirmed by energy-dispersive X-ray analysis (EDAX) and Brunauer-Emmett-Teller high surface area of materials was estimated to be 52.49m2/g, respectively. Thermogravimetric analysis (TGA) shows that biotemplate on zinc oxide nanocomposite has higher thermal stability than chitosan matrix. The results demonstrate that biotemplate on zinc oxide matrix causes immobilization effect among the two components. Therefore, chitosan-ZnO nanocomposite has a microcrystalline morphological structure and also good thermal stability, so it can be a promising material for sensors, medical, tissue engineering and wastewater treatment applications.

Effect of torrefaction conditions on greenhouse crop residue: Optimization of conditions to upgrade solid characteristics.

PubMed

Iáñez-Rodríguez, Irene; Martín-Lara, María Ángeles; Blázquez, Gabriel; Pérez, Antonio; Calero, Mónica

2017-11-01

This work investigated the possibility of using a greenhouse crop waste as a fuel, since it is an abundant residue in the Mediterranean area of Spain. The residue is mainly composed by biomass with a little quantity of plastic. The physical and chemical characteristics of the biomass were determined by elemental analysis, proximate analysis, FT-IR, FE-SEM and thermogravimetry. Additionally, a torrefaction process was carried out as a pre-treatment to improve the energy properties of the biomass material. The optimal conditions (time and temperature) of torrefaction were found to be 263°C and 15min using the gain and loss method. Further studies were carried out with the sample prepared with the nearest conditions to the optimal in order to determine the effect of the plastic fraction in the characteristics and torrefaction process of the waste studied. Copyright © 2017 Elsevier Ltd. All rights reserved.

Copper(II) cyanido-bridged bimetallic nitroprusside-based complexes: Syntheses, X-ray structures, magnetic properties, 57Fe Mössbauer spectroscopy and thermal studies

NASA Astrophysics Data System (ADS)

Trávníček, Zdeněk; Herchel, Radovan; Mikulík, Jiří; Zbořil, Radek

2010-05-01

Three heterobimetallic cyanido-bridged copper(II) nitroprusside-based complexes of the compositions [Cu(tet)Fe(CN) 5NO]·H 2O ( 1), where tet= N,N' -bis(3-aminopropyl)ethylenediamine, [Cu(hto)Fe(CN) 5NO]·2H 2O ( 2), where hto=1,3,6,9,11,14-hexaazatricyclo[12.2.1.1 6,9]octadecane and [Cu(nme) 2Fe(CN) 5NO]·H 2O ( 3), where nme= N-methylethylenediamine, were synthesized and characterized by elemental analyses, 57Fe Mössbauer and FTIR spectroscopies, thermal analysis, magnetic measurements and single-crystal X-ray analysis. The products of thermal degradation processes of 2 and 3 were studied by XRD, 57Fe Mössbauer spectroscopy, SEM and EDS, and they were identified as mixtures of CuFe 2O 4 and CuO.

Improving lead adsorption through chemical modification of wheat straw by lactic acid

NASA Astrophysics Data System (ADS)

Mu, Ruimin; Wang, Minxiang; Bu, Qingwei; Liu, Dong; Zhao, Yanli

2018-01-01

This work describes the creation of a new cellulosic material derived from wheat straw modified by lactic acid for adsorption of lead in aqueous solution, called 0.3LANS (the concentration of the lactic acid were 0.3mol/L). Batch experiments were conducted to study the effects of initial pH value, contact time, adsorbent dose, initial concentration and temperature. Fourier transform infrared (FTIR), Elemental analysis, BET surface area and Scanning electron micrographs (SEM) analysis were used to investigate the chemical modification. Adsorption isotherm models namely, Langmuir, Freundlich were used to analyse the equilibrium data, and the Langmuir isotherm model provided the best correlation, means that the adsorption was chemical monolayer adsorption and the adsorption capacity qm was increased with increasing temperature, and reached 51.49mg/g for 0.3LANS at 35°C, showing adsorption was exothermic.

Synthesis and structural characterization of CdS nanoparticles using nitrogen adducts of mixed diisopropylthiourea and dithiolate derivatives of Cd(II) complexes

NASA Astrophysics Data System (ADS)

Osuntokun, Jejenija; Ajibade, Peter A.

2015-07-01

[Cd(diptu)2(ced)], [Cd(diptu)2(ced)(bpy)], [Cd(diptu)2(ced)(phen)], (where diptu = diisopropyl thiourea; ced = 1-cyano-1-carboethoxylethylene-2,2‧-dithiolate; bpy = 2,2‧-bipyridine and phen = 1,10-phenanthroline) have been prepared and used as single source precursors for the preparation of hexadecylamine capped CdS nanoparticles. The precursor complexes were characterized by elemental analysis, FTIR and TGA. The structural properties of the nanoparticles were investigated using powder X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy techniques (SEM). The optical properties of the nanoparticles were studied using UV-Visible and photoluminescence spectroscopy. The XRD analysis showed that the nanoparticles were indexed to the hexagonal phase of CdS and the TEM results showed CdS nanoparticles with average crystallite sizes of 4.00-8.80 nm.

Microcellular foaming of arabinoxylan and PEGylated arabinoxylan with supercritical CO2.

PubMed

Härdelin, Linda; Ström, Anna; Di Maio, Ernesto; Iannace, Salvatore; Larsson, Anette

2018-02-01

In this study, arabinoxylan extracted from barley husks was reacted with polyethylene glycol (PEG) of various molecular weights to introduce an internal plasticizer into the polymer matrix. A successful PEGylation reaction was identified using FTIR and elemental analysis. Thermal and mechanical properties were studied using dynamic mechanical analysis, which revealed that the attachment of PEG chains reduced the glass transition temperature by up to 25°C. Foaming experiments were conducted under different test conditions in a batch foaming process with supercritical CO 2 in a thermoregulated and pressurized cylinder. The foams were evaluated using SEM by studying the morphology of the samples foamed at different temperatures. The unmodified arabinoxylan sample was found to produce the best foam morphology, though the PEGylated samples could be produced at lower temperatures than could the unmodified arabinoxylan. This was interpreted as due to the decrease in the glass transition temperature. Copyright © 2017. Published by Elsevier Ltd.

Preparation and characterization of a novel adsorbent from Moringa oleifera leaf

NASA Astrophysics Data System (ADS)

Bello, Olugbenga Solomon; Adegoke, Kayode Adesina; Akinyunni, Opeyemi Omowumi

2017-06-01

A new and novel adsorbent was obtained by impregnation of Moringa oleifera leaf in H2SO4 and NaOH, respectively. Prepared adsorbents were characterized using elemental analysis, FT-IR, SEM, TGA and EDX analyses, respectively. The effects of operational parameters, such as pH, moisture content, ash content, porosity and iodine number on these adsorbents were investigated and compared with those of commercial activated carbon (CAC). EDX results of acid activated M. oleifera leaf have the highest percentage of carbon by weight (69.40 %) and (76.11 %) by atom, respectively. Proximate analysis showed that the fixed carbon content of acid activated M. oleifera leaf (69.14 ± 0.01) was the highest of all adsorbents studied. Conclusively, the present investigation shows that acid activated M. oleifera leaf is a good alternative adsorbent that could be used in lieu of CAC for recovery of dyes and heavy metal from aqueous solutions and other separation techniques.

Nanostructured zirconium phosphate as ion exchanger: Synthesis, size dependent property and analytical application in radiochemical separation.

PubMed

Chakraborty, Rajesh; Bhattacharaya, Koustava; Chattopadhyay, Pabitra

2014-02-01

Nanostructured zirconium phosphates (ZPs) of different sizes were synthesized using Tritron X-100 (polyethylene glycol-p-isooctylphenyl ether) surfactant. The materials were characterized by FTIR and powdered X-ray diffraction (XRD). The structural and morphological details of the material were established by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The SEM study was followed by energy dispersive spectroscopic analysis (EDS) for elemental analysis of the sample. The particle sizes were determined by dynamic light scattering (DLS) method. Ion exchange capacity of these nanomaterials towards different metal ions was measured and size-dependent ion exchange property of the materials was investigated thoroughly. The nanomaterial of the smallest size (ca. 21.04nm) was employed to separate carrier-free (137m)Ba from (137)Cs in column chromatographic technique using 1.0M HNO3 as eluting agent at pH=5. © 2013 Elsevier Ltd. All rights reserved.

Efficient transformation of corn stover to furfural using p-hydroxybenzenesulfonic acid-formaldehyde resin solid acid.

PubMed

Zhang, Tingwei; Li, Wenzhi; An, Shengxin; Huang, Feng; Li, Xinzhe; Liu, Jingrong; Pei, Gang; Liu, Qiying

2018-05-24

In this work, p-hydroxybenzenesulfonic acid-formaldehyde resin acid catalyst (MSPFR), was synthesized by a hydrothermal method, and employed for the furfural production from raw corn stover. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), N 2 adsorption-desorption, elemental analysis (EA), thermogravimetric analysis (TGA), and Fourier transform infrared spectroscopy (FT-IR) were used to characterize the MSPFR. The effects of reaction time, temperature, solvents and corn stover loading were investigated. The MSPFR presented high catalytic activity for the formation of furfural from corn stover. When the MSPFR/corn stover mass loading ratio was 0.5, a higher furfural yield of 43.4% could be achieved at 190 °C in 100 min with 30.7% 5-hydroxymethylfurfural (HMF) yield. Additionally, quite importantly, the recyclability of the MSPFR for xylose dehydration is good, and for the conversion of corn stover was reasonable. Copyright © 2018 Elsevier Ltd. All rights reserved.

Carbonate-based zeolitic imidazolate framework for highly selective CO2 capture.

PubMed

Basnayake, Sajani A; Su, Jie; Zou, Xiadong; Balkus, Kenneth J

2015-02-16

In this study, we report the formation of a new crystal structure, ZIF-CO3-1, which results from the reaction of Zn(2+), 2-methylimidazole, and carbonate. ZIF-CO3-1 can be synthesized solvothermally in N,N-dimethylformamide (DMF)/water (H2O) or by utilizing of CO2 gas at various temperatures in DMF/H2O or H2O. This reaction selectively consumes CO2 because CO2 is incorporated in the ZIF as carbonate. CO2 can be quantitatively released by acidifying the ZIF. Powder X-ray diffraction, single-crystal X-ray diffraction, FTIR spectroscopy, scanning electron microscopy, elemental analysis, and thermogravimetric analysis were used to characterize the ZIF structure. ZIF-CO3-1 (chemical formula C9H10N4O3Zn2), crystallizes in the orthorhombic crystal system with noncentrosymmetric space group Pba2.

Synthesis, characterization and catalytic oxidation properties of multi-wall carbon nanotubes with a covalently attached copper(II) salen complex

NASA Astrophysics Data System (ADS)

Salavati-Niasari, Masoud; Bazarganipour, Mehdi

2009-06-01

Hydroxyl functionalized copper(II) Schiff-base, N,N'-bis(4-hydroxysalicylidene)-ethylene-1,2-diaminecopper(II), [Cu((OH) 2-salen)], has been covalently anchored on modified MWCNTs. The new modified MWCNTs ([Cu((OH) 2-salen)]-MWCNTs) have been characterized by TEM, thermal analysis, XRD, XPS, UV-vis, DRS, FT-IR spectroscopy and elemental analysis. The modified copper(II) MWCNTs solid was used to affect the catalytic oxidation of ethylbenzene with tert-butylhydroperoxide as the oxidant at 333 K. The system is truly heterogeneous (no leaching observed) and reusable (no decrease in activity) in three consecutive runs. Acetophenone was the major product though small amounts of o- and p-hydroxyacetophenones were also formed revealing that C-H bond activation takes place both at benzylic and aromatic ring carbon atoms. Ring hydroxylation was more over the "neat" complexes than over the encapsulated complexes.

Growth of L-Valinium Aluminium Chloride single crystal for OLED and super-capacitor applications

NASA Astrophysics Data System (ADS)

Kalaivani, D.; Vijayalakshmi, S.; Theras, J. Elberin Mary; Jayaraman, D.; Joseph, V.

2015-12-01

L-Valinium Aluminium Chloride (LVAC), a novel semi-organic material, was grown using slow evaporation under isothermal condition. The single crystal data reveal that the grown crystal belongs to monoclinic system. The SEM micrographs give clear picture about the surface morphology. Further, they confirm the inclusion of aluminium chloride into atomic sites of L-Valine. The compositional elements present in the crystal were identified through EDAX analysis. The mass spectral analysis was carried out to determine the molecular weight of the grown crystal. The optical transparency of the grown crystal was investigated by UV-vis-NIR spectrum. FTIR spectral study was used to identify the functional groups present in the grown material. The luminescence characteristics of grown material were analysed to confirm the effect of metal ion on the ligand. This property makes the material suitable for OLED application. The supercapacitive performance of the grown crystal was finally studied using cyclic voltammetry.

Mono and binuclear ruthenium(II) complexes containing 5-chlorothiophene-2-carboxylic acid ligands: Spectroscopic analysis and computational studies

NASA Astrophysics Data System (ADS)

Swarnalatha, Kalaiyar; Kamalesu, Subramaniam; Subramanian, Ramasamy

2016-11-01

New Ruthenium complexes I, II and III were synthesized using 5-chlorothiophene-2-carboxylic acid (5TPC), as ligand and the complexes were characterized by elemental analysis, FT-IR, 1H, 13C NMR, and mass spectroscopic techniques. Photophysical and electrochemical studies were carried out and the structures of the synthesized complex were optimized using density functional theory (DFT). The molecular geometry, the highest occupied molecular orbital (HOMO), the lowest unoccupied molecular orbital (LUMO) energies and Mulliken atomic charges of the molecules are determined at the B3LYP method and standard 6-311++G (d,p) basis set starting from optimized geometry. They possess excellent stabilities and their thermal decomposition temperatures are 185 °C, 180 °C and 200 °C respectively, indicating that the metal complexes are suitable for the fabrication processes of optoelectronic devices.

Synthesis, characterisation and anion exchange properties of copper, magnesium, zinc and nickel hydroxy nitrates

NASA Astrophysics Data System (ADS)

Biswick, Timothy; Jones, William; Pacuła, Aleksandra; Serwicka, Ewa

2006-01-01

Anion exchange reactions of four structurally related hydroxy salts, Cu 2(OH) 3NO 3, Mg 2(OH) 3NO 3, Ni 2(OH) 3NO 3 and Zn 3(OH) 4(NO 3) 2 are compared and trends rationalised in terms of the strength of the covalent bond between the nitrate group and the matrix cation. Powder X-ray diffraction (PXRD), Fourier-transform infrared (FTIR) spectroscopy, thermogravimetric analysis (TGA) and elemental analysis are used to characterise the materials. Replacement of the nitrate anions in the zinc and copper salts with benzoate anions is possible although exchange of the zinc salt is accompanied by modification of the layer structure from one where zinc is exclusively six-fold coordinated to a structure where there is both six- and four-fold zinc coordination. Magnesium and nickel hydroxy nitrates, on the other hand, hydrolyse to their respective metal hydroxides.

Heterotrophic Bioleaching of Sulfur, Iron, and Silicon Impurities from Coal by Fusarium oxysporum FE and Exophiala spinifera FM with Growing and Resting Cells.

PubMed

Etemadzadeh, Shekoofeh Sadat; Emtiazi, Giti; Etemadifar, Zahra

2016-06-01

Coal is the most abundant fossil fuel containing sulfur and other elements which promote environmental pollution after burning. Also the silicon impurities make the transportation of coal expensive. In this research, two isolated fungi from oil contaminated soil with accessory number KF554100 (Fusarium oxysporum FE) and KC925672 (Exophiala spinifera FM) were used for heterotrophic biological leaching of coal. The leaching were detected by FTIR, CHNS, XRF analyzer and compared with iron and sulfate released in the supernatant. The results showed that E. spinifera FM produced more acidic metabolites in growing cells, promoting the iron and sulfate ions removal while resting cells of F. oxysporum FE enhanced the removal of aromatic sulfur. XRF analysis showed that the resting cells of E. spinifera FM proceeded maximum leaching for iron and silicon (48.8, 43.2 %, respectively). CHNS analysis demonstrated that 34.21 % of sulfur leaching was due to the activities of resting cells of F. oxysporum FE. Also F. oxysporum FE removed organic sulfur more than E. spinifera FM in both growing and resting cells. FTIR data showed that both fungi had the ability to remove pyrite and quartz from coal. These data indicated that inoculations of these fungi to the coal are cheap and impurity removals were faster than autotrophic bacteria. Also due to the removal of dibenzothiophene, pyrite, and quartz, we speculated that they are excellent candidates for bioleaching of coal, oil, and gas.

Structural, optical and electrical properties of WO3-Ag nanocomposites for the electro-optical devices

NASA Astrophysics Data System (ADS)

Najafi-Ashtiani, Hamed; Bahari, Ali; Gholipour, Samira; Hoseinzadeh, Siamak

2018-01-01

The composites of tungsten trioxide and silver are synthesized by sodium tungstate and silver nitrate precursors. The structural properties of composite coatings are studied by FTIR, XRD, and XPS. The FTIR analysis of synthesized composite powder corroborated the bonds between tungsten and oxygen elements in WO3 molecules. Furthermore, the XRD spectra show crystalline nature while particle size analysis that is investigated by X-powder software shows average particle size of 24 and 25 nm for samples. The structural analyses show that the addition of silver dopant does not change the stoichiometry of tungsten trioxide and only increase the size of the aggregation in the films. Furthermore, these films have an average approximate roughness of about 10.7, 13.1 and 14.2 nm for sample 1, 2 and 3, respectively. The real and imaginative parts of permittivity are investigated using LCR meter in the frequency range 1 Hz-10 GHz. The optical spectra of composite coatings are characterized in the 300-900 nm wavelength range and the calculation of optical band gaps of them exhibited the directly allowed transition with the values of 3.8 and 3.85 eV. From UV-visible spectroscopy studies, the absorption coefficient of the composite thin films is determined to be of the order of 105 cm- 1 and the obtained refraction and extinction indexes indicated normal dispersive coatings. Due to their optical and electrical properties, the synthesized composite material is a promising candidate for use in electro-optical applicants.

Biosorption of Microelements by Spirulina: Towards Technology of Mineral Feed Supplements

PubMed Central

Chojnacka, Katarzyna

2014-01-01

Surface characterization and metal ion adsorption properties of Spirulina sp. and Spirulina maxima were verified by various instrumental techniques. FTIR spectroscopy and potentiometric titration were used for qualitative and quantitative determination of metal ion-binding groups. Comparative FTIR spectra of natural and Cu(II)-treated biomass proved involvement of both phosphoryl and sulfone groups in metal ions sorption. The potentiometric titration data analysis provided the best fit with the model assuming the presence of three types of surface functional groups and the carboxyl group as the major binding site. The mechanism of metal ions biosorption was investigated by comparing the results from multielemental analyses by ICP-OES and SEM-EDX. Biosorption of Cu(II), Mn(II), Zn(II), and Co(II) ions by lyophilized Spirulina sp. was performed to determine the metal affinity relationships for single- and multicomponent systems. Obtained results showed the replacement of naturally bound ions: Na(I), K(I), or Ca(II) with sorbed metal ions in a descending order of Mn(II) > Cu(II) > Zn(II) > Co(II) for single- and Cu(II) > Mn(II) > Co(II) > Zn(II) for multicomponent systems, respectively. Surface elemental composition of natural and metal-loaded material was determined both by ICP-OES and SEM-EDX analysis, showing relatively high value of correlation coefficient between the concentration of Na(I) ions in algal biomass. PMID:25386594

Green synthesis of Pd nanoparticles at Apricot kernel shell substrate using Salvia hydrangea extract: Catalytic activity for reduction of organic dyes.

PubMed

Khodadadi, Bahar; Bordbar, Maryam; Nasrollahzadeh, Mahmoud

2017-03-15

For the first time the extract of the plant of Salvia hydrangea was used to green synthesis of Pd nanoparticles (NPs) supported on Apricot kernel shell as an environmentally benign support. The Pd NPs/Apricot kernel shell as an effective catalyst was prepared through reduction of Pd 2+ ions using Salvia hydrangea extract as the reducing and capping agent and Pd NPs immobilization on Apricot kernel shell surface in the absence of any stabilizer or surfactant. According to FT-IR analysis, the hydroxyl groups of phenolics in Salvia hydrangea extract as bioreductant agents are directly responsible for the reduction of Pd 2+ ions and formation of Pd NPs. The as-prepared catalyst was characterized by Fourier transform infrared (FT-IR) and UV-Vis spectroscopy, field emission scanning electron microscopy (FESEM) equipped with an energy dispersive X-ray spectroscopy (EDS), Elemental mapping, X-ray diffraction analysis (XRD) and transmittance electron microscopy (TEM). The synthesized catalyst was used in the reduction of 4-nitrophenol (4-NP), Methyl Orange (MO), Methylene Blue (MB), Rhodamine B (RhB), and Congo Red (CR) at room temperature. The Pd NPs/Apricot kernel shell showed excellent catalytic activity in the reduction of these organic dyes. In addition, it was found that Pd NPs/Apricot kernel shell can be recovered and reused several times without significant loss of catalytic activity. Copyright © 2016 Elsevier Inc. All rights reserved.

Formation of cerussite and hydrocerussite during adsorption of lead from aqueous solution on oxidized carbons by cold oxygen plasma

NASA Astrophysics Data System (ADS)

De Velasco Maldonado, Paola S.; Hernández-Montoya, Virginia; Concheso, A.; Montes-Morán, Miguel A.

2016-11-01

A new procedure of elimination of Pb2+ from aqueous solution using carbon adsorbents, in which high amounts of cerussite and hydrocerussite are deposited on the carbon surfaces, is reported. The procedure includes the preparation of carbons from selected lignocellulosic wastes (pecan nut shells and peach stones) by single carbonization and further oxidation with cold oxygen plasma. The materials prior and after the oxidation treatment were characterized using elemental analysis, FT-IR spectroscopy, SEM/EDX analysis, adsorption of N2 at -196 °C and X-ray photoelectron spectroscopy. The adsorption of Pb2+ was carried out in batch systems under constant agitation. The formation of cerussite and hydrocerussite on the spent carbon surfaces was confirmed by XRD, SEM/EDX and FT-IR. A Pb2+ removal mechanism is proposed in which a co-precipitation of lead nitrate and calcium carbonate would render the formation of the lead carbonates. In such mechanism, the occurrence of CaCO3 on the surface of the adsorbents plays a crucial role. The presence of calcium carbonate on the precursors is understood on the basis of the thermal evolution of calcium oxalate originally present in the biomass. The oxygen plasma treatment helps to expose the calcium carbonate nanocrystals thus improving dramatically the removal capacity of Pb2+. Accordingly, retention capacities as high as 63 mg of Pb2+ per gram of adsorbent have been attained.

Rapid differentiation of Listeria monocytogenes epidemic clones III and IV and their intact compared with heat-killed populations using Fourier transform infrared spectroscopy and chemometrics.

PubMed

Nyarko, Esmond B; Puzey, Kenneth A; Donnelly, Catherine W

2014-06-01

The objectives of this study were to determine if Fourier transform infrared (FT-IR) spectroscopy and multivariate statistical analysis (chemometrics) could be used to rapidly differentiate epidemic clones (ECs) of Listeria monocytogenes, as well as their intact compared with heat-killed populations. FT-IR spectra were collected from dried thin smears on infrared slides prepared from aliquots of 10 μL of each L. monocytogenes ECs (ECIII: J1-101 and R2-499; ECIV: J1-129 and J1-220), and also from intact and heat-killed cell populations of each EC strain using 250 scans at a resolution of 4 cm(-1) in the mid-infrared region in a reflectance mode. Chemometric analysis of spectra involved the application of the multivariate discriminant method for canonical variate analysis (CVA) and linear discriminant analysis (LDA). CVA of the spectra in the wavelength region 4000 to 600 cm(-1) separated the EC strains while LDA resulted in a 100% accurate classification of all spectra in the data set. Further, CVA separated intact and heat-killed cells of each EC strain and there was 100% accuracy in the classification of all spectra when LDA was applied. FT-IR spectral wavenumbers 1650 to 1390 cm(-1) were used to separate heat-killed and intact populations of L. monocytogenes. The FT-IR spectroscopy method allowed discrimination between strains that belong to the same EC. FT-IR is a highly discriminatory and reproducible method that can be used for the rapid subtyping of L. monocytogenes, as well as for the detection of live compared with dead populations of the organism. Fourier transform infrared (FT-IR) spectroscopy and multivariate statistical analysis can be used for L. monocytogenes source tracking and for clinical case isolate comparison during epidemiological investigations since the method is capable of differentiating epidemic clones and it uses a library of well-characterized strains. The FT-IR method is potentially less expensive and more rapid compared to genetic subtyping methods, and can be used for L. monocytogenes strain typing by food industries and public health agencies to enable faster response and intervention to listeriosis outbreaks. FT-IR can also be applied for routine monitoring of the pathogen in food processing plants and for investigating postprocessing contamination because it is capable of differentiating heat-killed and viable L. monocytogenes populations. © 2014 Institute of Food Technologists®

Biocompatibility and Chemical Reaction Kinetics of Injectable, Settable Polyurethane/Allograft Bone Biocomposites

DTIC Science & Technology

2012-08-05

equivalents from the B-MBP [15]. 2.4. ATR-FTIR analysis of the reactivity of individual components ATR-FTIR spectroscopy measurements were conducted...isocyanate (de- scribed in greater detail in the Supplementary Data). The analysis was completed in triplicate (n = 3) for each reaction analyzed...using MetaMorph 7.1 im- age analysis software (MDS Analytical Technologies). The mass of each slice was used to obtain the density, and the measured den

Fourier transform infrared spectroscopy for analysis of kidney stones.

PubMed

Khan, Aysha Habib; Imran, Sheharbano; Talati, Jamsheer; Jafri, Lena

2018-01-01

To compare the results of a chemical method of kidney stone analysis with the results of Fourier transform infrared (FT-IR) spectroscopy. Kidney stones collected between June and October 2015 were simultaneously analyzed by chemical and FT-IR methods. Kidney stones (n=449) were collected from patients from 1 to 81 years old. Most stones were from adults, with only 11.5% from children (aged 3-16 years) and 1.5% from children aged <2 years. The male to female ratio was 4.6. In adults, the calcium oxalate stone type, calcium oxalate monohydrate (COM, n=224), was the most common crystal, followed by uric acid and calcium oxalate dihydrate (COD, n=83). In children, the most frequently occurring type was predominantly COD (n=21), followed by COM (n=11), ammonium urate (n=10), carbonate apatite (n=6), uric acid (n=4), and cystine (n=1). Core composition in 22 stones showed ammonium urate (n=2), COM (n=2), and carbonate apatite (n=1) in five stones, while uric acid crystals were detected (n=13) by FT-IR. While chemical analysis identified 3 stones as uric acid and the rest as calcium oxalate only. Agreement between the two methods was moderate, with a kappa statistic of 0.57 (95% confidence interval, 0.5-0.64). Disagreement was noted in the analysis of 77 stones. FT-IR analysis of kidney stones can overcome many limitations associated with chemical analysis.

FTIR Analysis of Aerogel Keystones from the Stardust Interstellar Dust Collector: Assessment of Terrestrial Organic Contamination and X-Ray Microprobe Beam Damage

NASA Astrophysics Data System (ADS)

Bechtel, H. A.; Allen, C.; Bajt, S.; Borg, J.; Brenker, F.; Bridges, J.; Brownlee, D. E.; Burchell, M.; Burghammer, M.; Butterworth, A. L.; Cloetens, P.; Davis, A. M.; Floss, C.; Flynn, G. J.; Frank, D.; Gainsforth, Z.; Grun, E.; Heck, P. R.; Hillier, J. K.; Hoppe, P.; Howard, L.; Huss, G. R.; Huth, J.; Kearsley, A.; King, A. J.; Lai, B.; Leitner, J.; Lemelle, L.; Leroux, H.; Nittler, L. R.; Ogliore, R. C.; Postberg, F.; Price, M. C.; Sandford, S. A.; Sans Tresseras, J. A.; Schmitz, S.; Schoonjans, T.; Silversmit, G.; Simionovici, A.; Srama, R.; Stadermann, F. J.; Stephan, T.; Stodolna, J.; Stroud, R. M.; Sutton, S. R.; Toucoulou, R.; Trieloff, M.; Tsou, P.; Tsuchiyama, A.; Tyliczszak, T.; Vekemans, B.; Vincze, L.; Westphal, A. J.; Zolensky, M. E.; 29,000 Stardust@Home Dusters

2011-03-01

More than 20 aerogel keystones, many of which contained candidates for interstellar dust, were extracted from the Stardust interstellar dust collector and examined with synchrotron FTIR spectromicroscopy.

Synthesis, characterization, shrinkage and curing kinetics of a new low-shrinkage urethane dimethacrylate monomer for dental applications.

PubMed

Atai, Mohammad; Ahmadi, Mehdi; Babanzadeh, Samal; Watts, David C

2007-08-01

The aim of the study was to synthesize and characterize an isophorone-based urethane dimethacrylate (IP-UDMA) resin-monomer and to investigate its shrinkage and curing kinetics. The IP-UDMA monomer was synthesized through the reaction of polyethylene glycol 400 and isophorone diisocyanate followed by reacting with HEMA to terminate it with methacrylate end groups. The reaction was followed using a standard back titration method and FTIR spectroscopy. The final product was purified and characterized using FTIR, (1)H NMR, elemental analysis and refractive index measurement. The shrinkage-strain of the specimens photopolymerized at circa 700mW/cm(2) was measured using the bonded-disk technique at 23, 35, and 45 degrees C. Initial shrinkage-strain-rates were obtained by numerical differentiation of shrinkage-strain data with respect to time. Degree-of-conversion of the specimens was measured using FTIR spectroscopy. The thermal curing kinetics of the monomer were also studied by differential scanning calorimetry (DSC). The characterization methods confirmed the suggested reaction route and the synthesized monomer. A low shrinkage-strain of about 4% was obtained for the new monomer. The results showed that the shrinkage-strain-rate of the monomer followed the autocatalytic model of Kamal and Sourour [Kamal MR, Sourour S. Kinetic and thermal characterization of thermoset cure. Polym Eng Sci 1973;13(1):59-64], which is used to describe the reaction kinetics of thermoset resins. The model parameters were calculated by linearization of the equation. The model prediction was in a good agreement with the experimental data. The properties of the new monomer compare favorably with properties of the commercially available resins.

Studies the alterations of biochemical and mineral contents in bone tissue of mus musculus due to aluminum toxicity and the protective action of desferrioxamine and deferiprone by FTIR, ICP-OES, SEM and XRD techniques.

PubMed

Sivakumar, S; Khatiwada, Chandra Prasad; Sivasubramanian, J

2014-05-21

The present study has attempt to analyze the changes in the biochemical and mineral contents of aluminum intoxicated bone and determine the protective action of desferrioxamine (DFO) and deferiprone (DFP) by using Fourier transform infrared (FTIR) spectroscopy, X-ray diffraction (XRD), inductively coupled plasma optical emission spectroscopy (ICP-OES), and scanning electron microscopy (SEM) techniques for four groups of animals such as control (Group I), aluminum intoxicated (Group II), Al+DFP (Group III) and Al+DFO+DFP (Group IV) treated groups respectively. The FTIR spectra of the aluminum intoxicated bone showed significant alteration in the biochemical constituents. The bands ratio at I1400/I877 significantly decreased from control to aluminum, but enhanced it by Al+DFP to Al+DFO+DFP treated bone tissue for treatments of 16 weeks. This result suggests that DFO and DFP are the carbonate inhibitor, recovered from chronic growth of bone diseases and pathologies. The alteration of proteins profile indicated by Amide I and Amide II, where peak area values decreased from control to aluminum respectively, but enhanced by treated with DFP (p.o.) and DFO+DFP (i.p.) respectively. The XRD analysis showed a decrease in crystallinity due to aluminum toxicity. Further, the Ca, Mg, and P contents of the aluminum exposed bone were less than those of the control group, and enhanced by treatments with DFO and DFP. The concentrations of trace elements were found by ICP-OES. Therefore, present study suggests that due to aluminum toxicity severe loss of bone minerals, decrease in the biochemical constituents and changes in the surface morphology. Copyright © 2014 Elsevier B.V. All rights reserved.

Comparative evaluation of bioactivity of crystalline trypsin for drying by Fourier-transformed infrared spectroscopy.

PubMed

Otsuka, Makoto; Fukui, Yuya; Ozaki, Yukihiro

2009-03-01

The purpose of this study was to evaluate the enzymatic stability of colloidal trypsin powder during heating in a solid-state by using Fourier transform infrared (FT-IR) spectra with chemoinformatics and generalized two-dimensional (2D) correlation spectroscopy. Colloidal crystalline trypsin powders were heated using differential scanning calorimetry. The enzymatic activity of trypsin was assayed by the kinetic degradation method. Spectra of 10 calibration sample sets were recorded three times with a FT-IR spectrometer. The maximum intensity at 1634cm(-1) of FT-IR spectra and enzymatic activity of trypsin decreased as the temperature increased. The FT-IR spectra of trypsin samples were analyzed by a principal component regression analysis (PCR). A plot of the calibration data obtained was made between the actual and predicted trypsin activity based on a two-component model with gamma(2)=0.962. On the other hand, a 2D method was applied to FT-IR spectra of heat-treated trypsin. The result was consistent with that of the chemoinformetrical method. The results for deactivation of colloidal trypsin powder by heat-treatment indicated that nano-structure of crystalline trypsin changed by heating reflecting that the beta-sheet was mainly transformed, since the peak at 1634cm(-1) decreased with dehydration. The FT-IR chemoinformetrical method allows for a solid-state quantitative analysis of the bioactivity of the bulk powder of trypsin during drying.

Application of Fourier-transform infrared (FT-IR) spectroscopy for simple and easy determination of chylomicron-triglyceride and very low density lipoprotein-triglyceride.

PubMed

Sato, Kenichi; Seimiya, Masanori; Kodera, Yoshio; Kitamura, Akihide; Nomura, Fumio

2010-02-01

Fourier-transform infrared (FT-IR) spectroscopy is a simple and reagent-free physicochemical analysis method, and is a potential alternative to more time-consuming and labor-intensive procedures. In this study, we aimed to use FT-IR spectroscopy to determine serum concentrations of chylomicron-triglyceride (TG) and very low density lipoprotein (VLDL)-TG. We analyzed a chylomicron fraction and VLDL fraction, which had been obtained by ultracentrifugation, to search for wavelengths to designate to each fraction. Then, partial least square (PLS) calibrations were developed using a training set of samples, for which TG concentrations had been determined by conventional procedures. Validation was conducted with another set of samples using the PLS model to predict serum TG concentrations on the basis of the samples' IR spectra. We analyzed a total of 150 samples. Serum concentrations of chylomicron-TG and VLDL-TG estimated by FT-IR spectroscopy agreed well with those obtained by the reference method (r=0.97 for both lipoprotein fractions). FT-IR spectrometric analysis required 15mul of serum and was completed within 1min. Serum chylomicron-TG and VLDL-TG concentrations can be determined with FT-IR spectroscopy. This rapid and simple test may have a great impact on the management of patients with dyslipidemia. Copyright 2009. Published by Elsevier B.V.

Thermal Cracking to Improve the Qualification of the Waxes

NASA Astrophysics Data System (ADS)

He, B.; Agblevor, F. A.; Chen, C. G.; Feng, J.

2018-05-01

Thermal cracking of waxes at mild conditions (430-500°C) has been reconsidered as a possible refining technology for the production of fuels and chemicals. In this study, the more moderate thermal cracking was investigated to process Uinta Basin soft waxes to achieve the required pour point so that they can be pumped to the refineries. The best thermal cracking conditions were set 420°C and 20 minutes. The viscosity and density of the final liquid product were respectively achieved as 2.63 mP•s and 0.784 g/cm3 at 40°C. The result of FT-IR analysis of the liquid product indicated that the unsaturated hydrocarbons were produced after thermal cracking, which was corroborated by the 13C NMR spectrum. The GC analysis of the final gas product indicated that the hydrogen was produced; the dehydrogenation reaction was also proved by the elemental analysis and HHV results. The pour point of the final liquid product met the requirement.

Isolation and chemical analysis of nanoparticles from English ivy (Hedera helix L.)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lenaghan, Scott C; Burris, Jason N; Chourey, Karuna

It was discovered that adventitious roots of English ivy secreted a high strength adhesive containing uniform nanoparticles. These nanoparticles were hypothesized to be organic in nature. Subsequent studies have revealed several applications for these nanoparticles, but their chemical composition remained unknown. Here, we describe an isolation procedure to obtain gram quantities of ivy nanoparticles from adventitious roots. In addition, ultraviolet/visible (UV/Vis) spectroscopy, inductively coupled plasma mass spectrometry (ICP-MS), elemental analysis, fourier transform infrared spectroscopy (FTIR), and gel electrophoresis were conducted to identify the chemical nature of the ivy nanoparticles. Based on this comprehensive analysis, we conclude that the ivy nanoparticlesmore » are proteinaceous consisting of 51.77% carbon, 4.72% nitrogen, and 0.32% sulfur, without the presence of metals. Liquid chromatography tandem mass spectrometry (LC-MS/MS) based protein profiling revealed the presence of at least 6 proteins, including heat shock proteins and other large molecular weight proteins. Identification of these protein candidates will facilitate gene discovery and bioproduction of ivy nanoparticles.« less

Synthesis, crystal growth and characterization of a phase matchable nonlinear optical single crystal: p-chloro dibenzylideneacetone

NASA Astrophysics Data System (ADS)

Ravindra, H. J.; John Kiran, A.; Nooji, Satheesha Rai; Dharmaprakash, S. M.; Chandrasekharan, K.; Kalluraya, Balakrishna; Rotermund, Fabian

2008-05-01

Good quality single crystals of p-chloro dibenzylideneacetone (CDBA) of size 13 mm×8 mm×2 mm were grown by slow evaporation solution growth technique. The grown crystals were confirmed by elemental analysis, Fourier transform infrared (FTIR) analysis and single crystal X-ray diffraction techniques. From the thermo gravimetric/differential thermal (TG/DT) analysis, the CDBA was found to be thermally stable up to 250 °C. The mechanical stability of the crystal is comparable with that of the other reported chalcones. The lower optical cut-off wavelength for this crystal was observed at 440 nm. The laser damage threshold of the crystal was 0.6 GW/cm 2 at 532 nm. The second harmonic generation conversion efficiency of the powder sample of CDBA was found to be 4.5 times greater than that of urea. We also demonstrate the existence of the phase matching property in this crystal using Kurtz powder technique.

Investigation of Magnetic Properties and Mechanical Responses on Hydrogel-TMAH-Magnetite

NASA Astrophysics Data System (ADS)

Sunaryono; Hidayat, M. F.; Insjaf, C.; Taufiq, A.; Mufti, N.; Munasir

2018-05-01

Hydrogel-TMAH-Magnetite (ferrogel) was fabricated by using polyvinyl alcohol (PVA) hydrogel and magnetite fluids with tetramethylammonium hydroxide (TMAH) surfactant. Iron sand as the raw material was used to synthesize magnetite nanoparticles by co-precipitation method. Magnetite nanoparticles and ferrogel were characterized using X-Ray Fluorescence (XRF) to determine the content of elements in it. To know the functional group network of magnetite nanoparticles, magnetite enclosed with TMAH and ferrogel; we investigated using Fourier Transform Infra-Red (FTIR). Meanwhile, the magnetic properties of the hydrogel-TMAH-magnetite were measured by using Vibrating Sample Magnetometer (VSM). Furthermore, the composition analysis of the ferrogels using FTIR showed that all the synthesis materials were inside the ferrogels. The saturation magnetization of the hydrogel-TMAH-magnetite with a composition of TMAH 1.2 mL (3.95 emu·g-1) was higher than that of TMAH 0.8 mL (0.85 emu·g-1). It exhibited that the composition of TMAH 1.2 mL was an optimum composition to produce nanoparticle magnetite-TMAH having a stable and high performance. Furthermore, the magneto-elasticity of hydrogel-TMAH-magnetite in the effect of the external magnetic field had a good response. However, the composition of the nanoparticle magnetite-TMAH in the ferrogel did not significantly affect the elongation of the gel.

Novel Organically Modified Core-Shell Clay for Epoxy Composites-"SOBM Filler 1".

PubMed

Iheaturu, Nnamdi Chibuike; Madufor, Innocent Chimezie

2014-01-01

Preparation of a novel organically modified clay from spent oil base drilling mud (SOBM) that could serve as core-shell clay filler for polymers is herein reported. Due to the hydrophilic nature of clay, its compatibility with polymer matrix was made possible through modification of the surface of the core clay sample with 3-aminopropyltriethoxysilane (3-APTES) compound prior to its use. Fourier transform infrared (FT-IR) spectroscopy was used to characterize clay surface modification. Electron dispersive X-ray diffraction (EDX) and scanning electron microscopy (SEM) were used to expose filler chemical composition and morphology, while electrophoresis measurement was used to examine level of filler dispersion. Results show an agglomerated core clay powder after high temperature treatment, while EDX analysis shows that the organically modified clay is composed of chemical inhomogeneities, wherein elemental compositions in weight percent vary from one point to the other in a probe of two points. Micrographs of the 3-APTES coupled SOBM core-shell clay filler clearly show cloudy appearance, while FT-IR indicates 25% and 5% increases in fundamental vibrations band at 1014 cm(-1) and 1435 cm(-1), respectively. Furthermore, 3-APTES coupled core-shell clay was used to prepare epoxy composites and tested for mechanical properties.

Modification of bamboo-based activated carbon using microwave radiation and its effects on the adsorption of methylene blue

NASA Astrophysics Data System (ADS)

Liu, Qing-Song; Zheng, Tong; Li, Nan; Wang, Peng; Abulikemu, Gulizhaer

2010-03-01

Modification of bamboo-based activated carbon was carried out in a microwave oven under N 2 atmosphere. The virgin and modified activated carbons were characterized by means of low temperature N 2 adsorption, acid-base titration, point of zero charge (pH pzc) measurement, FTIR and XPS spectra. A gradual decrease in the surface acidic groups was observed during the modification, while the surface basicity was enhanced to some extent, which gave rise to an increase in the pH pzc value. The species of the functional groups and relative content of various elements and groups were given further analysis using FTIR and XPS spectra. An increase in the micropores was found at the start, and the micropores were then extended into larger ones, resulting in an increase in the pore volume and average pore size. Adsorption studies showed enhanced adsorption of methylene blue on the modified activated carbons, caused mainly by the enlargement of the micropores. Adsorption isotherm fittings revealed that Langmuir and Freundlich models were applicable for the virgin and modified activated carbons, respectively. Kinetic studies exhibited faster adsorption rate of methylene blue on the modified activated carbons, and the pseudo-second-order model fitted well for all of the activated carbons.

Novel Organically Modified Core-Shell Clay for Epoxy Composites—“SOBM Filler 1”

PubMed Central

Iheaturu, Nnamdi Chibuike; Madufor, Innocent Chimezie

2014-01-01

Preparation of a novel organically modified clay from spent oil base drilling mud (SOBM) that could serve as core-shell clay filler for polymers is herein reported. Due to the hydrophilic nature of clay, its compatibility with polymer matrix was made possible through modification of the surface of the core clay sample with 3-aminopropyltriethoxysilane (3-APTES) compound prior to its use. Fourier transform infrared (FT-IR) spectroscopy was used to characterize clay surface modification. Electron dispersive X-ray diffraction (EDX) and scanning electron microscopy (SEM) were used to expose filler chemical composition and morphology, while electrophoresis measurement was used to examine level of filler dispersion. Results show an agglomerated core clay powder after high temperature treatment, while EDX analysis shows that the organically modified clay is composed of chemical inhomogeneities, wherein elemental compositions in weight percent vary from one point to the other in a probe of two points. Micrographs of the 3-APTES coupled SOBM core-shell clay filler clearly show cloudy appearance, while FT-IR indicates 25% and 5% increases in fundamental vibrations band at 1014 cm−1 and 1435 cm−1, respectively. Furthermore, 3-APTES coupled core-shell clay was used to prepare epoxy composites and tested for mechanical properties. PMID:27355022

Mild and modular surface modification of cellulose via hetero Diels-Alder (HDA) cycloaddition.

PubMed

Goldmann, Anja S; Tischer, Thomas; Barner, Leonie; Bruns, Michael; Barner-Kowollik, Christopher

2011-04-11

A combination of reversible addition-fragmentation chain transfer (RAFT) polymerization and hetero Diels-Alder (HDA) cycloaddition was used to effect, under mild (T ≈ 20 °C), fast, and modular conditions, the grafting of poly(isobornyl acrylate) (M(n) = 9800 g mol(-1), PDI = 1.19) onto a solid cellulose substrate. The active hydroxyl groups expressed on the cellulose fibers were converted to tosylate leaving groups, which were subsequently substituted by a highly reactive cyclopentadienyl functionality (Cp). By employing the reactive Cp-functionality as a diene, thiocarbonyl thio-capped poly(isobornyl acrylate) synthesized via RAFT polymerization (mediated by benzyl pyridine-2-yldithioformiate (BPDF)) was attached to the surface under ambient conditions by an HDA cycloaddition (reaction time: 15 h). The surface-modified cellulose samples were analyzed in-depth by X-ray photoelectron spectroscopy, scanning electron microscopy, elemental analysis, Fourier transform infrared (FT-IR) spectroscopy as well as Fourier transform infrared microscopy employing a focal plane array detector for imaging purposes. The analytical results provide strong evidence that the reaction of suitable dienophiles with Cp-functional cellulose proceeds under mild reaction conditions (T ≈ 20 °C) in an efficient fashion. In particular, the visualization of individual modified cellulose fibers via high-resolution FT-IR microscopy corroborates the homogeneous distribution of the polymer film on the cellulose fibers.

Application of Fourier transform infrared spectroscopy and chemometrics for differentiation of Salmonella enterica serovar Enteritidis phage types.

PubMed

Preisner, Ornella; Guiomar, Raquel; Machado, Jorge; Menezes, José Cardoso; Lopes, João Almeida

2010-06-01

Fourier transform infrared (FT-IR) spectroscopy and chemometric techniques were used to discriminate five closely related Salmonella enterica serotype Enteritidis phage types, phage type 1 (PT1), PT1b, PT4b, PT6, and PT6a. Intact cells and outer membrane protein (OMP) extracts from bacterial cell membranes were subjected to FT-IR analysis in transmittance mode. Spectra were collected over a wavenumber range from 4,000 to 600 cm(-1). Partial least-squares discriminant analysis (PLS-DA) was used to develop calibration models based on preprocessed FT-IR spectra. The analysis based on OMP extracts provided greater separation between the Salmonella Enteritidis PT1-PT1b, PT4b, and PT6-PT6a groups than the intact cell analysis. When these three phage type groups were considered, the method based on OMP extract FT-IR spectra was 100% accurate. Moreover, complementary local models that considered only the PT1-PT1b and PT6-PT6a groups were developed, and the level of discrimination increased. PT1 and PT1b isolates were differentiated successfully with the local model using the entire OMP extract spectrum (98.3% correct predictions), whereas the accuracy of discrimination between PT6 and PT6a isolates was 86.0%. Isolates belonging to different phage types (PT19, PT20, and PT21) were used with the model to test its robustness. For the first time it was demonstrated that FT-IR analysis of OMP extracts can be used for construction of robust models that allow fast and accurate discrimination of different Salmonella Enteritidis phage types.

Attenuated total reflectance-FT-IR spectroscopy for gunshot residue analysis: potential for ammunition determination.

PubMed

Bueno, Justin; Sikirzhytski, Vitali; Lednev, Igor K

2013-08-06

The ability to link a suspect to a particular shooting incident is a principal task for many forensic investigators. Here, we attempt to achieve this goal by analysis of gunshot residue (GSR) through the use of attenuated total reflectance (ATR) Fourier transform infrared spectroscopy (FT-IR) combined with statistical analysis. The firearm discharge process is analogous to a complex chemical process. Therefore, the products of this process (GSR) will vary based upon numerous factors, including the specific combination of the firearm and ammunition which was discharged. Differentiation of FT-IR data, collected from GSR particles originating from three different firearm-ammunition combinations (0.38 in., 0.40 in., and 9 mm calibers), was achieved using projection to latent structures discriminant analysis (PLS-DA). The technique was cross (leave-one-out), both internally and externally, validated. External validation was achieved via assignment (caliber identification) of unknown FT-IR spectra from unknown GSR particles. The results demonstrate great potential for ATR-FT-IR spectroscopic analysis of GSR for forensic purposes.

Application of Fourier transform infrared spectroscopy to biomolecular profiling of cultured fibroblast cells from Gaucher disease patients: A preliminary investigation.

PubMed

Igci, Nasit; Sharafi, Parisa; Demiralp, Duygu Ozel; Demiralp, Cemil Ozerk; Yuce, Aysel; Emre, Serap Dokmeci

2017-10-01

Gaucher disease (GD) is defined as an autosomal recessive disorder resulting from the deficiency of glucocerebrosidase (E.C. 3.2.1.45). Glucocerebrosidase is responsible for the degradation of glucosylceramide into ceramide and glucose. The deficiency of this enzyme results in the accumulation of undegraded glucosylceramide, almost exclusively in macrophages. With Fourier transform infrared (FTIR) spectroscopy, the complete molecular diversity of the samples can be studied comparatively and the amount of the particular materials can be determined. Also, the secondary structure ratios of proteins can be determined by analysing the amide peaks. The primary aim of this study is to introduce FTIR-ATR spectroscopy technique to GD research for the first time in the literature and to assess its potential as a new molecular method. Primary fibroblast cell cultures obtained from biopsy samples were used, since this material is widely used for the diagnosis of GD. Intact cells were placed onto a FTIR-ATR crystal and dried by purging nitrogen gas. Spectra were recorded in the mid-infrared region between 4500-850 cm-1 wavenumbers. Each peak in the spectra was assigned to as organic biomolecules according to their chemical bond information. A quantitative analysis was performed using peak areas and we also used a hierarchical cluster analysis as a multivariate spectral analysis. We obtained FTIR spectra of fibroblast samples and assigned the biomolecule origins of the peaks. We observed individual heterogeneity in FTIR spectra of GD fibroblast samples, confirming the well-known phenotypic heterogeneity in GD at the molecular level. Significant alterations in protein, lipid and carbohydrate levels related to the enzyme replacement therapy were also observed, which is also supported by cluster analysis. Our results showed that the application of FTIR spectroscopy to GD research deserves more attention and detailed studies with an increased sample size in order to evaluate its potential in the diagnosis and follow-up of GD patients.

Fourier Transform Infrared Spectroscopy (FT-IR) and Simple Algorithm Analysis for Rapid and Non-Destructive Assessment of Developmental Cotton Fibers.

PubMed

Liu, Yongliang; Kim, Hee-Jin

2017-06-22

With cotton fiber growth or maturation, cellulose content in cotton fibers markedly increases. Traditional chemical methods have been developed to determine cellulose content, but it is time-consuming and labor-intensive, mostly owing to the slow hydrolysis process of fiber cellulose components. As one approach, the attenuated total reflection Fourier transform infrared (ATR FT-IR) spectroscopy technique has also been utilized to monitor cotton cellulose formation, by implementing various spectral interpretation strategies of both multivariate principal component analysis (PCA) and 1-, 2- or 3-band/-variable intensity or intensity ratios. The main objective of this study was to compare the correlations between cellulose content determined by chemical analysis and ATR FT-IR spectral indices acquired by the reported procedures, among developmental Texas Marker-1 (TM-1) and immature fiber ( im ) mutant cotton fibers. It was observed that the R value, CI IR , and the integrated intensity of the 895 cm -1 band exhibited strong and linear relationships with cellulose content. The results have demonstrated the suitability and utility of ATR FT-IR spectroscopy, combined with a simple algorithm analysis, in assessing cotton fiber cellulose content, maturity, and crystallinity in a manner which is rapid, routine, and non-destructive.

Isolation and characterization of microcrystalline cellulose from roselle fibers.

PubMed

Kian, Lau Kia; Jawaid, Mohammad; Ariffin, Hidayah; Alothman, Othman Y

2017-10-01

In this study, microcrystalline cellulose (MCC) was extracted from roselle fiber through acid hydrolysis treatment and its properties were compared with those of commercially available MCC. The physicochemical and morphological characteristics, elemental composition, size distribution, crystallinity and thermal properties of the obtained MCC were analyzed in this work. Fourier transform infrared spectroscopy (FTIR) analysis provided clear evidence that the characteristic peak of lignin was absent in the spectrum of the MCC prepared from roselle fiber. Rough surface and slight aggregation of MCC were observed by scanning electron microscopy (SEM). Energy dispersive X-ray (EDX) analysis showed that pure MCC with small quantities of residues and impurities was obtained, with a similar elemental composition to that of commercial MCC. A mean diameter of approximately 44.28μm was measured for MCC by using a particle size analyzer (PSA). X-ray diffraction (XRD) showed the crystallinity increased from 63% in roselle pulp to 78% in roselle MCC, the latter having a slightly higher crystallinity than that of commercial MCC (74%). TGA and DSC results indicated that the roselle MCC had better thermal stability than the roselle pulp, whereas it had poorer thermal stability in comparison with commercial MCC. Thus, the isolated MCC from roselle fibers will be going to use as reinforcing element in green composites and may be a precursor for future roselle derived nanocellulose, and thus a promising subject in nanocomposite research. Copyright © 2017 Elsevier B.V. All rights reserved.

Discrimination of edible oils and fats by combination of multivariate pattern recognition and FT-IR spectroscopy: A comparative study between different modeling methods

NASA Astrophysics Data System (ADS)

Javidnia, Katayoun; Parish, Maryam; Karimi, Sadegh; Hemmateenejad, Bahram

2013-03-01

By using FT-IR spectroscopy, many researchers from different disciplines enrich the experimental complexity of their research for obtaining more precise information. Moreover chemometrics techniques have boosted the use of IR instruments. In the present study we aimed to emphasize on the power of FT-IR spectroscopy for discrimination between different oil samples (especially fat from vegetable oils). Also our data were used to compare the performance of different classification methods. FT-IR transmittance spectra of oil samples (Corn, Colona, Sunflower, Soya, Olive, and Butter) were measured in the wave-number interval of 450-4000 cm-1. Classification analysis was performed utilizing PLS-DA, interval PLS-DA, extended canonical variate analysis (ECVA) and interval ECVA methods. The effect of data preprocessing by extended multiplicative signal correction was investigated. Whilst all employed method could distinguish butter from vegetable oils, iECVA resulted in the best performances for calibration and external test set with 100% sensitivity and specificity.

In-situ chemical analyses of trans-polyisoprene by histochemical staining and Fourier transform infrared microspectroscopy in a rubber-producing plant, Eucommia ulmoides Oliver.

PubMed

Bamba, Takeshi; Fukusaki, Ei-Ichiro; Nakazawa, Yoshihisa; Kobayashi, Akio

2002-10-01

The localization of polyisoprene in young stem tissues of Eucommia ulmoides Oliver was investigated by histochemical staining and Fourier transform infrared (FT-IR) microspectroscopy. The fibrous structures were stained with Oil Red O. FT-IR microspectroscopic analysis proved that the fibrous structures were trans-polyisoprene. Granular structures stained with the dye, and characteristic absorptions at 2,960 cm(-1) and 1,430 cm(-1) in FT-IR suggested that trans-polyisoprene accumulated in the vicinity of the cambium layer. We have thus successfully shown for the first time the localization of trans-polyisoprene in plant tissues, and our histological investigation allowed us to presume the main sites of biosynthesis and accumulation of trans-rubber. Furthermore, a new technical approach, the preparation of sections using an electronic freezing unit and the in situ analysis of polyisoprene using FT-IR microspectroscopy, is demonstrated to be a promising method for determining the accumulation of polyisoprene as well as other metabolites.

Air Contamination Quantification by FTIR with Gas Cell

NASA Technical Reports Server (NTRS)

Freischlag, Jason

2017-01-01

Air quality is of utmost importance in environmental studies and has many industrial applications such as aviators grade breathing oxygen (ABO) for pilots and breathing air for fire fighters. Contamination is a major concern for these industries as identified in MIL-PRF-27210, CGA G-4.3, CGA G-7.1, and NFPA 1989. Fourier Transform Infrared Spectroscopy (FTIR) is a powerful tool that when combined with a gas cell has tremendous potential for gas contamination analysis. Current procedures focus mostly on GC-MS for contamination quantification. Introduction of this topic will be done through a comparison of the currently used deterministic methods for gas contamination with those of FTIR gas analysis. Certification of the mentioned standards through the ISOIEC 17065 certifying body A2LA will be addressed followed by an evaluation of quality information such as the determinations of linearity and the limits of detection and quantitation. Major interferences and issues arising from the use of the FTIR for accredited work with ABO and breathing air will be covered.

Step-Scan T-Cell Fourier Transform Infrared Photoacoustic Spectroscopy (FTIR-PAS) for Monitoring Environmental Air Pollutants

NASA Astrophysics Data System (ADS)

Liu, Lixian; Mandelis, Andreas; Melnikov, Alexander; Michaelian, Kirk; Huan, Huiting; Haisch, Christoph

2016-07-01

Air pollutants have adverse effects on the Earth's climate system. There is an urgent need for cost-effective devices capable of recognizing and detecting various ambient pollutants. An FTIR photoacoustic spectroscopy (FTIR-PAS) method based on a commercial FTIR spectrometer developed for air contamination monitoring will be presented. A resonant T-cell was determined to be the most appropriate resonator in view of the low-frequency requirement and space limitations in the sample compartment. Step-scan FTIR-PAS theory for regular cylinder resonator has been described as a reference for prediction of T-cell vibration principles. Both simulated amplitude and phase responses of the T-cell show good agreement with measurement data Carbon dioxide IR absorption spectra were used to demonstrate the capacity of the FTIR-PAS method to detect ambient pollutants. The theoretical detection limit for carbon dioxide was found to be 4 ppmv. A linear response to carbon dioxide concentration was found in the range from 2500 ppmv to 5000 ppmv. The results indicate that it is possible to use step-scan FTIR-PAS with a T-cell as a quantitative method for analysis of ambient contaminants.

Antimicrobial Applications of Transition Metal Complexes of Benzothiazole Based Terpolymer: Synthesis, Characterization, and Effect on Bacterial and Fungal Strains

PubMed Central

Riswan Ahamed, Mohamed A.; Azarudeen, Raja S.; Kani, N. Mujafar

2014-01-01

Terpolymer of 2-amino-6-nitro-benzothiazole-ethylenediamine-formaldehyde (BEF) has been synthesized and characterized by elemental analysis and various spectral techniques like FTIR, UV-Visible, and 1H and 13C-NMR. The terpolymer metal complexes were prepared with Cu2+, Ni2+, and Zn2+ metal ions using BEF terpolymer as a ligand. The complexes have been characterized by elemental analysis and IR, UV-Visible, ESR, 1H-NMR, and 13C-NMR spectral studies. Gel permeation chromatography was used to determine the molecular weight of the ligand. The surface features and crystalline behavior of the ligand and its complexes were analyzed by scanning electron microscope and X-ray diffraction methods. Thermogravimetric analysis was used to analyze the thermal stability of the ligand and its metal complexes. Kinetic parameters such as activation energy (E a) and order of reaction (n) and thermodynamic parameters, namely, ΔS, ΔF, S*, and Z, were calculated using Freeman-Carroll (FC), Sharp-Wentworth (SW), and Phadnis-Deshpande (PD) methods. Thermal degradation model of the terpolymer and its metal complexes was also proposed using PD method. Biological activities of the ligand and its complexes were tested against Shigella sonnei, Escherichia coli, Klebsiella species, Staphylococcus aureus, Bacillus subtilis, and Salmonella typhimurium bacteria and Aspergillus flavus, Aspergillus niger, Penicillium species, Candida albicans, Cryptococcus neoformans, Mucor species fungi. PMID:25298760

The use of novel biodegradable, optically active and nanostructured poly(amide-ester-imide) as a polymer matrix for preparation of modified ZnO based bionanocomposites

DOE Office of Scientific and Technical Information (OSTI.GOV)

Abdolmaleki, Amir, E-mail: abdolmaleki@cc.iut.ac.ir; Nanotechnology and Advanced Materials Institute, Isfahan University of Technology, Isfahan 84156-83111, Islamic Republic of Iran; Mallakpour, Shadpour, E-mail: mallak@cc.iut.ac.ir

Highlights: Black-Right-Pointing-Pointer A novel biodegradable and nanostructured PAEI based on two amino acids, was synthesized. Black-Right-Pointing-Pointer ZnO nanoparticles were modified via two different silane coupling agents. Black-Right-Pointing-Pointer PAEI/modified ZnO BNCs were synthesized through ultrasound irradiation. Black-Right-Pointing-Pointer ZnO particles were dispersed homogeneously in PAEI matrix on nanoscale. Black-Right-Pointing-Pointer The effect of ZnO nanoparticles on the properties of synthesized polymer was examined. -- Abstract: A novel biodegradable and nanostructured poly(amide-ester-imide) (PAEI) based on two different amino acids, was synthesized via direct polycondensation of biodegradable N,N Prime -bis[2-(methyl-3-(4-hydroxyphenyl)propanoate)]isophthaldiamide and N,N Prime -(pyromellitoyl)-bis-L-phenylalanine diacid. The resulting polymer was characterized by FT-IR, {sup 1}H NMR,more » specific rotation, elemental analysis, thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), X-ray diffraction (XRD) and field emission scanning electron microscopy (FE-SEM) analysis. The synthesized polymer showed good thermal stability with nano and sphere structure. Then PAEI/ZnO bionanocomposites (BNCs) were fabricated via interaction of pure PAEI and ZnO nanoparticles. The surface of ZnO was modified with two different silane coupling agents. PAEI/ZnO BNCs were studied and characterized by FT-IR, XRD, UV/vis, FE-SEM and TEM. The TEM and FE-SEM results indicated that the nanoparticles were dispersed homogeneously in PAEI matrix on nanoscale. Furthermore the effect of ZnO nanoparticle on the thermal stability of the polymer was investigated with TGA and DSC technique.« less

Synthesis of polyimides from α,αʹ-bis(3-aminophenoxy)-p-xylene: Spectroscopic, single crystal XRD and thermal studies

NASA Astrophysics Data System (ADS)

Ashraf, Ahmad Raza; Akhter, Zareen; Simon, Leonardo C.; McKee, Vickie; Castel, Charles Dal

2018-05-01

The meta-catenated ether-based diamine monomer α,αʹ-bis(3-aminophenoxy)-p-xylene (3APX) was synthesized from dinitro precursor α,αʹ-bis(3-nitrophenoxy)-p-xylene (3NPX). FTIR, 1H and 13C NMR spectroscopic studies accompanied by elemental analysis were performed for structural elucidations of 3NPX and 3APX. The spatial orientations of 3APX were explored by single crystal X-ray diffraction analysis. Its crystal system was found to be monoclinic, adopting the space group P21/c. The synthesized diamine monomer (3APX) was used for preparation of new series of polyimides by reacting with three different dianhydrides (BTDA, ODPA, 6FDA). The relevant copolyimides were developed via incorporation of 4,4ʹ-methylenedianiline (MDA) in the backbone of afore-synthesized polyimides. The structures of polyimides and copolyimides were verified by FTIR and 1H NMR spectroscopic techniques. Their properties were evaluated by dynamic and isothermal TGA (nitrogen and air atmospheres) and WAXRD studies. Polyimides displayed significantly high thermal stability as their degradation started around 400 °C and it was improved further by execution of copolymerization strategy with MDA. The 5% weight loss temperature (T5) of polyimides under nitrogen atmosphere was in the range of 425-460 °C while for copolyimides it increased to 454-498 °C. Thermal decomposition in air was slower than nitrogen between 400 and 550 °C however it was accelerated above 550 °C. Isothermal TGA disclosed that copolyimides have the ability to endure elevated temperatures for extended period. WAXRD analysis showed the amorphous nature of polyimides and copolyimides.

A study of Ganoderma lucidum spores by FTIR microspectroscopy

NASA Astrophysics Data System (ADS)

Wang, Xin; Chen, Xianliang; Qi, Zeming; Liu, Xingcun; Li, Weizu; Wang, Shengyi

2012-06-01

In order to obtain unique information of Ganoderma lucidum spores, FTIR microspectroscopy was used to study G. lucidum spores from Anhui Province (A), Liaoning Province (B) and Shangdong Province (C) of China. IR micro-spectra were acquired with high-resolution and well-reproducibility. The IR spectra of G. lucidum spores from different areas were similar and mainly made up of the absorption bands of polysaccharide, sterols, proteins, fatty acids, etc. The results of curve fitting indicated the protein secondary structures were dissimilar among the above G. lucidum spores. To identify G. lucidum spores from different areas, the H1078/H1640 value might be a potentially useful factor, furthermore FTIR microspectroscopy could realize this identification efficiently with the help of hierarchical cluster analysis. The result indicates FTIR microspectroscopy is an efficient tool for identification of G. lucidum spores from different areas. The result also suggests FTIR microspectroscopy is a potentially useful tool for the study of TCM.

2D FTIR correlation spectroscopy and EPR analysis of Urtica dioica leaves from areas of different environmental pollution

NASA Astrophysics Data System (ADS)

Moskal, Paulina; Wesełucha-Birczyńska, Aleksandra; Łabanowska, Maria; Kurdziel, Magdalena; Filek, Maria

2018-01-01

Leaves of Urtica dioica collected from two areas of different environmental pollution were analysed by fourier transform infrared spectroscopy (FTIR) and electron paramagnetic resonance (EPR) spectroscopy. Analysis of FTIR spectra allows to describe main component of plant like proteins, lipids and carbohydrates. Although the FTIR spectra of plants from these two geographical locations of different environmental pollution appear to be relatively similar, 2D correlation shows completely different patterns. Synchronous and asynchronous correlation maps showed sequences of changes occurring during development of plant, manly in Amide I and Amide II, lignin, lipids and cellulose. In addition, 2D analysis revealed another sequence of changes as the function of plant growth depending on the degree of the environmental pollution. Two various kinds of paramagnetic species, transition metal ions (Mn(II), Fe(III)) and stable organic radicals (chlorophyll, semiquinone, tyrosyl and carbon centered) were found in leaves of nettle collected at different stages of development and growing in clean and polluted environment. In plants growing in polluted area the injuries of protein molecules bonding metal ions and the disturbances of photosynthesis and redox equilibrium in cells, as well as instability of polysaccharide structure of cell walls were observed.

DSC, X-ray and FTIR studies of a gemfibrozil/dimethyl-β-cyclodextrin inclusion complex produced by co-grinding.

PubMed

Aigner, Z; Berkesi, O; Farkas, G; Szabó-Révész, P

2012-01-05

The steps of formation of an inclusion complex produced by the co-grinding of gemfibrozil and dimethyl-β-cyclodextrin were investigated by differential scanning calorimetry (DSC), X-ray powder diffractometry (XRPD) and Fourier transform infrared (FTIR) spectroscopy with curve-fitting analysis. The endothermic peak at 59.25°C reflecting the melting of gemfibrozil progressively disappeared from the DSC curves of the products on increase of the duration of co-grinding. The crystallinity of the samples too gradually decreased, and after 35min of co-grinding the product was totally amorphous. Up to this co-grinding time, XRPD and FTIR investigations indicated a linear correlation between the cyclodextrin complexation and the co-grinding time. After co-grinding for 30min, the ratio of complex formation did not increase. These studies demonstrated that co-grinding is a suitable method for the complexation of gemfibrozil with dimethyl-β-cyclodextrin. XRPD analysis revealed the amorphous state of the gemfibrozil-dimethyl-β-cyclodextrin product. FTIR spectroscopy with curve-fitting analysis may be useful as a semiquantitative analytical method for discriminating the molecular and amorphous states of gemfibrozil. Copyright © 2011 Elsevier B.V. All rights reserved.

Fourier transform infrared spectroscopy combined with chemometrics for discrimination of Curcuma longa, Curcuma xanthorrhiza and Zingiber cassumunar

NASA Astrophysics Data System (ADS)

Rohaeti, Eti; Rafi, Mohamad; Syafitri, Utami Dyah; Heryanto, Rudi

2015-02-01

Turmeric (Curcuma longa), java turmeric (Curcuma xanthorrhiza) and cassumunar ginger (Zingiber cassumunar) are widely used in traditional Indonesian medicines (jamu). They have similar color for their rhizome and possess some similar uses, so it is possible to substitute one for the other. The identification and discrimination of these closely-related plants is a crucial task to ensure the quality of the raw materials. Therefore, an analytical method which is rapid, simple and accurate for discriminating these species using Fourier transform infrared spectroscopy (FTIR) combined with some chemometrics methods was developed. FTIR spectra were acquired in the mid-IR region (4000-400 cm-1). Standard normal variate, first and second order derivative spectra were compared for the spectral data. Principal component analysis (PCA) and canonical variate analysis (CVA) were used for the classification of the three species. Samples could be discriminated by visual analysis of the FTIR spectra by using their marker bands. Discrimination of the three species was also possible through the combination of the pre-processed FTIR spectra with PCA and CVA, in which CVA gave clearer discrimination. Subsequently, the developed method could be used for the identification and discrimination of the three closely-related plant species.

Gd-Complexes of New Arylpiperazinyl Conjugates of DTPA-Bis(amides): Synthesis, Characterization and Magnetic Relaxation Properties.

PubMed

Ba-Salem, Abdullah O; Ullah, Nisar; Shaikh, M Nasiruzzaman; Faiz, Mohamed; Ul-Haq, Zaheer

2015-04-29

Two new DTPA-bis(amide) based ligands conjugated with the arylpiperazinyl moiety were synthesized and subsequently transformed into their corresponding Gd(III) complexes 1 and 2 of the type [Gd(L)H2O]·nH2O. The relaxivity (R1) of these complexes was measured, which turned out to be comparable with that of Omniscan®, a commercially available MRI contrast agent. The cytotoxicity studies of these complexes indicated that they are non-toxic, which reveals their potential and physiological suitability as MRI contrast agents. All the synthesized ligands and complexes were characterized with the aid of analytical and spectroscopic methods, including elemental analysis, 1H-NMR, FT-IR, XPS and fast atom bombardment (FAB) mass spectrometry.

Comparative studies of structural, thermal, optical, and electrochemical properties of azines with different end groups with their azomethine analogues toward application in (opto)electronics.

PubMed

Sek, Danuta; Siwy, Mariola; Bijak, Katarzyna; Grucela-Zajac, Marzena; Malecki, Grzegorz; Smolarek, Karolina; Bujak, Lukasz; Mackowski, Sebastian; Schab-Balcerzak, Ewa

2013-10-10

Two series of azines and their azomethine analogues were prepared via condensation reaction of benzaldehyde, 2-hydroxybenzaldehyde, 4-pyridinecarboxaldehyde, 2-thiophenecarboxaldehyde, and 4-(diphenylamino)benzaldehyde with hydrazine monohydrate and 1,4-phenylenediamine, respectively. The structures of given compounds were characterized by FTIR, (1)H NMR, and (13)C NMR spectroscopy as well as elemental analysis. Optical, electrochemical, and thermal properties of all compounds were investigated by means of differential scanning calorimetry (DSC), UV-vis spectroscopy, stationary and time-resolved photoluminescence spectroscopy, and cycling voltammetry (CV). Additionally, the electronic properties, that is, orbital energies and resulting energy gap were calculated theoretically by density functional theory (DFT). Influence of chemical structure of the compounds on their properties was analyzed.

A study of phosphate absorption by magnesium iron hydroxycarbonate.

PubMed

Du, Yi; Rees, Nicholas; O'Hare, Dermot

2009-10-21

A study of the mechanism of phosphate adsorption by magnesium iron hydroxycarbonate, [Mg(2.25)Fe(0.75)(OH)(6)](CO(3))(0.37).0.65H(2)O over a range of pH has been carried out. The efficiency of the phosphate removal from aqueous solution has been investigated between pH 3-9 and the resulting solid phases have been studied by elemental analysis, XRD, FT-IR, Raman, HRTEM, EDX and solid-state MAS (31)P NMR. The analytical and spectroscopic data suggest that phosphate removal from solution occurs not by anion intercalation of the relevant phosphorous oxyanion (H(2)PO(4)(-) or HPO(4)(2-)) into the LDH but by the precipitation of either an insoluble iron hydrogen phosphate hydrate and/or a magnesium phosphate hydrate.

Physicochemical Investigation of 2,4,5-Trimethoxybenzylidene Propanedinitrile (TMPN) Dye as Fluorescence off-on Probe for Critical Micelle Concentration (CMC) of SDS and CTAB.

PubMed

Khan, Salman A; Asiri, Abdullah M

2015-11-01

2,4,5-trimethoxybenzylidene propanedinitrile (TMPN) was synthesized by Knoevenagel condensation. Structure of the TMPN was conformed by the elemental analysis and EI-MS, FT-IR, (1)H-NMR, (13)C-NMR spectroscopy. Absorbance and emission spectrum of the TMPN was studied in different solvent provide that TMPN is good absorbent and emission red shift in absorbance and emission spectra as polarity of the solvents increase. Photophysical properties including, oscillator strength, extinction coefficient, transition dipole moment, stokes shift and fluorescence quantum yield were investigated in order to investigate the physicochemical behaviors of TMPN. Dye undergoes solubilization in different micelles and may be used as a probe to determine the critical micelle concentration (CMC) of SDS and CTAB.

Lipase-catalyzed synthesis of fattythioic acids from palm oil.

PubMed

Al-Mulla, Emad A Jaffar

2011-01-01

The present work focuses on the synthesis of fattythioic acids (FTAs) by a one-step lipase catalyzed reaction of palm oil with carbonothioic S,S-acid using Lipozyme. The product was characterized using Fourier transform infrared (FTIR) spectroscopy, proton nuclear magnetic resonance ((1)H NMR) technique and elemental analysis. The effects of various reaction parameters such as reaction time, temperature, amount of enzyme, molar ratio of substrates, and various organic solvents of the reaction system were investigated. The optimum conditions to produce FTAs were respectively, incubation time, 20 h, temperature, 40°C, amount of enzyme, 0.05 g and molar ratio of carbonothioic S,S-acid to palm oil, 5.0:1.0. Hexane was the best solvent for this reaction. The conversion of the products at optimum conditions was around 91%.

Synthesis, characterization and application of a nano-manganese-catalyst as an efficient solid catalyst for solvent free selective oxidation of ethylbenzene, cyclohexene, and benzylalcohol

NASA Astrophysics Data System (ADS)

Habibi, Davood; Faraji, Ali Reza

2013-07-01

The object of this study is to synthesize the heterogeneous Mn-nano-catalyst (MNC) which has been covalently anchored on a modified nanoscaleSiO2/Al2O3, and characterized by FT-IR, UV-Vis, CHN elemental analysis, EDS, TEM, and EDX. The method is efficient for the highly selective oxidation of ethylbenzene, cyclohexene, and benzylalcohol without the need to any solvents, using tert-butyl hydroperoxide (TBHP) as an oxidant. Oxidation of ethylbenzene, cyclohexene, and benzylalcohol gave acetophenone, 2-cyclohexene-1-one and benzaldehyde, respectively, as major products. Reaction conditions have been optimized by considering the effect of various factors such as reaction time, amounts of substrates and oxidant, Mn-nano-catalyst and application of various solvents.

Synthesis, spectral and thermal studies of the newly hydrogen bonded charge transfer complex of o-phenylenediamine with pi acceptor picric acid.

PubMed

Khan, Ishaat M; Ahmad, Afaq

2010-10-01

Newly proton or charge transfer complex [(OPDH)(+)(PA)(-)] was synthesized by the reaction of the donor, o-phenylenediamine (OPD) with acceptor, 2,4,6-trinitrophenol (PAH). The chemical reaction has occurred via strong hydrogen bonding followed by migration of proton from acceptor to donor. UV-vis, (1)H NMR and FTIR spectra, in addition to the thermal and elemental analysis were used to confirm the proposed occurrence of the chemical reaction and to investigate the newly synthesized solid CT complex. The stoichiometry of the CT complex was found to be 1:1. The formation constant and molar extinction coefficient of the CT complex were evaluated by the Benesi-Hildebrand equation. Copyright 2010 Elsevier B.V. All rights reserved.

New series of aromatic/ five-membered heteroaromatic butanesulfonyl hydrazones as potent biological agents: Synthesis, physicochemical and electronic properties

NASA Astrophysics Data System (ADS)

Hamurcu, Fatma; Mamaş, Serhat; Ozdemir, Ummuhan Ozmen; Gündüzalp, Ayla Balaban; Senturk, Ozan Sanlı

2016-08-01

The aromatic/five-membered heteroaromatic butanesulfonylhydrazone derivatives; 5-bromosalicylaldehydebutanesulfonylhydrazone(1), 2-hydroxy-1-naphthaldehydebutane sulfonylhydrazone(2), indole-3-carboxaldehydebutanesulfonylhydrazone (3), 2-acetylfuran- carboxyaldehydebutanesulfonylhydrazone(4), 2-acetylthiophenecarboxyaldehydebutane- sulfonylhydrazone(5) and 2-acetyl-5-chlorothiophenecarboxyaldehydebutanesulfonyl hydrazone (6) were synthesized by the reaction of butane sulfonic acid hydrazide with aldehydes/ketones and characterized by using elemental analysis, 1H NMR, 13C NMR and FT-IR technique. Their geometric parameters and electronic properties consist of global reactivity descriptors were also determined by theoretical methods. The electrochemical behavior of the butanesulfonylhydrazones were investigated by using cyclic voltammetry (CV), controlled potential electrolysis and chronoamperometry (CA) techniques. The number of electrons transferred (n), diffusion coefficient (D) and standard heterogeneous rate constants (ks) were determined by electrochemical methods.

Quantitative analysis of virgin coconut oil in cream cosmetics preparations using fourier transform infrared (FTIR) spectroscopy.

PubMed

Rohman, A; Man, Yb Che; Sismindari

2009-10-01

Today, virgin coconut oil (VCO) is becoming valuable oil and is receiving an attractive topic for researchers because of its several biological activities. In cosmetics industry, VCO is excellent material which functions as a skin moisturizer and softener. Therefore, it is important to develop a quantitative analytical method offering a fast and reliable technique. Fourier transform infrared (FTIR) spectroscopy with sample handling technique of attenuated total reflectance (ATR) can be successfully used to analyze VCO quantitatively in cream cosmetic preparations. A multivariate analysis using calibration of partial least square (PLS) model revealed the good relationship between actual value and FTIR-predicted value of VCO with coefficient of determination (R2) of 0.998.

Molecular and structural characteristics in toxic algae cultures of Ostreopsis ovata and Ostreopsis spp. evidenced by FTIR and FTNIR spectroscopy

NASA Astrophysics Data System (ADS)

Mecozzi, Mauro; Pietroletti, Marco; Tornambè, Andrea

2011-05-01

In this article we investigated the compositional and structural characteristics of the principal biomolecules such as carbohydrates, proteins, lipids, nucleic acids and chlorophyll pigments present in biofilm cultures of Ostreopsis spp. and in batch cultures of Ostreopsis ovata. Our approach based on the use of infrared (FTIR) and near infrared (FTNIR) spectroscopy showed the marked differences existing between biofilm cultures and batch cultures. FTIR spectroscopy showed the higher contents of polysaccharides and chlorophyll pigments in O. ovata from batch cultures with respect to Ostreopsis spp. Second derivative FTIR spectroscopy showed different features concerning the secondary structure of proteins because in O. ovata samples the beta sheet and beta turn structures were observed whereas in Ostreopsis spp. samples the alpha helix structure was the most evident. FTNIR spectroscopy showed other structural differences observed existing between O. ovata and Ostreopsis spp. mainly related to hydrogen bond interactions determining more packed structures in the nucleus of O. ovata. In addition, the interpretation of FTIR and FTNIR spectral information was also supported by the application of two statistical methods, the independent component analysis (ICA) and the spectral cross correlation analysis (SCCA). ICA was used as spectral deconvolution technique to separate the effects of the interference bicarbonate ion from algal FTIR spectra so to verify the high similar qualitative composition of the three biofilm samples of Ostreopsis spp. At last, SCCA applied to FTIR and FTNIR spectra was useful to evidence some structural differences involving -CH and CH 2 groups of aliphatic chains in O. ovata and Ostreopsis spp. samples. Though preliminary, these results agree with some previous studies suggesting that the presence of different ecophysiological characteristics in O. ovata and Ostreopsis spp. depending on the parameters related to the condition growth.

Exploring Geographical Differentiation of the Hoelen Medicinal Mushroom, Wolfiporia extensa (Agaricomycetes), Using Fourier-Transform Infrared Spectroscopy Combined with Multivariate Analysis.

PubMed

Li, Yan; Zhang, Ji; Zhao, Yanli; Liu, Honggao; Wang, Yuanzhong; Jin, Hang

2016-01-01

In this study the geographical differentiation of dried sclerotia of the medicinal mushroom Wolfiporia extensa, obtained from different regions in Yunnan Province, China, was explored using Fourier-transform infrared (FT-IR) spectroscopy coupled with multivariate data analysis. The FT-IR spectra of 97 samples were obtained for wave numbers ranging from 4000 to 400 cm-1. Then, the fingerprint region of 1800-600 cm-1 of the FT-IR spectrum, rather than the full spectrum, was analyzed. Different pretreatments were applied on the spectra, and a discriminant analysis model based on the Mahalanobis distance was developed to select an optimal pretreatment combination. Two unsupervised pattern recognition procedures- principal component analysis and hierarchical cluster analysis-were applied to enhance the authenticity of discrimination of the specimens. The results showed that excellent classification could be obtained after optimizing spectral pretreatment. The tested samples were successfully discriminated according to their geographical locations. The chemical properties of dried sclerotia of W. extensa were clearly dependent on the mushroom's geographical origins. Furthermore, an interesting finding implied that the elevations of collection areas may have effects on the chemical components of wild W. extensa sclerotia. Overall, this study highlights the feasibility of FT-IR spectroscopy combined with multivariate data analysis in particular for exploring the distinction of different regional W. extensa sclerotia samples. This research could also serve as a basis for the exploitation and utilization of medicinal mushrooms.

Identification and characterization of salmonella serotypes using DNA spectral characteristics by fourier transform infrared (FT-IR) spectroscopy

USDA-ARS?s Scientific Manuscript database

Analysis of DNA samples of Salmonella serotypes (Salmonella Typhimurium, Salmonella Enteritidis, Salmonella Infantis, Salmonella Heidelberg and Salmonella Kentucky) were performed using Fourier transform infrared spectroscopy (FT-IR) spectrometer by placing directly in contact with a diamond attenua...

[Differentiation and characterization of yeasts pathogenic for humans (Candida albicans, Exophiala dermatitidis) and algae pathogenic for animals (Prototheca spp.) using Fourier transform infrared spectroscopy (FTIR) in comparison with conventional methods].

PubMed

Schmalreck, A F; Tränkle, P; Vanca, E; Blaschke-Hellmessen, R

1998-01-01

Due to the Fourier-Transform Infrared Spectroscopy (FT-IR) of strain specific traits demonstrated to be a suitable and efficient method for diagnostic and epidemiological determinations for the yeasts Candida albicans, Exophiala dermatitidis and the chlorophylless algae of the genus Prototheca. FT-IR leads in a rapid and economical way to reproducible results according to the spectral differences of intact cells (IR-fingerprints). Different genera, species and sub-species respectively, different strains can be recognized and grouped into different clusters and subclusters. The FT-IR analysis of Candida albicans isolates (n = 150) of 22 newborns-at-risk of an intensive care unit showed, that 86% of the children were colonised with several (2-4) different strains in the oral cavities and faeces. Stationary cross-infections could definitely be determined. Exophiala dermatitidis isolates (n = 31), mostly isolated repetitively within a period of 3 years from sputa of patients suffering from cystic fibrosis could be characterized and grouped patient-specifically over the total sampling period. Of 6 from 8 patients (75%) their individual strains remain the same and could be tracked over the three years. Cross-infections during the stationary treatment could be clearly identified by FT-IR. The Prototheca isolate (n = 43) from live-stock and farm environment showed clear distinguishable clusters differentiating the species P. wickerhamii, P. zopfii and P. stagnora. In addition, the biotypes of P. zopfii could be distinguished, especially the subclusters of variants II and III. It could be demonstrated, that FT-IR is suitable for the routine identification and differentiation of yeasts and algae. However, in spite of the gain of knowledge by using FT-IR for the characterization of microorganisms, the conventional phenotyping and/or genetic analysis of yeast or algae strains cannot be replaced completely. For a final taxonomic classification a combination of conventional methods on FT-IR together with more sophisticated molecular genetic procedures is necessary.

Spectroscopic and statistical approach of archaeological artifacts recently excavated from Tamilnadu, South India

NASA Astrophysics Data System (ADS)

Seetha, D.; Velraj, G.

2015-10-01

The ancient materials characterization will bring back the more evidence of the ancient people life styles. In this study, the archaeological pottery shards recently excavated from Kodumanal, Erode District in Tamilnadu, South India were investigated. The experimental results enlighten us to the elemental and the mineral composition of the pottery shards. The FT-IR technique tells that the mineralogy and the firing temperature of the samples are less than 800 °C, in the oxidizing/reducing atmosphere and the XRD was used as a complementary technique for the mineralogy. A thorough scientific study of SEM-EDS with the help of statistical approach done to find the provenance of the selected pot shards has not yet been performed. EDS and XRF results revealed that the investigated samples have the elements O, Si, Al, Fe, Mn, Mg, Ca, Ti, K and Na are in different compositions. For establishing the provenance (same or different origin) of pottery samples, Al and Si concentration ratio as well as hierarchical cluster analysis (HCA) was used and the results are correlated.

Multivariate analysis of ATR-FTIR spectra for assessment of oil shale organic geochemical properties

USGS Publications Warehouse

Washburn, Kathryn E.; Birdwell, Justin E.

2013-01-01

In this study, attenuated total reflectance (ATR) Fourier transform infrared spectroscopy (FTIR) was coupled with partial least squares regression (PLSR) analysis to relate spectral data to parameters from total organic carbon (TOC) analysis and programmed pyrolysis to assess the feasibility of developing predictive models to estimate important organic geochemical parameters. The advantage of ATR-FTIR over traditional analytical methods is that source rocks can be analyzed in the laboratory or field in seconds, facilitating more rapid and thorough screening than would be possible using other tools. ATR-FTIR spectra, TOC concentrations and Rock–Eval parameters were measured for a set of oil shales from deposits around the world and several pyrolyzed oil shale samples. PLSR models were developed to predict the measured geochemical parameters from infrared spectra. Application of the resulting models to a set of test spectra excluded from the training set generated accurate predictions of TOC and most Rock–Eval parameters. The critical region of the infrared spectrum for assessing S1, S2, Hydrogen Index and TOC consisted of aliphatic organic moieties (2800–3000 cm−1) and the models generated a better correlation with measured values of TOC and S2 than did integrated aliphatic peak areas. The results suggest that combining ATR-FTIR with PLSR is a reliable approach for estimating useful geochemical parameters of oil shales that is faster and requires less sample preparation than current screening methods.

Source Determination of Red Gel Pen Inks using Raman Spectroscopy and Attenuated Total Reflectance Fourier Transform Infrared Spectroscopy combined with Pearson's Product Moment Correlation Coefficients and Principal Component Analysis.

PubMed

Mohamad Asri, Muhammad Naeim; Mat Desa, Wan Nur Syuhaila; Ismail, Dzulkiflee

2018-01-01

The potential combination of two nondestructive techniques, that is, Raman spectroscopy (RS) and attenuated total reflectance-fourier transform infrared (ATR-FTIR) spectroscopy with Pearson's product moment correlation (PPMC) coefficient (r) and principal component analysis (PCA) to determine the actual source of red gel pen ink used to write a simulated threatening note, was examined. Eighteen (18) red gel pens purchased from Japan and Malaysia from November to December 2014 where one of the pens was used to write a simulated threatening note were analyzed using RS and ATR-FTIR spectroscopy, respectively. The spectra of all the red gel pen inks including the ink deposited on the simulated threatening note gathered from the RS and ATR-FTIR analyses were subjected to PPMC coefficient (r) calculation and principal component analysis (PCA). The coefficients r = 0.9985 and r = 0.9912 for pairwise combination of RS and ATR-FTIR spectra respectively and similarities in terms of PC1 and PC2 scores of one of the inks to the ink deposited on the simulated threatening note substantiated the feasibility of combining RS and ATR-FTIR spectroscopy with PPMC coefficient (r) and PCA for successful source determination of red gel pen inks. The development of pigment spectral library had allowed the ink deposited on the threatening note to be identified as XSL Poppy Red (CI Pigment Red 112). © 2017 American Academy of Forensic Sciences.

Polymeric material prepared from Schiff base based on O-carboxymethyl chitosan and its Cu(II) and Pd(II) complexes

NASA Astrophysics Data System (ADS)

Baran, Talat; Menteş, Ayfer

2016-07-01

In this study, a new eco-friendly Schiff base based on O-carboxymethyl chitosan ([OCMCS-7a]) and its copper(II) and palladium(II) complexes were synthesized. Characterizations of [OCMCS-7a] and its metal complexes were conducted using FTIR, 1H NMR, 13C NMR, TG/DTG, XRD, SEM-EDAX, ICP, UV-VIS, GC-MS, elemental analysis, magnetic moment and molar conductivity measurements. The degree of substitution (DS) of [OCMCS-7a] was determined by elemental analysis to be 0.44. It was shown by the solubility test that [OCMCS-7a] was completely soluble in water. Surface images of chitosan, [OCMCS-7a] and its Cu(II) and Pd(II) complexes were investigated using the SEM-EDAX technique. Their thermal behaviors and crystallinities of the synthesized complexes were determined by TG/DTG and X-ray powder diffraction techniques, respectively. The metal contents of the obtained complexes were determined using an ICP-OES instrument. From the analyses, it was noted that the thermal stabilities and crystallinities of [OCMCS-7a] and its complexes decreased compared to chitosan. As a consequence of surface screening, it was also noted that the surface structure of the chitosan was smoother than that of the obtained compounds.

Investigations on structural, vibrational, morphological and optical properties of CdS and CdS/Co films by ultrasonic spray pyrolysis

NASA Astrophysics Data System (ADS)

Aksay, S.; Polat, M.; Özer, T.; Köse, S.; Gürbüz, G.

2011-09-01

CdS and CdS/Co films have been deposited on glass substrates by an ultrasonic spray pyrolysis method. The effects of Co incorporation on the structural, optical, morphological, elemental and vibrational properties of these films were investigated. XRD analysis confirmed the hexagonal wurtzite structure of all films and had no impurity phase. While CdS film has (0 0 2) as the preferred orientation, CdS/Co films have (1 1 0) as the preferred orientation. The direct optical band gap was found to decrease from 2.42 to 2.39 eV by Co incorporation. The decrease of the direct energy gaps by increasing Co contents is mainly due to the sp-d exchange interaction between the localized d-electrons of Co2+ ions and band electrons of CdS. After the optical investigations, it was seen that the transmittance of CdS films decreased by Co content. The Raman measurements revealed two peaks corresponding to the 1LO and 2LO modes of hexagonal CdS. The vibrational modes of Cd-S were obtained in the wavenumber range (590-715 cm-1) using Fourier transform infrared spectroscopy (FTIR). The elemental analysis of the film was done by energy dispersive X-ray spectrometry.

Grafting of Oligo(ethylene glycol)-Functionalized Calix[4]arene-Tetradiazonium Salts for Antifouling Germanium and Gold Surfaces.

PubMed

Blond, Pascale; Mattiuzzi, Alice; Valkenier, Hennie; Troian-Gautier, Ludovic; Bergamini, Jean-François; Doneux, Thomas; Goormaghtigh, Erik; Raussens, Vincent; Jabin, Ivan

2018-05-29

Biosensors that can determine protein concentration and structure are highly desired for biomedical applications. For the development of such biosensors, the use of Fourier transform infrared (FTIR) spectroscopy with the attenuated internal total reflection (ATR) configuration is particularly attractive, but it requires appropriate surface functionalization of the ATR optical element. Indeed, the surface has to specifically interact with a target protein in close contact with the optical element and must display antifouling properties to prevent nonspecific adsorption of other proteins. Here, we report robust monolayers of calix[4]arenes bearing oligo(ethylene glycol) (oEG) chains, which were grafted on germanium and gold surfaces via their tetradiazonium salts. The formation of monolayers of oEGylated calix[4]arenes was confirmed by AFM, IR, and contact angle measurements. The antifouling properties of these modified surfaces were studied by ATR-FTIR spectroscopy and fluorescence microscopy, and the nonspecific absorption of bovine serum albumin was found to be reduced by 85% compared to that of unmodified germanium. In other words, the organic coating by oEGylated calix[4]arenes provides remarkable antifouling properties, opening the way for the design of germanium- or gold-based biosensors.

Characterisations of collagen-silver-hydroxyapatite nanocomposites

NASA Astrophysics Data System (ADS)

Ciobanu, C. S.; Popa, C. L.; Petre, C. C.; Jiga, G.; Trusca, R.; Predoi, D.

2016-05-01

The XRD analysis were performed to confirm the formation of hydroxyapatite structure in collagen-silver-hydroxyapatite nanocomposites. The molecular interaction in collagen-hydroxyapatite nanocomposites was highlighted by Fourier transform infrared spectroscopy (FTIR) analysis. The SEM showed a nanostructure of collagen-silverhydroxyapatite nanocomposites composed of nano needle-like particles in a veil with collagen texture. The presence of vibrational groups characteristics to the hydroxyapatite structure in collagen-silver-hydroxyapatite (AgHApColl) nanocomposites was investigated by FTIR.

Effects of Er:YAG laser irradiation on human dentin: polarizing microscopic, light microscopic and microradiographic observations, and FT-IR analysis.

PubMed

Ishizaka, Yaeko; Eguro, Toru; Maeda, Toru; Tanaka, Hisayoshi

2002-01-01

The effects of Er:YAG laser irradiation on dentin have not been sufficiently investigated. The purpose of this study was to investigate the effects of Er:YAG laser irradiation on dentin. After cavities were prepared using Er:YAG laser irradiation or rotary cutting instruments, histological observations of cavity-floor dentin utilizing polarizing microscopy, microradiography and light microscopy, and analysis of composition of cavity-floor dentin using Fourier-transformed (FT-IR) spectrometry were conducted. In the laser-treated side, a deeply stained basophilic layer was observed. The number of odontoblastic processes present was obviously less in the laser-treated side than in the bur-treated side. FT-IR analysis revealed that compared to the bur-treated side, a broad background peak at around 1,600 cm(-1) was present. Er:YAG laser irradiation might have denatured the organic materials of dentin. Copyright 2002 Wiley-Liss, Inc.

High-definition Fourier Transform Infrared (FT-IR) Spectroscopic Imaging of Human Tissue Sections towards Improving Pathology

PubMed Central

Nguyen, Peter L.; Davidson, Bennett; Akkina, Sanjeev; Guzman, Grace; Setty, Suman; Kajdacsy-Balla, Andre; Walsh, Michael J.

2015-01-01

High-definition Fourier Transform Infrared (FT-IR) spectroscopic imaging is an emerging approach to obtain detailed images that have associated biochemical information. FT-IR imaging of tissue is based on the principle that different regions of the mid-infrared are absorbed by different chemical bonds (e.g., C=O, C-H, N-H) within cells or tissue that can then be related to the presence and composition of biomolecules (e.g., lipids, DNA, glycogen, protein, collagen). In an FT-IR image, every pixel within the image comprises an entire Infrared (IR) spectrum that can give information on the biochemical status of the cells that can then be exploited for cell-type or disease-type classification. In this paper, we show: how to obtain IR images from human tissues using an FT-IR system, how to modify existing instrumentation to allow for high-definition imaging capabilities, and how to visualize FT-IR images. We then present some applications of FT-IR for pathology using the liver and kidney as examples. FT-IR imaging holds exciting applications in providing a novel route to obtain biochemical information from cells and tissue in an entirely label-free non-perturbing route towards giving new insight into biomolecular changes as part of disease processes. Additionally, this biochemical information can potentially allow for objective and automated analysis of certain aspects of disease diagnosis. PMID:25650759

Quantitative analysis of Sudan dye adulteration in paprika powder using FTIR spectroscopy

USDA-ARS?s Scientific Manuscript database

The presence of Sudan dye used illegally for coloring in food stuffs has become a point of food safety concern, especially in paprika- and chili-containing food products. Fourier transform infrared (FTIR) spectroscopy has been extensively used as an analytical method for quality control and safety m...

Limitations and potential of spectral subtractions in fourier-transform infrared (FTIR) spectroscopy of soil samples

USDA-ARS?s Scientific Manuscript database

Soil science research is increasingly applying Fourier transform infrared (FTIR) spectroscopy for analysis of soil organic matter (SOM). However, the compositional complexity of soils and the dominance of the mineral component can limit spectroscopic resolution of SOM and other minor components. The...

Quantitative assessment of copper proteinates used as animal feed additives using ATR-FTIR spectroscopy and powder X-ray diffraction (PXRD) analysis.

PubMed

Cantwell, Caoimhe A; Byrne, Laurann A; Connolly, Cathal D; Hynes, Michael J; McArdle, Patrick; Murphy, Richard A

2017-08-01

The aim of the present work was to establish a reliable analytical method to determine the degree of complexation in commercial metal proteinates used as feed additives in the solid state. Two complementary techniques were developed. Firstly, a quantitative attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectroscopic method investigated modifications in vibrational absorption bands of the ligand on complex formation. Secondly, a powder X-ray diffraction (PXRD) method to quantify the amount of crystalline material in the proteinate product was developed. These methods were developed in tandem and cross-validated with each other. Multivariate analysis (MVA) was used to develop validated calibration and prediction models. The FTIR and PXRD calibrations showed excellent linearity (R 2  > 0.99). The diagnostic model parameters showed that the FTIR and PXRD methods were robust with a root mean square error of calibration RMSEC ≤3.39% and a root mean square error of prediction RMSEP ≤7.17% respectively. Comparative statistics show excellent agreement between the MVA packages assessed and between the FTIR and PXRD methods. The methods can be used to determine the degree of complexation in complexes of both protein hydrolysates and pure amino acids.

Quantitative analysis of Sudan dye adulteration in paprika powder using FTIR spectroscopy.

PubMed

Lohumi, Santosh; Joshi, Ritu; Kandpal, Lalit Mohan; Lee, Hoonsoo; Kim, Moon S; Cho, Hyunjeong; Mo, Changyeun; Seo, Young-Wook; Rahman, Anisur; Cho, Byoung-Kwan

2017-05-01

As adulteration of foodstuffs with Sudan dye, especially paprika- and chilli-containing products, has been reported with some frequency, this issue has become one focal point for addressing food safety. FTIR spectroscopy has been used extensively as an analytical method for quality control and safety determination for food products. Thus, the use of FTIR spectroscopy for rapid determination of Sudan dye in paprika powder was investigated in this study. A net analyte signal (NAS)-based methodology, named HLA/GO (hybrid linear analysis in the literature), was applied to FTIR spectral data to predict Sudan dye concentration. The calibration and validation sets were designed to evaluate the performance of the multivariate method. The obtained results had a high determination coefficient (R 2 ) of 0.98 and low root mean square error (RMSE) of 0.026% for the calibration set, and an R 2 of 0.97 and RMSE of 0.05% for the validation set. The model was further validated using a second validation set and through the figures of merit, such as sensitivity, selectivity, and limits of detection and quantification. The proposed technique of FTIR combined with HLA/GO is rapid, simple and low cost, making this approach advantageous when compared with the main alternative methods based on liquid chromatography (LC) techniques.

Spatial and molecular resolution of diffuse malignant mesothelioma heterogeneity by integrating label-free FTIR imaging, laser capture microdissection and proteomics

NASA Astrophysics Data System (ADS)

Großerueschkamp, Frederik; Bracht, Thilo; Diehl, Hanna C.; Kuepper, Claus; Ahrens, Maike; Kallenbach-Thieltges, Angela; Mosig, Axel; Eisenacher, Martin; Marcus, Katrin; Behrens, Thomas; Brüning, Thomas; Theegarten, Dirk; Sitek, Barbara; Gerwert, Klaus

2017-03-01

Diffuse malignant mesothelioma (DMM) is a heterogeneous malignant neoplasia manifesting with three subtypes: epithelioid, sarcomatoid and biphasic. DMM exhibit a high degree of spatial heterogeneity that complicates a thorough understanding of the underlying different molecular processes in each subtype. We present a novel approach to spatially resolve the heterogeneity of a tumour in a label-free manner by integrating FTIR imaging and laser capture microdissection (LCM). Subsequent proteome analysis of the dissected homogenous samples provides in addition molecular resolution. FTIR imaging resolves tumour subtypes within tissue thin-sections in an automated and label-free manner with accuracy of about 85% for DMM subtypes. Even in highly heterogeneous tissue structures, our label-free approach can identify small regions of interest, which can be dissected as homogeneous samples using LCM. Subsequent proteome analysis provides a location specific molecular characterization. Applied to DMM subtypes, we identify 142 differentially expressed proteins, including five protein biomarkers commonly used in DMM immunohistochemistry panels. Thus, FTIR imaging resolves not only morphological alteration within tissue but it resolves even alterations at the level of single proteins in tumour subtypes. Our fully automated workflow FTIR-guided LCM opens new avenues collecting homogeneous samples for precise and predictive biomarkers from omics studies.

Spatial and molecular resolution of diffuse malignant mesothelioma heterogeneity by integrating label-free FTIR imaging, laser capture microdissection and proteomics.

PubMed

Großerueschkamp, Frederik; Bracht, Thilo; Diehl, Hanna C; Kuepper, Claus; Ahrens, Maike; Kallenbach-Thieltges, Angela; Mosig, Axel; Eisenacher, Martin; Marcus, Katrin; Behrens, Thomas; Brüning, Thomas; Theegarten, Dirk; Sitek, Barbara; Gerwert, Klaus

2017-03-30

Diffuse malignant mesothelioma (DMM) is a heterogeneous malignant neoplasia manifesting with three subtypes: epithelioid, sarcomatoid and biphasic. DMM exhibit a high degree of spatial heterogeneity that complicates a thorough understanding of the underlying different molecular processes in each subtype. We present a novel approach to spatially resolve the heterogeneity of a tumour in a label-free manner by integrating FTIR imaging and laser capture microdissection (LCM). Subsequent proteome analysis of the dissected homogenous samples provides in addition molecular resolution. FTIR imaging resolves tumour subtypes within tissue thin-sections in an automated and label-free manner with accuracy of about 85% for DMM subtypes. Even in highly heterogeneous tissue structures, our label-free approach can identify small regions of interest, which can be dissected as homogeneous samples using LCM. Subsequent proteome analysis provides a location specific molecular characterization. Applied to DMM subtypes, we identify 142 differentially expressed proteins, including five protein biomarkers commonly used in DMM immunohistochemistry panels. Thus, FTIR imaging resolves not only morphological alteration within tissue but it resolves even alterations at the level of single proteins in tumour subtypes. Our fully automated workflow FTIR-guided LCM opens new avenues collecting homogeneous samples for precise and predictive biomarkers from omics studies.

Development of a Fourier transform infrared spectroscopy coupled to UV-Visible analysis technique for aminosides and glycopeptides quantitation in antibiotic locks.

PubMed

Sayet, G; Sinegre, M; Ben Reguiga, M

2014-01-01

Antibiotic Lock technique maintains catheters' sterility in high-risk patients with long-term parenteral nutrition. In our institution, vancomycin, teicoplanin, amikacin and gentamicin locks are prepared in the pharmaceutical department. In order to insure patient safety and to comply to regulatory requirements, antibiotic locks are submitted to qualitative and quantitative assays prior to their release. The aim of this study was to develop an alternative quantitation technique for each of these 4 antibiotics, using a Fourier transform infrared (FTIR) coupled to UV-Visible spectroscopy and to compare results to HPLC or Immunochemistry assays. Prevalidation studies permitted to assess spectroscopic conditions used for antibiotic locks quantitation: FTIR/UV combinations were used for amikacin (1091-1115cm(-1) and 208-224nm), vancomycin (1222-1240cm(-1) and 276-280nm), and teicoplanin (1226-1230cm(-1) and 278-282nm). Gentamicin was quantified with FTIR only (1045-1169cm(-1) and 2715-2850cm(-1)) due to interferences in UV domain of parabens, preservatives present in the commercial brand used to prepare locks. For all AL, the method was linear (R(2)=0.996 to 0.999), accurate, repeatable (intraday RSD%: from 2.9 to 7.1% and inter-days RSD%: 2.9 to 5.1%) and precise. Compared to the reference methods, the FTIR/UV method appeared tightly correlated (Pearson factor: 97.4 to 99.9%) and did not show significant difference in recovery determinations. We developed a new simple reliable analysis technique for antibiotics quantitation in locks using an original association of FTIR and UV analysis, allowing a short time analysis to identify and quantify the studied antibiotics. Copyright © 2013 Elsevier Masson SAS. All rights reserved.

A simple model for cell type recognition using 2D-correlation analysis of FTIR images from breast cancer tissue

NASA Astrophysics Data System (ADS)

Ali, Mohamed H.; Rakib, Fazle; Al-Saad, Khalid; Al-Saady, Rafif; Lyng, Fiona M.; Goormaghtigh, Erik

2018-07-01

Breast cancer is the second most common cancer after lung cancer. So far, in clinical practice, most cancer parameters originating from histopathology rely on the visualization by a pathologist of microscopic structures observed in stained tissue sections, including immunohistochemistry markers. Fourier transform infrared spectroscopy (FTIR) spectroscopy provides a biochemical fingerprint of a biopsy sample and, together with advanced data analysis techniques, can accurately classify cell types. Yet, one of the challenges when dealing with FTIR imaging is the slow recording of the data. One cm2 tissue section requires several hours of image recording. We show in the present paper that 2D covariance analysis singles out only a few wavenumbers where both variance and covariance are large. Simple models could be built using 4 wavenumbers to identify the 4 main cell types present in breast cancer tissue sections. Decision trees provide particularly simple models to reach discrimination between the 4 cell types. The robustness of these simple decision-tree models were challenged with FTIR spectral data obtained using different recording conditions. One test set was recorded by transflection on tissue sections in the presence of paraffin while the training set was obtained on dewaxed tissue sections by transmission. Furthermore, the test set was collected with a different brand of FTIR microscope and a different pixel size. Despite the different recording conditions, separating extracellular matrix (ECM) from carcinoma spectra was 100% successful, underlying the robustness of this univariate model and the utility of covariance analysis for revealing efficient wavenumbers. We suggest that 2D covariance maps using the full spectral range could be most useful to select the interesting wavenumbers and achieve very fast data acquisition on quantum cascade laser infrared imaging microscopes.

Standardization of Shodhita Naga with special reference to thermogravimetry and infra-red spectroscopy.

PubMed

Rajput, Dhirajsingh S; Patgiri, Biswajyoti; Shukla, Vinay J

2014-01-01

Standardization of Ayurvedic medicine is the need of hour to obtain desired quality of final product. Shodhana literally means purification, is the initial step to make drugs like metals, minerals and poisonous herbs suitable for further procedure. Shodhana of metals/minerals help to expose maximum surface area of drug for chemical reactions and also in impregnation of organic materials and their properties in the drug. Thermo-gravimetric analysis (TGA) facilitates in identifying the presence of organic matter and change in the melting point of metal whereas Fourier transform infra-red spectroscopy (FTIR) assists in identifying the presence of various functional groups. To standardize the process of Naga Shodhana and to study the change in chemical nature of Shodhita Naga in each media through TGA and FTIR. Samanya and Vishesha Shodhana of Naga was carried out. Time taken for melting of Naga, physico-chemical changes in media used for Shodhana and weight changes after Shodhana were recorded. Samples of Naga were collected after Shodhana in each media for TGA and FTIR analysis. Average loss occurred during Shodhana was 6.26%. Melting point of Ashuddha Naga was 327.46°C, and it was 328.42°C after Shodhana. Percentage purity of Naga (percentage of lead in Naga) decreased after Shodhana from 99.80% to 99.40%. FTIR analysis of Shodhita Naga in each sample showed stretching vibrations particularly between C-H and C-N bonds that are indicating the presence of various organic compounds. According to TGA and FTIR analysis, Shodhana process increases melting point of Naga and initiation of new physico-chemical properties which are indicated by detection of large number of functional groups and organo-metallic nature of Shodhita Naga.

Standardization of Shodhita Naga with special reference to thermogravimetry and infra-red spectroscopy

PubMed Central

Rajput, Dhirajsingh S.; Patgiri, Biswajyoti; Shukla, Vinay J.

2014-01-01

Background: Standardization of Ayurvedic medicine is the need of hour to obtain desired quality of final product. Shodhana literally means purification, is the initial step to make drugs like metals, minerals and poisonous herbs suitable for further procedure. Shodhana of metals/minerals help to expose maximum surface area of drug for chemical reactions and also in impregnation of organic materials and their properties in the drug. Thermo-gravimetric analysis (TGA) facilitates in identifying the presence of organic matter and change in the melting point of metal whereas Fourier transform infra-red spectroscopy (FTIR) assists in identifying the presence of various functional groups. Aim: To standardize the process of Naga Shodhana and to study the change in chemical nature of Shodhita Naga in each media through TGA and FTIR. Material and Methods: Samanya and Vishesha Shodhana of Naga was carried out. Time taken for melting of Naga, physico-chemical changes in media used for Shodhana and weight changes after Shodhana were recorded. Samples of Naga were collected after Shodhana in each media for TGA and FTIR analysis. Results: Average loss occurred during Shodhana was 6.26%. Melting point of Ashuddha Naga was 327.46°C, and it was 328.42°C after Shodhana. Percentage purity of Naga (percentage of lead in Naga) decreased after Shodhana from 99.80% to 99.40%. FTIR analysis of Shodhita Naga in each sample showed stretching vibrations particularly between C-H and C-N bonds that are indicating the presence of various organic compounds. Conclusion: According to TGA and FTIR analysis, Shodhana process increases melting point of Naga and initiation of new physico-chemical properties which are indicated by detection of large number of functional groups and organo-metallic nature of Shodhita Naga. PMID:26664241

Control of separation and quantitative analysis by GC-FTIR

NASA Astrophysics Data System (ADS)

Semmoud, A.; Huvenne, Jean P.; Legrand, P.

1992-03-01

Software for 3-D representations of the 'Absorbance-Wavenumber-Retention time' is used to control the quality of the GC separation. Spectral information given by the FTIR detection allows the user to be sure that a chromatographic peak is 'pure.' The analysis of peppermint essential oil is presented as an example. This assurance is absolutely required for quantitative applications. In these conditions, we have worked out a quantitative analysis of caffeine. Correlation coefficients between integrated absorbance measurements and concentration of caffeine are discussed at two steps of the data treatment.

Sonochemical synthesis and DFT studies of nano novel Schiff base cadmium complexes: Green, efficient, recyclable catalysts and precursors of Cd NPs

NASA Astrophysics Data System (ADS)

Parsaee, Zohreh

2017-10-01

Novel asymmetric (N4) Schiff bases (Ln, n = 1-3) and their nanosized cadmium complexes derived of 4,4'-(pentylazanediyl) dibenzaldehyde and aminobenzaldehyde are synthesized by sonochemical method and characterized based on physicochemical analysis including 1H NMR, 13C NMR, SEM, TGA, Mass, FT-IR, UV-Vis spectroscopy, elemental analysis, magnetic moment and molar conductance measurements. According to the analytic results of the NMR, UV-Vis and magnetic moment studies, it is found that the geometrical structures of these complexes [CdII2LnCl4], (L = C45H40N5X, X = CH3, Cl, OH) are square planer. The synthesized complexes were so effective as nanocatalyst on the oxidation of primary and secondary alcohols. The oxidation reactions were carried out in ethyl-methyl-imidazolium ionic liquid in presence of NaOCl. In addition Cd NPs were synthesized through the thermal decomposition of mentioned complexes and characterized by using FT-IR, SEM, TEM, EDX and XRD methods, which indicated close accordance to the standard pattern of CdO nanoparticles and an acceptable size at the nanorange (22-27 nm). Furthermore geometrical optimization of the Cd2LnCl4 calculated using DFT/B3LYP with LanL2DZ/6-311+G (d,p) level. The electronic parameter including HOMO-LUMO orbitals, bond gap, chemical hardness-softness, electronegativity, electrophilicity, NMR chemical shifts and IR frequencies were calculated. The calculated NMR shifts and vibrational frequencies showed excellent agreement with experimental data.

Controlled release formulation of an anti-depression drug based on a L-phenylalanate-zinc layered hydroxide intercalation compound

NASA Astrophysics Data System (ADS)

Hashim, Norhayati; Sharif, Sharifah Norain Mohd; Isa, Illyas Md; Hamid, Shahidah Abdul; Hussein, Mohd Zobir; Bakar, Suriani Abu; Mamat, Mazidah

2017-06-01

The intercalation of L-phenylalanate (LP) into the interlayer gallery of zinc layered hydroxide (ZLH) has been successfully executed using a simple direct reaction method. The synthesised intercalation compound, zinc layered hydroxide-L-phenylalanate (ZLH-LP), was characterised using PXRD, FTIR, CHNS, ICP-OES, TGA/DTG, FESEM and TEM. The PXRD patterns of the intercalation compound demonstrate an intense and symmetrical peak, indicating a well-ordered crystalline layered structure. The appearance of an intercalation peak at a low angle of 2θ with a basal spacing of 16.3 Å, signifies the successful intercalation of the L-phenylalanate anion into the interlayer gallery of the host. The intercalation is also validated by FTIR spectroscopy and CHNS elemental analysis. Thermogravimetric analysis confirms that the ZLH-LP intercalation compound has higher thermal stability than the pristine L-phenylalanine. The observed percentage of L-phenylalanate accumulated release varies in each release media, with 84.5%, 79.8%, 63.8% and 61.8% release in phosphate buffer saline (PBS) solution at pH 4.8, deionised water, PBS solution at pH 7.4 and NaCl solution, respectively. The release behaviour of LP from its intercalation compounds in deionised water and PBS solution at pH 4.8 follows pseudo second order, whereas in NaCl solution and PBS solution at pH 7.4, it follows the parabolic diffusion model. This study shows that the synthesised ZLH-LP intercalation compound can be used for the formation of a new generation of materials for targeted drug release with controlled release properties.

Water Retention and Rheology of Ti-doped, Synthetic Olivine

NASA Astrophysics Data System (ADS)

Faul, U.; Jackson, I.; Fitz Gerald, J. D.

2012-12-01

Upper mantle flow laws are currently based almost entirely on experiments with olivine from San Carlos in Arizona. Synthetically produced olivine enables the exploration of the effects of trace elements on the rheology. We have conducted a range of experiments in a gas medium apparatus with solution-gelation derived olivine that show that titanium is the most effective in binding water in the olivine structure. The FTIR signature of this structurally bound water is most similar to that of water-undersaturated natural olivine with absorption bands at 3575 and 3525 cm-1. Water added, titanium-free solgel contains little water after hotpressing and shows adsorption bands at wavenumbers near 3200 cm-1. Noble metal capsules such as Pt or AuPd, providing more oxidizing conditions, are more effective in retaining water. Experiments with NiFe-lined welded Pt capsules retain no more water than NiFe lined samples without Pt capsule. Water retention is, however, again dependent on trace element content, with Ti doped samples containing tens of ppm after hotpressing. By comparison undoped samples run under the same conditions contain little water, again with different FTIR spectra to Ti-doped samples. Our experiments suggest that Ti by itself, or with water contents at the FTIR detection limit enhances diffusion creep rates relative to undoped, dry solgel olivine. Water contents around 10 ppm in NiFe wrapped samples show an enhancement of strain rates of more than one order of magnitude. The addition of Ti, together with the presence of water, also enhances grain growth. For more coarse-grained samples in the dislocation creep regime the enhancement of the stain rate as a function of water content is approximately consistent with the flow laws of Hirth and Kohlstedt (2003).

Chemical composition and surfactant characteristics of marine foams investigated by means of UV-vis, FTIR and FTNIR spectroscopy.

PubMed

Mecozzi, Mauro; Pietroletti, Marco

2016-11-01

In this study, we collected the ultraviolet-visible (UV-vis), Fourier transform infrared (FTIR) and Fourier transform near-infrared (FTNIR) spectra of marine foams from different sites and foams produced by marine living organisms (i.e. algae and molluscs) to retrieve information about their molecular and structural composition. UV-vis spectra gave information concerning the lipid and pigment contents of foams. FTIR spectroscopy gave a more detailed qualitative information regarding carbohydrates, lipids and proteins in addition with information about the mineral contents of foams. FTNIR spectra confirmed the presence of carbohydrates, lipids and proteins in foams. Then, due to the higher content of structural information of FTIR spectroscopy with respect to FTNIR and UV-vis, we join the FTIR spectra of marine foams to those of humic substance from marine sediments and to the spectra of foams obtained by living organisms. We submitted this resulting FTIR spectral dataset to statistical multivariate methods to investigate specific aspects of foams such as structural similarity among foams and in addition, contributions from the organic matter of living organisms. Cluster analysis (CA) evidenced several cases (i.e. clusters) of marine foams having high structural similarity with foams from vegetal and animal samples and with humic substance extracted from sediments. These results suggested that all the living organisms of the marine environment can give contributions to the chemical composition of foams. Moreover, as CA also evidenced cases of structural differences within foam samples, we applied two-dimensional correlation analysis (2DCORR) to the FTIR spectra of marine foams to investigate the molecular characteristics which caused these structural differences. Asynchronous spectra of two-dimensional correlation analysis showed that the structural heterogeneity among foam samples depended reasonably on the presence and on the qualitative difference of electrostatic (hydrogen bonds) and nonpolar (van der Waals and π-π) interactions involving carbohydrate proteins and lipids present. The presence and relevance of these interactions agree with the supramolecular and surfactant characteristics of marine organic matter described in the scientific literature.

A Trinuclear Ni(II) Enediolate Complex: Synthesis, Characterization, and O2 Reactivity

PubMed Central

Arif, Atta M.; Berreau, Lisa M.

2009-01-01

Using a new N4-donor chelate ligand having a mixture of hydrophobic phenyl and hydrogen bond donor appendages, a trinuclear Ni(II) complex of the doubly deprotonated form of 2-hydroxy-1,3-diphenylpropane-1,3-dione was isolated, characterized (X-ray crystallography, elemental analysis, UV-vis, 1H NMR, FTIR, magnetic moment measurement), and evaluated for O2 reactivity. This complex, [(6-NA-6-Ph2TPANi)2(μ-PhC(O)C(O)C(O)Ph)2Ni](ClO4)2 (4), has two terminal pseudo octahedral Ni(II) centers supported by the tetradentate chelate ligand, and a central square planar Ni(II) ion ligated by oxygen atoms of two bridging enediolate ligands. In CH3CN, 4 exhibits a deep orange/brown color and λmax = 463 nm (ε = 16,000 M-1cm-1). The room temperature magnetic moment of 4, determined by Evans method, is μeff = 5.3(2) μB. This is consistent with the presence of two non-interacting high-spin Ni(II) centers, a diamagnetic central Ni(II) ion, and an overall quintet ground state. Exposure of a CH3CN solution of 4 to O2 results in the rapid loss of the orange/brown color to give a green solution. The products identified from this reaction are [(κ3-6-NA-6-Ph2TPA)Ni(O2Ph)(H2O)]ClO4 (5), benzil (PhC(O)C(O)Ph), and CO. Identification of 5 was achieved via its independent synthesis and comparison of its 1H NMR and mass spectral features with those of the 6-NA-6-Ph2TPA-containing product generated upon reaction of 4 with O2. The independently prepared sample of 5 was characterized by X-ray crystallography, elemental analysis, UV-vis, mass spectrometry, and FTIR. The O2 reactivity of 4 has relevance to the active site chemistry of Ni(II)-containing acireductone dioxygenase (Ni(II)-ARD). PMID:18959363

External cavity-quantum cascade laser infrared spectroscopy for secondary structure analysis of proteins at low concentrations

PubMed Central

Schwaighofer, Andreas; Alcaráz, Mirta R.; Araman, Can; Goicoechea, Héctor; Lendl, Bernhard

2016-01-01

Fourier transform infrared (FTIR) and circular dichroism (CD) spectroscopy are analytical techniques employed for the analysis of protein secondary structure. The use of CD spectroscopy is limited to low protein concentrations (<2 mg ml−1), while FTIR spectroscopy is commonly used in a higher concentration range (>5 mg ml−1). Here we introduce a quantum cascade laser (QCL)-based IR transmission setup for analysis of protein and polypeptide secondary structure at concentrations as low as 0.25 mg ml−1 in deuterated buffer solution. We present dynamic QCL-IR spectra of the temperature-induced α-helix to β-sheet transition of poly-L-lysine. The concentration dependence of the α-β transition temperature between 0.25 and 10 mg ml−1 was investigated by QCL-IR, FTIR and CD spectroscopy. By using QCL-IR spectroscopy it is possible to perform IR spectroscopic analysis in the same concentration range as CD spectroscopy, thus enabling a combined analysis of biomolecules secondary structure by CD and IR spectroscopy. PMID:27633337

External cavity-quantum cascade laser infrared spectroscopy for secondary structure analysis of proteins at low concentrations.

PubMed

Schwaighofer, Andreas; Alcaráz, Mirta R; Araman, Can; Goicoechea, Héctor; Lendl, Bernhard

2016-09-16

Fourier transform infrared (FTIR) and circular dichroism (CD) spectroscopy are analytical techniques employed for the analysis of protein secondary structure. The use of CD spectroscopy is limited to low protein concentrations (<2 mg ml(-1)), while FTIR spectroscopy is commonly used in a higher concentration range (>5 mg ml(-1)). Here we introduce a quantum cascade laser (QCL)-based IR transmission setup for analysis of protein and polypeptide secondary structure at concentrations as low as 0.25 mg ml(-1) in deuterated buffer solution. We present dynamic QCL-IR spectra of the temperature-induced α-helix to β-sheet transition of poly-L-lysine. The concentration dependence of the α-β transition temperature between 0.25 and 10 mg ml(-1) was investigated by QCL-IR, FTIR and CD spectroscopy. By using QCL-IR spectroscopy it is possible to perform IR spectroscopic analysis in the same concentration range as CD spectroscopy, thus enabling a combined analysis of biomolecules secondary structure by CD and IR spectroscopy.

A Study of the Applicability of Atomic Emission Spectroscopy (AES), Fourier Transform Infrared (FT-IR) Spectroscopy, Direct Reading and Analytical Ferrography on High Performance Aircraft Engine Lubricating Oils

DTIC Science & Technology

1998-01-01

Ferrography on High Performance Aircraft Engine Lubricating Oils Allison M. Toms, Sharon 0. Hem, Tim Yarborough Joint Oil Analysis Program Technical...turbine engines by spectroscopy (AES and FT-IR) and direct reading and analytical ferrography . A statistical analysis of the data collected is...presented. Key Words: Analytical ferrography ; atomic emission spectroscopy; condition monitoring; direct reading ferrography ; Fourier transform infrared

Differentiation of Asian ginseng, American ginseng and Notoginseng by Fourier transform infrared spectroscopy combined with two-dimensional correlation infrared spectroscopy

NASA Astrophysics Data System (ADS)

Lu, Guang-hua; Zhou, Qun; Sun, Su-qin; Leung, Kelvin Sze-yin; Zhang, Hao; Zhao, Zhong-zhen

2008-07-01

The herbal materials of Asian ginseng (the root of Panax ginseng), American ginseng (the root of Panax quinquefolius) and Notoginseng (the root of Panax notoginseng) were differentiated by conventional Fourier transform infrared spectroscopy (1D-FTIR) and two-dimensional (2D) correlation FTIR applying a thermal perturbation. Altogether 30 samples were collected and analyzed. Their entire 1D-FTIR spectra in the range of 4000-400 cm -1 and 2D-FTIR spectra in the region of 850-1530 cm -1 were generally similar based on the peaks position and intensities. This indicated the chemical constituents in these species of herbs were not distinctively different. However, variation in peak intensity were observed at about 1640 cm -1, 1416 cm -1, 1372 cm -1 and 1048 cm -1 in the 1D-FTIR spectra among these species for their ease differentiation. Clustering analysis of 1D-FTIR showed that these species located in different clusters. Much difference in their second derivative FTIR pattern among the three species also provided information for easy differentiation. These species of herbs were further identified based on the positions and intensities of relatively strong auto-peaks, positive or negative cross-peaks in their 2D-FTIR spectra. The findings provide a rapid and new operational procedure for the differentiation of these notable herbs. The visual and colorful 2D-FTIR spectra can provide dynamic structural information of chemical components in analyte and demonstrated as a powerful and useful approach for herbs identification.

Structural analysis of the industrial grade calcite

NASA Astrophysics Data System (ADS)

Shah, Rajiv P.; Raval, Kamlesh G.

2017-05-01

The chemical, optical and structural characterization of the industrial grade Calcite by EDAX, FT-IR and XRD. EDAX is a widely used technique to analyze the chemical components in a material, FT-IR stands for Fourier Transform Infra-Red, the preferred method of infrared spectroscopy. The resultant spectrum represents the molecular absorption and transmission, creating a molecular fingerprint of the sample, The atomic planes of a crystal cause an incident beam of X-rays to interfere with one another as they leave the crystal. The phenomenon is called X ray diffraction.(XRD). Data analysis of EDAX, FT-IR and XRD has been carried out with help of various instruments and software and find out the results of the these industrial grade materials which are mostly used in ceramics industries

Tortoiseshell or Polymer? Spectroscopic Analysis to Redefine a Purported Tortoiseshell Box with Gold Decorations as a Plastic Box with Brass.

PubMed

Pereira, António; Caldeira, Ana Teresa; Maduro, Belmira; Vandenabeele, Peter; Candeias, António

2016-01-01

The study and preservation of museum collections requires complete knowledge and understanding of constituent materials that can be natural, synthetic, or semi-synthetic polymers. In former times, objects were incorporated in museum collections and classified solely by their appearance. New studies, prompted by severe degradation processes or conservation-restoration actions, help shed light on the materiality of objects that can contradict the original information or assumptions. The selected case study presented here is of a box dating from the beginning of the 20th century that belongs to the Portuguese National Ancient Art Museum. Museum curators classified it as a tortoiseshell box decorated with gold applications solely on the basis of visual inspection and the information provided by the donor. This box has visible signs of degradation with white veils, initially assumed to be the result of biological degradation of a proteinaceous matrix. This paper presents the methodological rationale behind this study and proposes a totally non-invasive methodology for the identification of polymeric materials in museum artifacts. The analysis of surface leachates using (1)H and (13)C nuclear magnetic resonance (NMR) complemented by in situ attenuated total reflection infrared spectroscopy (ATR FT-IR) allowed for full characterization of the object s substratum. The NMR technique unequivocally identified a great number of additives and ATR FT-IR provided information about the polymer structure and while also confirming the presence of additives. The pressure applied during ATR FT-IR spectroscopy did not cause any physical change in the structure of the material at the level of the surface (e.g., color, texture, brightness, etc.). In this study, variable pressure scanning electron microscopy (VP-SEM-EDS) was also used to obtain the elemental composition of the metallic decorations. Additionally, microbiologic and enzymatic assays were performed in order to identify the possible biofilm composition and understand the role of microorganisms in the biodeterioration process. Using these methodologies, the box was correctly identified as being made of cellulose acetate plastic with brass decorations and the white film was identified as being composed mainly of polymer exudates, namely sulphonamides and triphenyl phosphate. © The Author(s) 2015.

A proposed origin for fossilized Pennsylvanian plant cuticles by pyrite oxidation (Sydney Coalfield, Nova Scotia, Canada)

USGS Publications Warehouse

Zodrow, E.L.; Mastalerz, Maria

2009-01-01

Fossilized cuticles, though rare in the roof rocks of coal seam in the younger part of the Pennsylvanian Sydney Coalfield, Nova Scotia, represent nearly all of the major plant groups. Selected for investigation, by methods of Fourier transform infrared spectroscopy (FTIR) and elemental analysis, are fossilized cuticles (FCs) and cuticles extracted from compressions by Schulze's process (CCs) of Alethopteris ambigua. These investigations are supplemented by FTIR analysis of FCs and CCs of Cordaites principalis, and a cuticle-fossilized medullosalean(?) axis. The purpose of this study is threefold: (1) to try to determine biochemical discriminators between FCs and CCs of the same species using semi-quantitative FTIR techniques; (2) to assess the effects chemical treatments have, particularly Schulze's process, on functional groups; and most importantly (3) to study the primary origin of FCs. Results are equivocal in respect to (1); (2) after Schulze's treatment aliphatic moieties tend to be reduced relative to oxygenated groups, and some aliphatic chains may be shortened; and (3) a primary chemical model is proposed. The model is based on a variety of geological observations, including stratal distribution, clay and pyrite mineralogies associated with FCs and compressions, and regional geological structure. The model presupposes compression-cuticle fossilization under anoxic conditions for late authigenic deposition of sub-micron-sized pyrite on the compressions. Rock joints subsequently provided conduits for oxygen-enriched ground-water circulation to initiate in situ pyritic oxidation that produced sulfuric acid for macerating compressions, with resultant loss of vitrinite, but with preservation of cuticles as FCs. The timing of the process remains undetermined, though it is assumed to be late to post-diagenetic. Although FCs represent a pathway of organic matter transformation (pomd) distinct from other plant-fossilization processes, global applicability of the chemical models remains to be tested. CCs and FCs are inferred endpoints on a spectrum of pomd which complicates assessing origin of in-between transformations (partially macerated cuticles). FCs index highly acidic levels that existed locally in the roof rocks.

Application of FT-IR spectroscopy on breast cancer serum analysis

NASA Astrophysics Data System (ADS)

Elmi, Fatemeh; Movaghar, Afshin Fayyaz; Elmi, Maryam Mitra; Alinezhad, Heshmatollah; Nikbakhsh, Novin

2017-12-01

Breast cancer is regarded as the most malignant tumor among women throughout the world. Therefore, early detection and proper diagnostic methods have been known to help save women's lives. Fourier Transform Infrared (FT-IR) spectroscopy, coupled with PCA-LDA analysis, is a new technique to investigate the characteristics of serum in breast cancer. In this study, 43 breast cancer and 43 healthy serum samples were collected, and the FT-IR spectra were recorded for each one. Then, PCA analysis and linear discriminant analysis (LDA) were used to analyze the spectral data. The results showed that there were differences between the spectra of the two groups. Discriminating wavenumbers were associated with several spectral differences over the 950-1200 cm- 1(sugar), 1190-1350 cm- 1 (collagen), 1475-1710 cm- 1 (protein), 1710-1760 cm- 1 (ester), 2800-3000 cm- 1 (stretching motions of -CH2 & -CH3), and 3090-3700 cm- 1 (NH stretching) regions. PCA-LDA performance on serum IR could recognize changes between the control and the breast cancer cases. The diagnostic accuracy, sensitivity, and specificity of PCA-LDA analysis for 3000-3600 cm- 1 (NH stretching) were found to be 83%, 84%, 74% for the control and 80%, 76%, 72% for the breast cancer cases, respectively. The results showed that the major spectral differences between the two groups were related to the differences in protein conformation in serum samples. It can be concluded that FT-IR spectroscopy, together with multivariate data analysis, is able to discriminate between breast cancer and healthy serum samples.

Pharmacokinetics Evaluation of Carbon Nanotubes Using FTIR Analysis and Histological Analysis.

PubMed

Gherman, Claudia; Tudor, Matea Cristian; Constantin, Bele; Flaviu, Tabaran; Stefan, Razvan; Maria, Bindea; Chira, Sergiu; Braicu, Cornelia; Pop, Laura; Petric, Roxana Cojocneanu; Berindan-Neagoe, Ioana

2015-04-01

Carbon nanotubes (CNTs) are biologically non-toxic and long-circulating nanostructures that have special physical properties. This study was focused on developing alternative methods that track carbon nanotubes, like FR-IR to classical tissue histological procedure. FT-IR absorption spectra were used to confirm the carboxylation of carbon nanotubes and to evaluate the presence of carbon nanotubes from bulk spleen samples and histologically prepared samples (control spleen and spleen with SWCNT-COOH). FT-IR spectrum of spleen sample from animals injected with CNTs shows major spectral differences consisting in infrared bands located at ~1173 cm(-1), ~ 1410 cm(-1); ~1658 cm(-1), ~1737 cm(-1) and around 1720 cm(-1) respectively. In terms of localization of carbon nanotubes, selective accumulation of marginal zone macrophages and splenic red pulp is observed for all treated groups, indicating the presence of carbon nanotubes even at 3, 4 and 7 days after treatment. In summary, we believe that histological evaluation and FT-IR can provide more characteristic information about the pharmacokinetcis and the clearance of carbon nanotubes.

Discrimination of edible oils and fats by combination of multivariate pattern recognition and FT-IR spectroscopy: a comparative study between different modeling methods.

PubMed

Javidnia, Katayoun; Parish, Maryam; Karimi, Sadegh; Hemmateenejad, Bahram

2013-03-01

By using FT-IR spectroscopy, many researchers from different disciplines enrich the experimental complexity of their research for obtaining more precise information. Moreover chemometrics techniques have boosted the use of IR instruments. In the present study we aimed to emphasize on the power of FT-IR spectroscopy for discrimination between different oil samples (especially fat from vegetable oils). Also our data were used to compare the performance of different classification methods. FT-IR transmittance spectra of oil samples (Corn, Colona, Sunflower, Soya, Olive, and Butter) were measured in the wave-number interval of 450-4000 cm(-1). Classification analysis was performed utilizing PLS-DA, interval PLS-DA, extended canonical variate analysis (ECVA) and interval ECVA methods. The effect of data preprocessing by extended multiplicative signal correction was investigated. Whilst all employed method could distinguish butter from vegetable oils, iECVA resulted in the best performances for calibration and external test set with 100% sensitivity and specificity. Copyright © 2012 Elsevier B.V. All rights reserved.

The influence of organic-mineral complexes on micro-elements dynamic in ecological systems of vegetables cultivation

NASA Astrophysics Data System (ADS)

Bulgariu, D.; Buzgar, N.; Bulgariu, L.; Rusu, C.; Munteanu, N.

2009-04-01

In ecological systems of vegetable cultivation (hortic antrosols; soils from greenhouses), exists an ensemble of equilibriums between organic-mineral combinations, very sensitive even to relatively small variations of physical-chemical conditions in soils. As such, these can manifest a strong influence on organic matter, clay minerals and microelements from soil, which in turn impacts on the productivity of these soils and the quality of obtained products (vegetables, fruit). Although many studies consider these organic-mineral combinations are meta-stable combinations, our work has shown that the stability of organic-mineral combinations in hortic antrosols (especially for clay-humic, clay-ironhumic combinations and chelates) is higher. We believe that this is due to the higher flexibility of these combinations' structures with the variation of chemical-mineralogical composition and physical-chemical conditions in soil. This paper highlights the results of our research on the differentiation possibility of organic-mineral complexes, depending on their structure and composition (using Raman and FT-IR spectrometry) and the influences manifested by the organic-mineral complexes on the micro-elements dynamic from ecological systems of fresh vegetable cultivation. The non-destructive separation of organic-mineral compounds from soil samples was carried out through iso-dynamic magnetic separation and extraction in aqueous two-phase systems (PEG-based). The Raman and FT-IR spectrometry analyses on raw soil samples, extracts obtained from soil samples and separated mineral fractions have been supplemented by the results obtained through chemical, microscopic and thermal analyses and by UV-VIS absorption spectrometry. Ours experimental studies have been done on representative samples of hortic antrosol from Copou glasshouse (Iasi, Romania), and was studied five micro-elements: Zn, Ni, Cu, Mn, Cr and P. The total contents of the five microelements and their fractions differential bonded on mineral and organic components of hortic antrosols, have been determined by atomic absorption spectrometry after combined sequential extraction in solid phase extraction - aqueous biphasic (PEG based) systems. The specific mechanisms of the microelements interaction with organic components have been estimated on the basis of studies realized on fractions obtained after each extraction step by Raman and FTIR spectrometry. These data have been correlated with those obtained by chemical analysis and UV-VIS spectrometry. In conditions of hortic antrosol, from total contents of Zn, Ni, Cu, Mn and Cr, more than 65 % are binding on organic components. A specific phenomenon of hortic antrosols is the microelements complexation exclusively with the functional groups of organic macromolecules. This phenomenon has two important consequences: (i) the strong fixation of microelements (these can be extracted only in very extremely conditions, which implied the organic part destroying) and (ii) their presence determined major modifications in the structure, conformation and stability of organic macromolecules. Under these conditions, the type and structure of organic-mineral compounds represent determinant factors for the dynamic of micro-elements and organic compounds in ecological systems of vegetables cultivation. Acknowledgments The authors would like to acknowledge the financial support from Romanian Ministry of Education and Research (Project PNCDI 2-D5 no. 51045/07 an Project PNCDI 2-D5 no. 52141 / 08).

In-situ ATR-FTIR and surface complexation modeling studies on the adsorption of dimethylarsenic acid and p-arsanilic acid on iron-(oxyhydr)oxides

USDA-ARS?s Scientific Manuscript database

Arsenic is an element that exists naturally in many rocks and minerals around the world. It also accumulates in petroleum, shale, oil sands and coal deposits as a result of biogeochemical processes, and it has been found in fly ash from the combustion of solid biofuels. Arsenic compounds in their o...

FTIR microspectroscopy for rapid screening and monitoring of polyunsaturated fatty acid production in commercially valuable marine yeasts and protists.

PubMed

Vongsvivut, Jitraporn; Heraud, Philip; Gupta, Adarsha; Puri, Munish; McNaughton, Don; Barrow, Colin J

2013-10-21

The increase in polyunsaturated fatty acid (PUFA) consumption has prompted research into alternative resources other than fish oil. In this study, a new approach based on focal-plane-array Fourier transform infrared (FPA-FTIR) microspectroscopy and multivariate data analysis was developed for the characterisation of some marine microorganisms. Cell and lipid compositions in lipid-rich marine yeasts collected from the Australian coast were characterised in comparison to a commercially available PUFA-producing marine fungoid protist, thraustochytrid. Multivariate classification methods provided good discriminative accuracy evidenced from (i) separation of the yeasts from thraustochytrids and distinct spectral clusters among the yeasts that conformed well to their biological identities, and (ii) correct classification of yeasts from a totally independent set using cross-validation testing. The findings further indicated additional capability of the developed FPA-FTIR methodology, when combined with partial least squares regression (PLSR) analysis, for rapid monitoring of lipid production in one of the yeasts during the growth period, which was achieved at a high accuracy compared to the results obtained from the traditional lipid analysis based on gas chromatography. The developed FTIR-based approach when coupled to programmable withdrawal devices and a cytocentrifugation module would have strong potential as a novel online monitoring technology suited for bioprocessing applications and large-scale production.

2D FTIR correlation spectroscopy and EPR analysis of Urtica dioica leaves from areas of different environmental pollution.

PubMed

Moskal, Paulina; Wesełucha-Birczyńska, Aleksandra; Łabanowska, Maria; Kurdziel, Magdalena; Filek, Maria

2018-01-15

Leaves of Urtica dioica collected from two areas of different environmental pollution were analysed by fourier transform infrared spectroscopy (FTIR) and electron paramagnetic resonance (EPR) spectroscopy. Analysis of FTIR spectra allows to describe main component of plant like proteins, lipids and carbohydrates. Although the FTIR spectra of plants from these two geographical locations of different environmental pollution appear to be relatively similar, 2D correlation shows completely different patterns. Synchronous and asynchronous correlation maps showed sequences of changes occurring during development of plant, manly in Amide I and Amide II, lignin, lipids and cellulose. In addition, 2D analysis revealed another sequence of changes as the function of plant growth depending on the degree of the environmental pollution. Two various kinds of paramagnetic species, transition metal ions (Mn(II), Fe(III)) and stable organic radicals (chlorophyll, semiquinone, tyrosyl and carbon centered) were found in leaves of nettle collected at different stages of development and growing in clean and polluted environment. In plants growing in polluted area the injuries of protein molecules bonding metal ions and the disturbances of photosynthesis and redox equilibrium in cells, as well as instability of polysaccharide structure of cell walls were observed. Copyright © 2017 Elsevier B.V. All rights reserved.

Advanced algorithms for the identification of mixtures using condensed-phase FT-IR spectroscopy

NASA Astrophysics Data System (ADS)

Arnó, Josep; Andersson, Greger; Levy, Dustin; Tomczyk, Carol; Zou, Peng; Zuidema, Eric

2011-06-01

FT-IR spectroscopy is the technology of choice to identify solid and liquid phase unknown samples. Advances in instrument portability have made possible the use of FT-IR spectroscopy in emergency response and military field applications. The samples collected in those harsh environments are rarely pure and typically contain multiple chemical species in water, sand, or inorganic matrices. In such critical applications, it is also desired that in addition to broad chemical identification, the user is warned immediately if the sample contains a threat or target class material (i.e. biological, narcotic, explosive). The next generation HazMatID 360 combines the ruggedized design and functionality of the current HazMatID with advanced mixture analysis algorithms. The advanced FT-IR instrument allows effective chemical assessment of samples that may contain one or more interfering materials like water or dirt. The algorithm was the result of years of cumulative experience based on thousands of real-life spectra sent to our ReachBack spectral analysis service by customers in the field. The HazMatID 360 combines mixture analysis with threat detection and chemical hazard classification capabilities to provide, in record time, crucial information to the user. This paper will provide an overview of the software and algorithm enhancements, in addition to examples of improved performance in mixture identification.

Analysis of Complex Carbohydrate Composition in Plant Cell Wall Using Fourier Transformed Mid-Infrared Spectroscopy (FT-IR).

PubMed

Badhan, Ajay; Wang, Yuxi; McAllister, Tim A

2017-01-01

Fourier transformed mid-infrared spectroscopy (FTIR) is a powerful tool for compositional analysis of plant cell walls (Acebes et al., Front Plant Sci 5:303, 2014; Badhan et al., Biotechnol Biofuels 7:1-15, 2014; Badhan et al., BioMed Res Int 2015: 562952, 2015; Roach et al., Plant Physiol 156:1351-1363, 2011). The infrared spectrum generates a fingerprint of a sample with absorption peaks corresponding to the frequency of vibrations between the bonds of the atoms making up the material. Here, we describe a method focused on the use of FTIR in combination with principal component analysis (PCA) to characterize the composition of the plant cell wall. This method has been successfully used to study complex enzyme saccharification processes like rumen digestion to identify recalcitrant moieties in low-quality forage which resist rumen digestion (Badhan et al., BioMed Res Int 2015: 562952, 2015), as well as to characterize cell wall mutant lines or transgenic lines expressing exogenous hydrolases (Badhan et al., Biotechnol Biofuels 7:1-15, 2014; Roach et al., Plant Physiol 156:1351-1363, 2011). The FTIR method described here facilitates high-throughput identification of the major compositional differences across a large set of samples in a low cost and nondestructive manner.

Fourier transform infrared spectroscopy combined with chemometrics for discrimination of Curcuma longa, Curcuma xanthorrhiza and Zingiber cassumunar.

PubMed

Rohaeti, Eti; Rafi, Mohamad; Syafitri, Utami Dyah; Heryanto, Rudi

2015-02-25

Turmeric (Curcuma longa), java turmeric (Curcuma xanthorrhiza) and cassumunar ginger (Zingiber cassumunar) are widely used in traditional Indonesian medicines (jamu). They have similar color for their rhizome and possess some similar uses, so it is possible to substitute one for the other. The identification and discrimination of these closely-related plants is a crucial task to ensure the quality of the raw materials. Therefore, an analytical method which is rapid, simple and accurate for discriminating these species using Fourier transform infrared spectroscopy (FTIR) combined with some chemometrics methods was developed. FTIR spectra were acquired in the mid-IR region (4000-400 cm(-1)). Standard normal variate, first and second order derivative spectra were compared for the spectral data. Principal component analysis (PCA) and canonical variate analysis (CVA) were used for the classification of the three species. Samples could be discriminated by visual analysis of the FTIR spectra by using their marker bands. Discrimination of the three species was also possible through the combination of the pre-processed FTIR spectra with PCA and CVA, in which CVA gave clearer discrimination. Subsequently, the developed method could be used for the identification and discrimination of the three closely-related plant species. Copyright © 2014 Elsevier B.V. All rights reserved.

Piper betle-mediated green synthesis of biocompatible gold nanoparticles

NASA Astrophysics Data System (ADS)

Punuri, Jayasekhar Babu; Sharma, Pragya; Sibyala, Saranya; Tamuli, Ranjan; Bora, Utpal

2012-08-01

Here, we report the novel use of the ethonolic leaf extract of Piper betle for gold nanoparticle (AuNP) synthesis. The successful formation of AuNPs was confirmed by UV-visible spectroscopy, and different parameters such as leaf extract concentration (2%), gold salt concentration (0.5 mM), and time (18 s) were optimized. The synthesized AuNPs were characterized with different biophysical techniques such as transmission electron microscopy (TEM), Fourier transform infrared (FT-IR) spectroscopy, X-ray diffraction (XRD), and energy-dispersive X-ray spectroscopy (EDX). TEM experiments showed that nanoparticles were of various shapes and sizes ranging from 10 to 35 nm. FT-IR spectroscopy revealed that AuNPs were functionalized with biomolecules that have primary amine group -NH2, carbonyl group, -OH groups, and other stabilizing functional groups. EDX showed the presence of the elements on the surface of the AuNPs. FT-IR and EDX together confirmed the presence of biomolecules bounded on the AuNPs. Cytotoxicity of the AuNPs was tested on HeLa and MCF-7 cancer cell lines, and they were found to be nontoxic, indicating their biocompatibility. Thus, synthesized AuNPs have potential for use in various biomedical applications.

Glycolysis of carbon fiber-epoxy unidirectional mat catalysed by sodium hydroxide

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zaini, Mariana Binti Mohd; Badri, Khairiah Haji

2014-09-03

This study was conducted to recycle carbon fibre-epoxy (CFRP) composite in woven sheet/ mat form. The CFRP was recycled through glycolysis with polyethlyene glycol (PEG 200) as the solvent. The CFRP was loaded into the solvent at a ratio of 4:1 (w/w). PEG200 was diluted with water to a ratio of 80:20 (v/v). This reaction was catalysed by sodium hydroxide (NaOH) solution with varying concentrations at 1.5, 1.7 and 1.9% (w/v). The glycolysis was conducted at 180-190 °C. The recovered CF (rCF) was analysed using Fourier Transform Infrared (FTIR), Scanning Electron Microscopy (SEM) and Energy Dispersive X-Ray (EDX) while themore » degraded solution was analysed using FTIR and the epoxy content was determined. The FTIR spectrum of the rCF exhibited the disappearance of the COC peak belonged to epoxy and supported by the SEM micrographs that showed clear rCF. On the other hand, the analysed filtrate detected the disappearance of oxygen peak element in the EDX spectrum for all rCF samples. This gave an indication that the epoxy resin has been removed from the surface of the carbon fiber.« less

Glycolysis of carbon fiber-epoxy unidirectional mat catalysed by sodium hydroxide

NASA Astrophysics Data System (ADS)

Zaini, Mariana Binti Mohd; Badri, Khairiah Haji

2014-09-01

This study was conducted to recycle carbon fibre-epoxy (CFRP) composite in woven sheet/ mat form. The CFRP was recycled through glycolysis with polyethlyene glycol (PEG 200) as the solvent. The CFRP was loaded into the solvent at a ratio of 4:1 (w/w). PEG200 was diluted with water to a ratio of 80:20 (v/v). This reaction was catalysed by sodium hydroxide (NaOH) solution with varying concentrations at 1.5, 1.7 and 1.9% (w/v). The glycolysis was conducted at 180-190 °C. The recovered CF (rCF) was analysed using Fourier Transform Infrared (FTIR), Scanning Electron Microscopy (SEM) and Energy Dispersive X-Ray (EDX) while the degraded solution was analysed using FTIR and the epoxy content was determined. The FTIR spectrum of the rCF exhibited the disappearance of the COC peak belonged to epoxy and supported by the SEM micrographs that showed clear rCF. On the other hand, the analysed filtrate detected the disappearance of oxygen peak element in the EDX spectrum for all rCF samples. This gave an indication that the epoxy resin has been removed from the surface of the carbon fiber.

Surveillance system for air pollutants by combination of the decision support system COMPAS and optical remote sensing systems

NASA Astrophysics Data System (ADS)

Flassak, Thomas; de Witt, Helmut; Hahnfeld, Peter; Knaup, Andreas; Kramer, Lothar

1995-09-01

COMPAS is a decision support system designed to assist in the assessment of the consequences of accidental releases of toxic and flammable substances. One of the key elements of COMPAS is a feedback algorithm which allows us to calculate the source term with the aid of concentration measurements. Up to now the feedback technique is applied to concentration measurements done with test tubes or conventional point sensors. In this paper the extension of the actual method is presented which is the combination of COMPAS and an optical remote sensing system like the KAYSER-THREDE K300 FTIR system. Active remote sensing methods based on FTIR are, among other applications, ideal for the so-called fence line monitoring of the diffuse emissions and accidental releases from industrial facilities, since from the FTIR spectra averaged concentration levels along the measurement path can be achieved. The line-averaged concentrations are ideally suited as on-line input for COMPAS' feedback technique. Uncertainties in the assessment of the source term related with both shortcomings of the dispersion model itself and also problems of a feedback strategy based on point measurements are reduced.

Label-Free Determination of Protein Binding in Aqueous Solution using Overlayer Enhanced Attenuated Total Reflectance Fourier Transform Infrared Spectroscopy (OE-ATR-FTIR)

NASA Astrophysics Data System (ADS)

Ruthenburg, Travis; Aweda, Tolulope; Park, Simon; Meares, Claude; Land, Donald

2009-03-01

Protein binding/affinity studies are often performed using Surface Plasmon Resonance techniques that don't produce much spectral information. Measurement of protein binding affinity using FTIR is traditionally performed using high protein concentration or deuterated solvent. By immobilizing a protein near the surface of a gold-coated germanium internal reflection element interactions can be measured between an immobilized protein and free proteins or small molecules in aqueous solution. By monitoring the on and off rates of these interactions, the dissociation constant for the system can be determined. The dissociation constant for the molecule Yttrium-DOTA binding to the antibody 2D12.5 system was determined to be 100nM. Results will also be presented from our measurements of Bovine Serum Albumin (BSA) binding to anti-BSA.

Synthesis and structural study on (1E,2E,1'E,2'E)-3,3'-bis[(4-bromophenyl)-3,3'-(4-methy-1,2-phenylene diimine)] acetaldehyde dioxime: A combined experimental and theoretical study

NASA Astrophysics Data System (ADS)

Topal, T.; Kart, H. H.; Tunay Taşlı, P.; Karapınar, E.

2015-06-01

Tetradentate (1E,2E,1'E,2'E)-3,3'-bis[(4-bromophenyl)-3,3'-(4-methy-1,2-phenylene diimine)] acetaldehyde dioxime which possess N4 donor sets derived from the condensation of isonitroso- p-bromoacetophenone and 3,4-diaminotoluene are synthesized and characterized. The characterization of tetradentate Schiff base ligand has been deduced from LC-MS, FTIR, 13C and 1H NMR spectra and elemental analysis. Furthermore, the molecular geometry, infrared and NMR spectra of the title molecule in the ground state have been calculated by using the quantum chemical computational methods such as density functional theory (DFT) and ab initio Hartree-Fock (HF) methods with the 6-31G(d) and 6-311G(d) basis sets. The computed bond lengths and bond angles by using the both methods show the good agreement with each other. Moreover, the vibrational frequencies have been calculated and the scaled values have been compared with the experimental FTIR spectroscopic data. Assignments of the vibrational modes are made on the basis of potential energy distribution (PED) calculated from by using VEDA program. The correlations between the observed and calculated frequencies are in good agreement with each other as well as the correlation of the NMR data.

Syntheses, spectroscopic and thermal analyses of cyanide bridged heteronuclear polymeric complexes: [M(L)2Ni(CN)4]n (Ldbnd N-methylethylenediamine or N-ethylethylenediamine; Mdbnd Ni(II), Cu(II), Zn(II) or Cd(II))

NASA Astrophysics Data System (ADS)

Karaağaç, Dursun; Kürkçüoğlu, Güneş Süheyla

2016-02-01

Polymeric tetracyanonickelate(II) complexes of the type [M(L)2Ni(CN)4]n (Ldbnd N-methylethylenediamine (men) or N-ethylethylenediamine (neen); Mdbnd Ni(II), Cu(II), Zn(II) or Cd(II)) have been prepared and characterized by FT-IR, Raman spectroscopy, thermal and elemental analysis techniques. Additionally, FT-IR and Raman spectral analyses of men and neen have experimentally and theoretically investigated in the range of 4000-250 cm-1. The corresponding vibration assignments of men and neen are performed by using B3LYP density functional theory (DFT) method together with 6-31 G(d) basis set. The spectral features of the complexes suggest that the coordination environment of the M(II) ions are surrounded by the two symmetry related men and neen ligands and the two symmetry related N atom of cyanide groups, whereas the Ni(II) atoms are coordinated with a square-planar to four C atoms of the cyanide groups. Polymeric structures of the complexes consist of one dimensional alternative chains of [M(L)2]2+ and [Ni(CN)4]2- moieties. The thermal decompositions in the temperature range 30-700 °C of the complexes were investigated in the static air atmosphere.

Synthesis, single crystal X-ray, spectroscopic (FT-IR, UV-vis, fluorescence, 1H &13C NMR), computational (DFT/B3LYP) studies of some imidazole based picrates

NASA Astrophysics Data System (ADS)

Arockia doss, M.; Rajarajan, G.; Thanikachalam, V.; Selvanayagam, S.; Sridhar, B.

2018-04-01

2,4,5-triphenyl-1H-imidazol-3-ium picrate (1), 2-(4-fluorophenyl)-4,5-diphenyl-1H-imidazol-3-ium picrate (2), 2-(4-methylphenyl)-4,5-diphenyl-1H-imidazol-3-ium picrate (3) were synthesised. These compounds 1-3 were characterized by elemental, FT-IR, 1H NMR and 13C NMR analyses. The structure of compound 3 was further confirmed by single crystal X-ray diffraction. The studies reveal that the molecule is associated with weak Nsbnd H⋯O and Csbnd H⋯N and van der Waals interactions which are responsible for the formation and strengthening of supramolecular assembly. The nature of the interactions and their importance are explored using the Hirshfeld surface method. The physicochemical properties of the compounds 1-3 were evaluated by UV-vis spectroscopy, fluorescence spectroscopy, and thermogravimetric analysis. According to thermal data the salts possess excellent thermal stabilities with decomposition temperatures ranging from 220 to 280 °C. Second-harmonic generation (SHG) results exposed that the picrates 1-3 were about 1.13-1.50 times greater than potassium dihydrogen phosphate (KDP). Here we also used Density functional theory (DFT) calculations in order to investigate the opto-electronic properties. The obtained theoretical results validate with available experimental data.

Green synthesis of nano sized transition metal complexes containing heterocyclic Schiff base: Structural and morphology characterization and bioactivity study

NASA Astrophysics Data System (ADS)

Jawoor, Shailaja S.; Patil, Sangamesh A.; Kumbar, Mahantesh; Ramawadgi, Prashant B.

2018-07-01

In the current involvement of our research work in coordination chemistry, novel transition metal complexes were synthesized from regular reflux method and hydrothermal method using Schiff base prepared via condensation of ethyl 2-amino-4,5,6,7-tetrahydrobenzo[b]thiophene-3-carboxylate with 8-carbaldehyde-7-hydroxy-4-methylcoumarin. All the synthesized compounds were interpreted using different analytical, physicochemical and spectral methods such as magnetic moment measurement, FT-IR, 1H and 13C NMR, GCMS/ESI-MS, UV/Vis spectroscopy and TGA. The size and morphology of the nano metal complexes were determined using atomic force microscope (AFM), field emission scanning electron spectroscopy (FE-SEM) and X-ray powder diffraction (PXRD). The non-electrolytic nature of the metal complexes was confirmed by molar conductance studies. The obtained FT-IR data supports the binding of metal ion to Schiff base. Elemental analysis study suggests [ML2(H2O)2] stoichiometry, here M = Co(II), Ni(II) and Cu(II), L = deprotonated ligand. Electronic spectral results reveal six-coordinated geometry for the synthesized metal complexes. All the tested compounds show good DNA cleavage (Calf Thymus DNA) and in vitro anticancer activity (PA-I cell line), the activity results for the tested compounds are prominent and compound 9 exhibited a little enhanced activity than the other tested compounds.

FT-IR imaging for quantitative determination of liver fat content in non-alcoholic fatty liver.

PubMed

Kochan, K; Maslak, E; Chlopicki, S; Baranska, M

2015-08-07

In this work we apply FT-IR imaging of large areas of liver tissue cross-section samples (∼5 cm × 5 cm) for quantitative assessment of steatosis in murine model of Non-Alcoholic Fatty Liver (NAFLD). We quantified the area of liver tissue occupied by lipid droplets (LDs) by FT-IR imaging and Oil Red O (ORO) staining for comparison. Two alternative FT-IR based approaches are presented. The first, straightforward method, was based on average spectra from tissues and provided values of the fat content by using a PLS regression model and the reference method. The second one – the chemometric-based method – enabled us to determine the values of the fat content, independently of the reference method by means of k-means cluster (KMC) analysis. In summary, FT-IR images of large size liver sections may prove to be useful for quantifying liver steatosis without the need of tissue staining.

A rapid Fourier-transform infrared (FTIR) spectroscopic method for direct quantification of paracetamol content in solid pharmaceutical formulations

NASA Astrophysics Data System (ADS)

Mallah, Muhammad Ali; Sherazi, Syed Tufail Hussain; Bhanger, Muhammad Iqbal; Mahesar, Sarfaraz Ahmed; Bajeer, Muhammad Ashraf

2015-04-01

A transmission FTIR spectroscopic method was developed for direct, inexpensive and fast quantification of paracetamol content in solid pharmaceutical formulations. In this method paracetamol content is directly analyzed without solvent extraction. KBr pellets were formulated for the acquisition of FTIR spectra in transmission mode. Two chemometric models: simple Beer's law and partial least squares employed over the spectral region of 1800-1000 cm-1 for quantification of paracetamol content had a regression coefficient of (R2) of 0.999. The limits of detection and quantification using FTIR spectroscopy were 0.005 mg g-1 and 0.018 mg g-1, respectively. Study for interference was also done to check effect of the excipients. There was no significant interference from the sample matrix. The results obviously showed the sensitivity of transmission FTIR spectroscopic method for pharmaceutical analysis. This method is green in the sense that it does not require large volumes of hazardous solvents or long run times and avoids prior sample preparation.

Detection and identification of explosive particles in fingerprints using attenuated total reflection-Fourier transform infrared spectromicroscopy.

PubMed

Mou, Yongyan; Rabalais, J Wayne

2009-07-01

The application of attenuated total reflection (ATR)-Fourier transform infrared (FTIR) spectromicroscopy for detection of explosive particles in fingerprints is described. The combined functions of ATR-FTIR spectromicroscopy are visual searching of particles in fingerprints and measuring the FTIR spectra of the particles. These functions make it possible to directly identify whether a suspect has handled explosives from the fingerprints alone. Particles in explosive contaminated fingerprints are either ingredients of the explosives, finger residues, or other foreign materials. These cannot normally be discriminated by their morphology alone. ATR-FTIR spectra can provide both particle morphology and composition. Fingerprints analyzed by ATR-FTIR can be used for further analysis and identification because of its non-destructive character. Fingerprints contaminated with three different types of explosives, or potential explosives, have been analyzed herein. An infrared spectral library was searched in order to identify the explosive residues. The acquired spectra are compared to those of finger residue alone, in order to differentiate such residue from explosive residue.

Distinction of broken cellular wall Ganoderma lucidum spores and G. lucidum spores using FTIR microspectroscopy

NASA Astrophysics Data System (ADS)

Chen, Xianliang; Liu, Xingcun; Sheng, Daping; Huang, Dake; Li, Weizu; Wang, Xin

2012-11-01

In this paper, FTIR microspectroscopy was used to identify broken cellular wall Ganoderma lucidum spores and G. lucidum spores. For IR spectra, broken cellular wall G. lucidum spores and G. lucidum spores were mainly different in the regions of 3000-2800, 1660-1600, 1400-1200 and 1100-1000 cm-1. For curve fitting, the results showed the differences in the protein secondary structures and the polysaccharide structures/content between broken cellular wall G. lucidum spores and G. lucidum spores. Moreover, the value of A1078/A1741 might be a potentially useful factor to distinguish broken cellular wall G. lucidum spores from G. lucidum spores. Additionally, FTIR microspectroscopy could identify broken cellular wall G. lucidum spores and G. lucidum spores accurately when it was combined with hierarchical cluster analysis. The result suggests FTIR microspectroscopy is very simple and efficient for distinction of broken cellular wall G. lucidum spores and G. lucidum spores. The result also indicates FTIR microspectroscopy may be useful for TCM identification.

Identifying Plant Part Composition of Forest Logging Residue Using Infrared Spectral Data and Linear Discriminant Analysis

PubMed Central

Acquah, Gifty E.; Via, Brian K.; Billor, Nedret; Fasina, Oladiran O.; Eckhardt, Lori G.

2016-01-01

As new markets, technologies and economies evolve in the low carbon bioeconomy, forest logging residue, a largely untapped renewable resource will play a vital role. The feedstock can however be variable depending on plant species and plant part component. This heterogeneity can influence the physical, chemical and thermochemical properties of the material, and thus the final yield and quality of products. Although it is challenging to control compositional variability of a batch of feedstock, it is feasible to monitor this heterogeneity and make the necessary changes in process parameters. Such a system will be a first step towards optimization, quality assurance and cost-effectiveness of processes in the emerging biofuel/chemical industry. The objective of this study was therefore to qualitatively classify forest logging residue made up of different plant parts using both near infrared spectroscopy (NIRS) and Fourier transform infrared spectroscopy (FTIRS) together with linear discriminant analysis (LDA). Forest logging residue harvested from several Pinus taeda (loblolly pine) plantations in Alabama, USA, were classified into three plant part components: clean wood, wood and bark and slash (i.e., limbs and foliage). Five-fold cross-validated linear discriminant functions had classification accuracies of over 96% for both NIRS and FTIRS based models. An extra factor/principal component (PC) was however needed to achieve this in FTIRS modeling. Analysis of factor loadings of both NIR and FTIR spectra showed that, the statistically different amount of cellulose in the three plant part components of logging residue contributed to their initial separation. This study demonstrated that NIR or FTIR spectroscopy coupled with PCA and LDA has the potential to be used as a high throughput tool in classifying the plant part makeup of a batch of forest logging residue feedstock. Thus, NIR/FTIR could be employed as a tool to rapidly probe/monitor the variability of forest biomass so that the appropriate online adjustments to parameters can be made in time to ensure process optimization and product quality. PMID:27618901

Investigating the origins of rhythmic major-element zoning in HP/LT garnets from worldwide subduction mélanges

NASA Astrophysics Data System (ADS)

Viete, D. R.; Hacker, B. R.; Seward, G.; Allen, M. B.

2016-12-01

Rhythmic major-element zoning has been documented in garnets from high pressure/low temperature (HP/LT) lenses within a number of worldwide subduction mélanges (e.g. California, Chinese Tianshan, Cuba, Greek Cyclades, Guatemala, Japan, Venezuela). The origin of these features has implications for the nature of subduction-zone processes. Conditions of rhythmic zoning acquirement in HP/LT garnets of California and Venezuela were investigated by use of Raman and FTIR microspectroscopy, and thermodynamic modelling of phase equilibria. Quartz-in-garnet Raman barometry reveals varying P—on the order of 100­-300 MPa, over radial distances of 10s of µm—in association with the high-Mn (and low-Mg) bands that define the fine-scale rhythmic zoning. Results from FTIR microspectroscopy demonstrate association between the high-Mn bands and locally depressed (structural) OH and elevated (molecular) H2O concentrations. The microspectroscopy results suggest changes in P and fluid activity attended development of the cryptic rhythmic zoning. Perple_X modelling of phase equilibria shows that, for specific rock chemistry and subduction P-T conditions, garnet modal abundance is extremely sensitive to changes in P (e.g. 10-20 vol.% growth/dissolution for ΔP = 200 MPa). Rhythmic major-element zoning may reflect P- and/or fluid-driven cycles of garnet stability-instability and/or varying reaction progress/kinetics during subduction. Steep compositional gradients that define the rhythmic major-element zoning limit time scales at subduction T, requiring that such individual stability-instability and/or accelerated reaction cycles were extremely brief. Seismic cycles or porosity waves represent ephemeral phenomena capable of accounting for development of rhythmic major-element zoning in HP/LT garnet, during subduction, as a result of fluctuations in both P and fluids. Metamorphic rocks may well carry detailed records of the catastrophism that punctuates longer-term tectonometamorphic processes.

Glycine and metformin as new counter ions for mono and dinuclear vanadium(V)-dipicolinic acid complexes based on the insulin-enhancing anions: Synthesis, spectroscopic characterization and crystal structure

NASA Astrophysics Data System (ADS)

Ghasemi, Fatemeh; Rezvani, Ali Reza; Ghasemi, Khaled; Graiff, Claudia

2018-02-01

Complexes [VO(dipic) (H2O)2]·2H2O (1), [H2Met][V2O4(dipic)2] (2) and [HGly][VO2(dipic)] (3), where H2dipic = 2,6-pyridinedicarboxylic acid, Met = Metformin (N,N-dimethylbiguanide) and Gly = glycine, were synthesized. The three complexes were characterized by elemental analysis, FTIR, 1H and 13C NMR, and UV-Vis spectroscopy. Solid-state structures of (2) and (3) were determined by single-crystal X-ray diffraction analysis. The coordination geometry around the vanadium atoms in 2 is octahedral, while the coordination geometry in 3 is between trigonal bipyramidal and squared pyramidal. In the binuclear complex 2 and mononuclear complex 3, metformin and glycine are diprotonated and monoprotonated respectively, and act as a counter ion. The redox behavior of the complexes was also investigated by cyclic voltammetry.

Site-Selective Modification of Cellulose Nanocrystals with Isophorone Diisocyanate and Formation of Polyurethane-CNC Composites.

PubMed

Girouard, Natalie M; Xu, Shanhong; Schueneman, Gregory T; Shofner, Meisha L; Meredith, J Carson

2016-01-20

The unequal reactivity of the two isocyanate groups in an isophorone diisocyante (IPDI) monomer was exploited to yield modified cellulose nanocrystals (CNCs) with both urethane and isocyanate functionality. The chemical functionality of the modified CNCs was verified with ATR-FTIR analysis and elemental analysis. The selectivity for the secondary isocyanate group using dibutyl tin dilaurate (DBTDL) as the reaction catalyst was confirmed with (13)C NMR. The modified CNCs showed improvements in the onset of thermal degradation by 35 °C compared to the unmodified CNCs. Polyurethane composites based on IPDI and a trifunctional polyether alcohol were synthesized using unmodified (um-CNC) and modified CNCs (m-CNC). The degree of nanoparticle dispersion was qualitatively assessed with polarized optical microscopy. It was found that the modification step facilitated superior nanoparticle dispersion compared to the um-CNCs, which resulted in increases in the tensile strength and work of fracture of over 200% compared to the neat matrix without degradation of elongation at break.

New Insights into CO2 Adsorption on Layered Double Hydroxide (LDH)-Based Nanomaterials

NASA Astrophysics Data System (ADS)

Tang, Nian; He, Tingyu; Liu, Jie; Li, Li; Shi, Han; Cen, Wanglai; Ye, Zhixiang

2018-02-01

The interlamellar spacing of layered double hydroxides (LDHs) was enlarged by dodecyl sulfonate ions firstly, and then, (3-aminopropyl)triethoxysilane (APS) was chemically grafted (APS/LDHs). The structural characteristics and thermal stability of these prepared samples were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), reflectance Fourier transform infrared spectrometer (FTIR), thermogravimetric analysis (TG), and elemental analysis (EA) respectively. The CO2 adsorption performance was investigated adopting TG and diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS). The results presented that the CO2 adsorption capacity on APS/LDHs was as high as 90 mg/g and showed no obvious reduction during a five cyclic adsorption-desorption test, indicating its superior performance stability. The DRIFTS results showed that both carbamates and weakly bounded CO2 species were generated on APS/LDHs. The weakly adsorbed species was due to the different local chemical environment for CO2 capture provided by the surface moieties of LDHs like free silanol and hydrogen bonds.

Crystal Structure and Antitumor Activity of the Novel Zwitterionic Complex of tri-n-Butyltin(IV) with 2-Thiobarbituric Acid

PubMed Central

Balas, Vasilios I.; Hadjikakou, Sotiris K.; Hadjiliadis, Nick; Kourkoumelis, Nikolaos; Light, Mark E.; Hursthouse, Mike; Metsios, Apostolos K.; Karkabounas, Spyros

2008-01-01

A novel tri-n-butyl(IV) derivative of 2-thiobarbituric acid (HTBA) of formula [(n-Bu)3Sn(TBA) H2O] (1) has been synthesized and characterized by elemental analysis and 119Sn-NMR and FT-IR spectroscopic techniques. The crystal structure of complex 1 has been determined by single crystal X-ray diffraction analysis at 120(2) K. The geometry around Sn(IV) is trigonal bipyramidal. Three n-butyl groups and one oxygen atom from a deprotonated 2-thiobarbituric ligand are bonded to the metal center. The geometry is completed with one oxygen from a water molecule. Compound 1 exhibits potent, in vitro, cytotoxicity against sarcoma cancer cells (mesenchymal tissue) from the Wistar rat, polycyclic aromatic hydrocarbons (PAH, benzo[a]pyrene) carcinogenesis. In addition, the inhibition caused by 1, in the rate of lipoxygenase (LOX) catalyzed oxidation reaction of linoleic acid to hyperoxolinoleic acid, has been also kinetically and theoretically studied. The results are compared to that of cisplatin. PMID:18401456

Tuning effect of polysaccharide Chitosan on structural, morphological, optical and photoluminescence properties of ZnO nanoparticles

NASA Astrophysics Data System (ADS)

Magesh, G.; Bhoopathi, G.; Nithya, N.; Arun, A. P.; Ranjith Kumar, E.

2018-05-01

Chitosan/ZnO nanocomposites was synthesized by in-situ chemical precipitation method. The effect of polysaccharide Chitosan concentration (0.1 g, 0.5 g, 1 g and 3 g) was investigated by X-ray diffraction (XRD), Field Emission Scanning Electron Microscopy (FESEM) with Energy dispersive spectroscopy (EDX), High Resolution Transmission Electron Microscopy (HRTEM), UV-visible (UV), Fourier Transform Infrared (FTIR) and Photoluminescence Spectroscopy (PL). XRD pattern confirms the hexagonal wurtzite structure of the Chitosan/ZnO nanocomposites. The structural morphology and the elemental composition of the samples were analysed by FESEM and EDX respectively. From TEM analysis, it is observed that the particles in spindle shape morphology with average particle size ranges 10-20 nm. UV-Vis analysis reveals that the Chitosan concentration affect the absorption band edge and shift towards lower wavelength. The oxygen vacancy induced photoluminescence of ZnO nanoparticles was observed and its intensity decreases by tuning the Chitosan concentration.

Synthesis, structural, spectroscopic and optical studies of charge transfer complex salts.

PubMed

Manikandan, Maruthappan; Mahalingam, Thaiyan; Hayakawa, Yasuhiro; Ravi, Ganesan

2013-01-15

New charge transfer molecular complex adducts of picric acid (C6H3N3O7) with triethylamine (C6H15N) and dimethylformamide (HCON(CH3)2) were synthesized successfully for the first time. Chemical composition and stoichiometry of the synthesized complex salts were verified by CHN elemental analysis. Solubility of the complex salts have been determined by gravimetric method and single crystals of two new salts were grown by low temperature solution growth technique. Crystal system, crystalline nature and cell parameters of the grown crystals were determined by single crystal X-ray diffraction (SXRD) and powder X-ray diffraction (PXRD) analyses. The formations of the charge-transfer complex, functional groups and the modes of vibrations have been confirmed by Fourier transform infrared (FTIR) spectroscopy. In order to know the linear and nonlinear optical suitability for device fabrication, UV-Vis (UV) spectral analysis and relative second harmonic generation (SHG) efficiency test were performed for the grown crystals. Copyright © 2012 Elsevier B.V. All rights reserved.

Spent coffee-based activated carbon: specific surface features and their importance for H2S separation process.

PubMed

Kante, Karifala; Nieto-Delgado, Cesar; Rangel-Mendez, J Rene; Bandosz, Teresa J

2012-01-30

Activated carbons were prepared from spent ground coffee. Zinc chloride was used as an activation agent. The obtained materials were used as a media for separation of hydrogen sulfide from air at ambient conditions. The materials were characterized using adsorption of nitrogen, elemental analysis, SEM, FTIR, and thermal analysis. Surface features of the carbons depend on the amount of an activation agent used. Even though the residual inorganic matter takes part in the H(2)S retention via salt formation, the porous surface of carbons governs the separation process. The chemical activation method chosen resulted in formation of large volume of pores with sizes between 10 and 30Å, optimal for water and hydrogen sulfide adsorption. Even though the activation process can be optimized/changed, the presence of nitrogen in the precursor (caffeine) is a significant asset of that specific organic waste. Nitrogen functional groups play a catalytic role in hydrogen sulfide oxidation. Copyright © 2011 Elsevier B.V. All rights reserved.

Pyrolysis of Date palm waste in a fixed-bed reactor: Characterization of pyrolytic products.

PubMed

Bensidhom, Gmar; Ben Hassen-Trabelsi, Aïda; Alper, Koray; Sghairoun, Maher; Zaafouri, Kaouther; Trabelsi, Ismail

2018-01-01

The pyrolysis of several Tunisian Date Palm Wastes (DPW): Date Palm Rachis (DPR), Date Palm Leaflets (DPL), Empty Fruit Bunches (EFB) and Date Palm Glaich (DPG) was run using a fixed-bed reactor, from room temperature to 500°C, with 15°C/min as heating rate and -5°C as condensation temperature, in order to produce bio-oil, biochar and syngas. In these conditions, the bio-oil yield ranges from 17.03wt% for DPL to 25.99wt% for EFB. For the biochar, the highest yield (36.66wt%) was obtained for DPL and the lowest one (31.66wt%) was obtained from DPG while the syngas production varies from 39.10wt% for DPR to 46.31wt% DPL. The raw material and pyrolysis products have been characterized using elemental analysis thermogravimetric analysis (TGA), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM). The syngas composition has been characterized using gas analyzer. Copyright © 2017 Elsevier Ltd. All rights reserved.

A combined experimental and DFT investigation of disazo dye having pyrazole skeleton

NASA Astrophysics Data System (ADS)

Şener, Nesrin; Bayrakdar, Alpaslan; Kart, Hasan Hüseyin; Şener, İzzet

2017-02-01

Disazo dye containing pyrazole skeleton has been synthesized. The structure of the dye has been confirmed by using FT-IR, 1H NMR, 13C NMR, HRMS spectral technique and elemental analysis. The molecular geometry and infrared spectrum are also calculated by the Density Functional Theory (DFT) employing B3LYP level with 6-311G (d,p) basis set. The chemical shifts calculation for 1H NMR of the title molecule is done by using by Gauge-Invariant Atomic Orbital (GIAO) method by utilizing the same basis sets. The total density of state, the partial density of state and the overlap population density of state diagram analysis are done via Gauss Sum 3.0 program. Frontier molecular orbitals such as highest occupied molecular orbital (HOMO) and lowest unoccupied molecular orbital (LUMO) and molecular electrostatic potential surface on the title molecule are predicted for various intramolecular interactions that are responsible for the stabilization of the molecule. The experimental results and theoretical values have been compared.

Synthesis and characterization of boric acid mediated metal-organic frameworks based on trimesic acid and terephthalic acid

NASA Astrophysics Data System (ADS)

Ozer, Demet; Köse, Dursun A.; Şahin, Onur; Oztas, Nursen Altuntas

2017-08-01

The new metal-organic framework materials based on boric acid reported herein. Sodium and boron containing metal-organic frameworks were synthesized by one-pot self-assembly reaction in the presence of trimesic acid and terephthalic acid in water/ethanol solution. Boric acid is a relatively cheap boron source and boric acid mediated metal-organic framework prepared mild conditions compared to the other boron source based metal-organic framework. The synthesized compounds were characterized by FT-IR, p-XRD, TGA/DTA, elemental analysis, 13C-MAS NMR, 11B-NMR and single crystal measurements. The molecular formulas of compounds were estimated as C18H33B2Na5O28 and C8H24B2Na2O17 according to the structural analysis. The obtained complexes were thermally stable. Surface properties of inorganic polymer complexes were investigated by BET analyses and hydrogen storage properties of compound were also calculated.

Ferrocenylaniline based amide analogs of methoxybenzoic acids: Synthesis, structural characterization and butyrylcholinesterase (BChE) inhibition studies

NASA Astrophysics Data System (ADS)

Altaf, Ataf Ali; Kausar, Samia; Hamayun, Muhammad; Lal, Bhajan; Tahir, Muhammad Nawaz; Badshah, Amin

2017-10-01

Three new ferrocene based amides were synthesized with slight structural difference. The general formula of the amides is C5H5FeC5H4C6H4NHCOC6H4(OCH3). The synthesized compounds were characterized by instrumental techniques like elemental analysis, FTIR and NMR spectroscopy. Structure of the two compounds was also studied by single crystal X-rays diffraction analysis. Structural studies provide the evidence that pMeO (one of the synthesized compounds) is an example of amides having no intermolecular hydrogen bonding in solid structure. In the BChE inhibition assay, compound (oMeO) having strong intermolecular force in the solid structure is less active than the compound (pMeO) with weak intermolecular forces in the solid structure. The docking studies proved that hydrogen bonding between inhibitor and BChE enzyme is of more importance for the activity, rather than intermolecular hydrogen bonding in the solid structure of inhibitor.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hornemann, Andrea, E-mail: andrea.hornemann@ptb.de; Hoehl, Arne, E-mail: arne.hoehl@ptb.de; Ulm, Gerhard, E-mail: gerhard.ulm@ptb.de

Bio-diagnostic assays of high complexity rely on nanoscaled assay recognition elements that can provide unique selectivity and design-enhanced sensitivity features. High throughput performance requires the simultaneous detection of various analytes combined with appropriate bioassay components. Nanoparticle induced sensitivity enhancement, and subsequent multiplexed capability Surface-Enhanced InfraRed Absorption (SEIRA) assay formats are fitting well these purposes. SEIRA constitutes an ideal platform to isolate the vibrational signatures of targeted bioassay and active molecules. The potential of several targeted biolabels, here fluorophore-labeled antibody conjugates, chemisorbed onto low-cost biocompatible gold nano-aggregates substrates have been explored for their use in assay platforms. Dried films were analyzedmore » by synchrotron radiation based FTIR/SEIRA spectro-microscopy and the resulting complex hyperspectral datasets were submitted to automated statistical analysis, namely Principal Components Analysis (PCA). The relationships between molecular fingerprints were put in evidence to highlight their spectral discrimination capabilities. We demonstrate that robust spectral encoding via SEIRA fingerprints opens up new opportunities for fast, reliable and multiplexed high-end screening not only in biodiagnostics but also in vitro biochemical imaging.« less

Synthesis, structural, spectroscopic and optical studies of charge transfer complex salts

NASA Astrophysics Data System (ADS)

Manikandan, Maruthappan; Mahalingam, Thaiyan; Hayakawa, Yasuhiro; Ravi, Ganesan

2013-01-01

New charge transfer molecular complex adducts of picric acid (C6H3N3O7) with triethylamine (C6H15N) and dimethylformamide (HCON(CH3)2) were synthesized successfully for the first time. Chemical composition and stoichiometry of the synthesized complex salts were verified by CHN elemental analysis. Solubility of the complex salts have been determined by gravimetric method and single crystals of two new salts were grown by low temperature solution growth technique. Crystal system, crystalline nature and cell parameters of the grown crystals were determined by single crystal X-ray diffraction (SXRD) and powder X-ray diffraction (PXRD) analyses. The formations of the charge-transfer complex, functional groups and the modes of vibrations have been confirmed by Fourier transform infrared (FTIR) spectroscopy. In order to know the linear and nonlinear optical suitability for device fabrication, UV-Vis (UV) spectral analysis and relative second harmonic generation (SHG) efficiency test were performed for the grown crystals.

Synthesis of zinc sulfide nanoparticles and their incorporation into poly(hydroxybutyrate) matrix in the formation of a novel nanocomposite

NASA Astrophysics Data System (ADS)

Riaz, Shahina; Raza, Zulfiqar Ali; Majeed, Muhammad Irfan; Jan, Tariq

2018-05-01

In the present study, zinc sulfide (ZnS) nanoparticles (NPs) were successfully synthesized through a modified chemical precipitation protocol and then mediated into poly(hydroxybutyrate) (PHB) matrix to get ZnS/PHB nanocomposite. Mean diameter and zeta potential of ZnS NPs, as determined using dynamic light scattering technique (DLS), were observed to be 53 nm and ‑89 mV, respectively. The structural investigations performed using x-ray diffraction (XRD) technique depicted the phase purity of ZnS NPs exhibiting cubic crystal structure. Fourier transform infrared (FTIR) spectroscopic analysis was conducted to identify the presence or absence of bonding vibrational modes on the surface of synthesized single phase ZnS NPs. The FTIR analysis confirmed the metal to sulphur bond formation by showing the characteristic band at 1123 cm‑1. The UV–vis absorption spectra of ZnS NPs confirmed the synthesis of particles in nanoscale regime showing a λ max of 302 nm. These NPs were then successfully incorporated into PHB matrix to synthesize ZnS/PHB nanocomposite. The synthesis of nanocomposite was confirmed by EDX analysis. The chemical bonding and structural properties of ZnS/PHB nanocomposite were determined by FTIR and XRD analysis, respectively. The FTIR analysis confirmed the synthesis of ZnS/PHB nanocomposite. Moreover, XRD analysis showed that structure of nanocomposite was completely controlled by ZnS NPs as pure PHB exhibited orthorhombic crystal structure while the nanocomposite demonstrated cubic crystal structure of ZnS. Thermal properties of nanocomposite were studied through thermogravimetric analysis revealing that the incorporation of ZnS NPs into PHB matrix lead to enhance heat resistance properties of PHB.

Surface Functionalization of Diamond Films by Photoreaction of Elemental Sulfur and Their Surface Properties

NASA Astrophysics Data System (ADS)

Nakamura, Takako; Ohana, Tsuguyori

2012-08-01

A useful method for direct sulfurization of diamond film surfaces by photoreaction of elemental sulfur was developed. The introduction of thiol groups onto the diamond films was confirmed by X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FT-IR), Raman spectroscopy, and scanning electron microscopy (SEM) analyses. The sulfur-modified diamond films attached to gold nanoparticles by self-assembly. The degrees of thiol group introduction and gold attachment were found to depend on photoirradiation time by monitoring by XPS. The gold-modified diamond film was observed to act as a surface-enhanced Raman scattering substrate for measurement of picric acid.

Zero-order release of aspirin, theophylline and atenolol in water from novel methylcellulose glutarate matrix tablets.

PubMed

Khairuzzaman, A; Ahmed, S U; Savva, M; Patel, N K

2006-08-02

A novel hydrocolloidal polymer, methylcellulose glutarate (MC-GA), was prepared by esterifying methylcellulose with glutaric anhydride. The formation of ester was confirmed by FTIR and NMR spectroscopy, DSC and elemental analysis. The physicochemical properties such as, rate of swelling in water, viscosity and hygroscopicity of MC-GA were determined and compared with those of methycellulose A (MC). Aspirin, theophylline and atenolol tablets were compacted on a Carver press using the wet granulation method. Each tablet contained: 200 mg active, 80 mg anhydrous lactose, 8 mg povidone, 4 mg magnesium stearate, 4 mg talc, 50mg MC or MC-GA (drug-to-polymer ratio, 4:1). Contrary to the first-order release profile of all the drugs from the MC matrix tablets, a zero-order release was obtained from the MC-GA matrix tablets in water.

Synthesis, Characterization and Biological Studies of New Linear Thermally Stable Schiff Base Polymers with Flexible Spacers.

PubMed

Qureshi, Farah; Khuhawar, Muhammad Yar; Jahangir, Taj Muhammad; Channar, Abdul Hamid

2016-01-01

Five new linear Schiff base polymers having azomethine structures, ether linkages and extended aliphatic chain lengths with flexible spacers were synthesized by polycondensation of dialdehyde (monomer) with aliphatic and aromatic diamines. The formation yields of monomer and polymers were obtained within 75-92%. The polymers with flexible spacers of n-hexane were somewhat soluble in acetone, chloroform, THF, DMF and DMSO on heating. The monomer and polymers were characterized by melting point, elemental microanalysis, FT-IR, (1)HNMR, UV-Vis spectroscopy, thermogravimetry (TG), differential thermal analysis (DTA), fluorescence emission, scanning electron microscopy (SEM) and viscosities and thermodynamic parameters measurements of their dilute solutions. The studies supported formation of the monomer and polymers and on the basis of these studies their structures have been assigned. The synthesized polymers were tested for their antibacterial and antifungal activities.

A porous Cd(II) metal-organic framework with high adsorption selectivity for CO2 over CH4

NASA Astrophysics Data System (ADS)

Zhu, Chunlan

2017-05-01

Metal-organic frameworks (MOFs) have attracted a lot of attention in recent decades. We applied a semi-rigid four-carboxylic acid linker to assemble with Cd(II) ions to generate a novel microporous Cd(II) MOF material. Single crystal X-ray diffraction study reveals the different two dimension (2D) layers can be further packed together with an AB fashion by hydrogen bonds (O4sbnd H4⋯O7 = 1.863 Å) to construct a three dimension (3D) supermolecular architecture. The resulting sample can be synthesized under solvothermal reactions successfully, which exhibits high selectivity adsorption of CO2 over CH4 at room temperature. In addition, the obtained sample was characterized by thermal gravimetric analyses (TGA), Fourier-transform infrared spectra (FT-IR), elemental analysis (CHN) and powder X-ray diffraction (PXRD).

The first report of the physicochemical structure of chitin isolated from Hermetia illucens.

PubMed

Waśko, Adam; Bulak, Piotr; Polak-Berecka, Magdalena; Nowak, Katarzyna; Polakowski, Cezary; Bieganowski, Andrzej

2016-11-01

This is the first report on the physicochemical properties of chitin obtained from larvae and imagoes of black soldier flies (Hermetia illucens). Scanning electron microscopy revealed differences in surface morphologies of the two types of chitin. The crystalline index values of chitins from adult flies and larvae were 24.9% and 35%, respectively. This is a trait that differentiates these biopolymers from chitins extracted from other sources described so far. X-ray diffraction patterns and IR spectroscopy revealed that both types of samples of chitin were in an α crystalline form. Also, the results of elemental analysis, thermal stabilities and FTIR spectroscopy of the chitins from larvae and adults of H. illucens were similar, which points to a general similarity in their physicochemical structure. Copyright © 2016 Elsevier B.V. All rights reserved.

Functional Aromatic Poly(1,3,4-Oxadiazole-Ether)s with Benzimidazole Pendants: Synthesis, Thermal and Dielectric Studies

PubMed Central

Ganesh, Shimoga D.; Pai, Vasantakumar K.; Kariduraganavar, Mahadevappa Y.; Jayanna, Madhu B.

2014-01-01

Poly(1,3,4-oxadiazole-ether) with reactive carboxylic acid pendants was synthesized from solution polymerization via nucleophilic displacement polycondensation among 2,5-bis(4-fluorophenyl)-1,3,4-oxadiazole (BFPOx) and 4,4′-bis(4-hydroxyphenyl) valeric acid (BHPA). Without altering the polymeric segments, benzimidazole modified poly(1,3,4-oxadiazole-ether)s were prepared by varying stoichiometric ratios of 1,2-phenylenediamine. The molecular structural characterization of these polymers was achieved by, FT-IR, NMR, TGA, elemental analysis, and analytical techniques. The weight-average molecular weight of virgin polymer with carboxylic acid functionality was determined by gel permeation chromatography (GPC) and was found to be 22400 (Mw/Mn = 2.07). All the synthesized polyethers were compressed into pellets and electrical contacts were established to perform dielectric properties. PMID:27437448

Synthesis, structure and solvatochromic properties of some novel 5-arylazo-6-hydroxy-4-phenyl-3-cyano-2-pyridone dyes

PubMed Central

2012-01-01

Background A series of some novel arylazo pyridone dyes was synthesized from the corresponding diazonium salt and 6-hydroxy-4-phenyl-3-cyano-2-pyridone using a classical reaction for the synthesis of the azo compounds. Results The structure of the dyes was confirmed by UV-vis, FT-IR, 1H NMR and 13C NMR spectroscopic techniques and elemental analysis. The solvatochromic behavior of the dyes was evaluated with respect to their visible absorption properties in various solvents. Conclusions The azo-hydrazone tautomeric equilibration was found to depend on the substituents as well as on the solvent. The geometry data of the investigated dyes were obtained using DFT quantum-chemical calculations. The obtained calculational results are in very good agreement with the experimental data. PMID:22824496

Synthesis and characterization of a prominent NLO active MOF of lead with 1,5-naphthalenedisulfonic acid

NASA Astrophysics Data System (ADS)

Prasad, S. Shibu; Sudarsanakumar, M. R.; Dhanya, V. S.; Suma, S.; Kurup, M. R. Prathapachandra

2018-09-01

A new metal-organic framework of lead, [Pb(1,5-nds)(H2O)3]n (1,5-nds = 1,5-naphthalenedisulfonate) having prominent nonlinear optical property has been prepared by single gel diffusion technique at ambient condition using sodium metasilicate. The second harmonic generation efficiency was analyzed using Kurtz and Perry powder method and was found to be 30 times as large as potassium dihydrogen phosphate (KDP). Single crystal X-ray diffraction studies reveal the crystal structure. The grown crystals were further characterized by elemental analysis, powder XRD study, thermogravimetry, FT-IR and UV-visible spectral studies. The Pb2S2O4 rings in the crystal structure form a 1D channel. Hydrogen bonding and π-π interactions provide additional stability to the compound. Photoluminescence studies were also carried out.

Synthesis, characterization and antibacterial activity of new sulfonyl hydrazone derivatives and their nickel(II) complexes

NASA Astrophysics Data System (ADS)

Özmen, Ümmühan Özdemir; Olgun, Gülçin

2008-08-01

Prophane sulfonic acid hydrazide (psh: CH 3CH 2CH 2SO 2NHNH 2) derivatives as salicylaldehydeprophanesulfonylhydrazone (salpsh), 5-methylsalicylaldehydeprophanesulfonylhydrazone (5-msalpsh), 2-hydroxyacetophenoneprophanesulfonylhydrazone (afpsh), 5-methyl-2-hydroxyacetophenoneprophanesulfonylhydrazone (5-mafpsh) and their Ni(II) complexes have been synthesized. The structure of these compounds has been investigated by using elemental analysis, FTIR, 1H NMR, LC/MS, UV-vis spectrophotometric method, magnetic susceptibility and conductivity measurements. The complexes were found to have general compositions [NiL2]. Square-planer structures are proposed for the Ni(II) complexes on the basis of magnetic evidence, electronic spectra and TGA data. Bacterial activities of sulfonyl hydrazone compounds were studied against gram-positive bacteria: Staphylococcus aureus, Bacillus subtilis, Bacillus magaterium and gram-negative bacteria: Salmonella enteritidis, Escherichia coli by using minimum inhibitory concentrations (MICs) method.

Ferrocene-functionalized graphene electrode for biosensing applications.

PubMed

Rabti, Amal; Mayorga-Martinez, Carmen C; Baptista-Pires, Luis; Raouafi, Noureddine; Merkoçi, Arben

2016-07-05

A novel ferrocene-functionalized reduced graphene oxide (rGO)-based electrode is proposed. It was fabricated by the drop casting of ferrocene-functionalized graphene onto polyester substrate as the working electrode integrated within screen-printed reference and counter electrodes. The ferrocene-functionalized rGO has been fully characterized using FTIR, XPS, contact angle measurements, SEM and TEM microscopy, and cyclic voltammetry. The XPS and EDX analysis showed the presence of Fe element related to the introduced ferrocene groups, which is confirmed by a clear CV signal at ca. 0.25 V vs. Ag/AgCl (0.1 KCl). Mediated redox catalysis of H2O2 and bio-functionalization with glucose oxidase for glucose detection were achieved by the bioelectrode providing a proof for potential biosensing applications. Copyright © 2016 Elsevier B.V. All rights reserved.

Microwave Assisted Synthesis, Physicochemical, Photophysical, Single Crystal X-ray and DFT Studies of Novel Push-Pull Chromophores.

PubMed

Khan, Salman A; Asiri, Abdullah M; Basisi, Hadi Mussa; Arshad, Muhammad Nadeem; Sharma, Kamlesh

2015-11-01

Two push-pull chromophores were synthesized by knoevenagel condensation under microwave irradiation. The structure of synthesized chromophores were established by spectroscopic (FT-IR, (1)H NMR, (13)C NMR, EI-MS) and elemental analysis. Structure of the chromophores was further conformed by X-ray crystallographic. UV-Vis and fluorescence spectroscopy measurements provided that chromophores were good absorbent and fluorescent properties. Fluorescence polarity studies demonstrated that chromophores were sensitive to the polarity of the microenvironment provided by different solvents. Physicochemical parameters, including singlet absorption, extinction coefficient, stokes shift, oscillator strength, dipole moment and flurescence quantum yield were investigated in order to explore the analytical potential of the synthesized chromophores. In addition, the total energy, frontier molecular orbitals, hardness, electron affinity, ionization energy, electrostatic potential map were also studied computationally by using density functional theoretical method.

Preparation, spectroscopic characterization and antimicrobial activities of mixed metal (Sb and Bi) bridged derivatives with mixed sulfur donor ligands

NASA Astrophysics Data System (ADS)

Joshi, Sapana; Chauhan, H. P. S.; Carpenter, Nitin

2017-01-01

This article explores the syntheses of six mixed metal derivatives of antimony(III) and bismuth(III) by the reaction of ethane-1,2-dithiol and metal bis derivatives of dithiocarbamates and/or dithiophosphates ligands in 1:1:1 M stoichiometry. These derivatives have been characterized by physicochemical [elemental analysis (C, H, N, S, Sb and Bi), molecular weight and melting point determinations], spectral [UV-Visible, FTIR, NMR (1H, 13C and 31P)], powder X-ray diffraction studies. These derivatives have nano-ranged crystallite size (8.18-18.04 nm) with monoclinic crystal system. All the synthesized derivatives have two metal centers (Sb and Bi) which elevate the zone of inhibition against four bacterial and two fungal species as compared to single metal species (metal precursors) as well as standard drugs.

Fast discrimination of traditional Chinese medicine according to geographical origins with FTIR spectroscopy and advanced pattern recognition techniques

NASA Astrophysics Data System (ADS)

Li, Ning; Wang, Yan; Xu, Kexin

2006-08-01

Combined with Fourier transform infrared (FTIR) spectroscopy and three kinds of pattern recognition techniques, 53 traditional Chinese medicine danshen samples were rapidly discriminated according to geographical origins. The results showed that it was feasible to discriminate using FTIR spectroscopy ascertained by principal component analysis (PCA). An effective model was built by employing the Soft Independent Modeling of Class Analogy (SIMCA) and PCA, and 82% of the samples were discriminated correctly. Through use of the artificial neural network (ANN)-based back propagation (BP) network, the origins of danshen were completely classified.

Analysis and optimization of process parameters for production of polyhydroxyalkanoates along with wastewater treatment by Serratia sp. ISTVKR1.

PubMed

Gupta, Asmita; Kumar, Madan; Thakur, Indu Shekhar

2017-10-01

A previously reported biodegrading bacterial strain Serratia sp. ISTVKR1 was studied for polyhydroxyalkanoate (PHA) production along with wastewater contaminant removal. Nile red fluorescence, GC-MS, FT-IR, NMR and TEM confirmed the accumulation of homopolymer poly-3-hydroxyvalerate (PHV) within the bacterial cells. Analysis of culture after 72h of bacterial treatment showed maximum COD removal (8.4-fold), non-detection of organic contaminants such as 1H-Cyclopropa [a] naphthalene (R.T.=10.12) using GC-MS and increased proportion of elements like Cr, Mn, Fe, Ni, Cu, Cd and Pb in the bacterial cell pellets by SEM-EDX analysis. Optimization of process parameters for enhanced PHA production along with wastewater treatment done using Response Surface Methodology (RSM) showed 5% and 0.74% increase in the PHA production (0.3368±0.13gL -1 ) and % COD reduction (88.93±2.41) of wastewater, respectively. The study, thus established the production of PHA along with wastewater contaminant removal by Serratia sp. ISTVKR1. Copyright © 2017 Elsevier Ltd. All rights reserved.

Synthesis, characterization, and thermal analysis of a new energetic salt based on 1'-hydroxy-1H,1'H-5,5'-bitetrazol-1-olate

NASA Astrophysics Data System (ADS)

Niu, Chunhuan; Jin, Bo; Shang, Yu; Liu, Qiangqiang; Peng, Rufang

2018-04-01

4-Amino-1,2,4-triazolium 1'-hydroxy-1H,1'H-5,5'-bitetrazol-1-olate (ATHBTO) was synthesized by reacting 4-amino-1,2,4-triazole (AT) and 1H,1‧H-5,5‧-bistetrazole-1,1‧-diolate dihydrate (H2BTO.2H2O). Its crystal structure was characterized through single-crystal X-ray diffraction. Meanwhile, FTIR, 1H NMR, 13C NMR, and elemental analysis were also introduced to analyze its composition. The thermal stability was investigated by differential scanning calorimetry, thermogravimetric analysis, and thermogravimetric tandem infrared spectrum. Results indicated that ATHBTO exhibited excellent resistance to thermal decompositions reaching 511.4 K and had a 64.6% mass loss between 475.7 and 552.3 K. The kinetics parameters were calculated by Kissinger's method and Ozawa-Doyle's method. Moreover, according to the Kamlet-Jacobs formula, the calculated detonation velocity and detonation pressure of ATHBTO attained 8218 m/s and 28.69 GPa, respectively.

FT-IR and C-13 NMR analysis of soil humic fractions from a long term cropping systems study

USDA-ARS?s Scientific Manuscript database

Increased knowledge of humic fractions is important due to its involvement in many soil ecosystem processes. Soil humic acid (HA) and fulvic acid (FA) from a nine-year agroecosystem study with different tillage, cropping system, and N source treatments were characterized using FT-IR andsolid-state ...

Sol-gel synthesis and characterizations of crystalline NaGd(WO4)2 powder for anisotropic transparent ceramic laser application

NASA Astrophysics Data System (ADS)

Durairajan, A.; Thangaraju, D.; Balaji, D.; Moorthy Babu, S.

2013-02-01

NaGd(WO4)2 powders were synthesized at different pH (3.5, 4.5, 5.5, 6.5 and 7.5) values by conventional Pechini method. Sodium and gadolinium nitrate salts and ammonium paratungstate are used as starting precursors. Metal cations were chelated by citric acid and individual citrates were bound together with ethylene glycol. Synthesized gel was analyzed using differential thermal analysis (DTA), thermo gravimetric (TG) and FT-IR spectroscopy to understand the degradation of gel and formation of metal citrates. Calcined powders (250, 600, 700 and 800 °C) were characterized by powder XRD, FT-IR, Raman and FE-SEM analysis. The temperature dependent phase formation was examined by powder XRD. The morphological changes at different pH derived powders were observed with FE-SEM micrographs. Stepwise organic liberation with respect to temperature and presence of carbon content in the pre-fired powder were analyzed using FT-IR analysis. Raman spectrum reveals disordered tungstate vibrations in the NGW matrix.

Enhancing forensic science with spectroscopic imaging

NASA Astrophysics Data System (ADS)

Ricci, Camilla; Kazarian, Sergei G.

2006-09-01

This presentation outlines the research we are developing in the area of Fourier Transform Infrared (FTIR) spectroscopic imaging with the focus on materials of forensic interest. FTIR spectroscopic imaging has recently emerged as a powerful tool for characterisation of heterogeneous materials. FTIR imaging relies on the ability of the military-developed infrared array detector to simultaneously measure spectra from thousands of different locations in a sample. Recently developed application of FTIR imaging using an ATR (Attenuated Total Reflection) mode has demonstrated the ability of this method to achieve spatial resolution beyond the diffraction limit of infrared light in air. Chemical visualisation with enhanced spatial resolution in micro-ATR mode broadens the range of materials studied with FTIR imaging with applications to pharmaceutical formulations or biological samples. Macro-ATR imaging has also been developed for chemical imaging analysis of large surface area samples and was applied to analyse the surface of human skin (e.g. finger), counterfeit tablets, textile materials (clothing), etc. This approach demonstrated the ability of this imaging method to detect trace materials attached to the surface of the skin. This may also prove as a valuable tool in detection of traces of explosives left or trapped on the surfaces of different materials. This FTIR imaging method is substantially superior to many of the other imaging methods due to inherent chemical specificity of infrared spectroscopy and fast acquisition times of this technique. Our preliminary data demonstrated that this methodology will provide the means to non-destructive detection method that could relate evidence to its source. This will be important in a wider crime prevention programme. In summary, intrinsic chemical specificity and enhanced visualising capability of FTIR spectroscopic imaging open a window of opportunities for counter-terrorism and crime-fighting, with applications ranging from analysis of trace evidence (e.g. in soil), tablets, drugs, fibres, tape explosives, biological samples to detection of gunshot residues and imaging of fingerprints.

Spectroscopic (FTIR, FT-Raman), molecular electrostatic potential, NBO and HOMO-LUMO analysis of P-bromobenzene sulfonyl chloride based on DFT calculations

NASA Astrophysics Data System (ADS)

Jeyavijayan, S.

2015-02-01

The FTIR and FT-Raman spectra of P-bromobenzene sulfonyl chloride (P-BBSC) have been recorded in the regions 4000-400 cm-1 and 3500-50 cm-1, respectively. Utilizing the observed FTIR and FT-Raman data, a complete vibrational assignment and analysis of the fundamental modes of the compound were carried out. The optimum molecular geometry, harmonic vibrational frequencies, infrared intensities and Raman scattering activities, were calculated by density functional theory (DFT/B3LYP) method. A good agreement between experimental and calculated normal modes of vibrations has been observed. A detailed interpretation of the infrared and Raman spectra of P-BBSC is also reported based on total energy distribution (TED). Stability of the molecule arising from hyperconjugative interactions, charge delocalization have been analyzed using natural bond orbital (NBO) analysis. The MEP map shows the negative potential sites are on oxygen atoms as well as the positive potential sites are around the hydrogen atoms. The UV-vis spectral analysis of P-BBSC has also been done which confirms the charge transfer of the molecule.

Hydrogen concentration analysis in clinopyroxene using proton-proton scattering analysis

NASA Astrophysics Data System (ADS)

Weis, Franz A.; Ros, Linus; Reichart, Patrick; Skogby, Henrik; Kristiansson, Per; Dollinger, Günther

2018-02-01

Traditional methods to measure water in nominally anhydrous minerals (NAMs) are, for example, Fourier transformed infrared (FTIR) spectroscopy or secondary ion mass spectrometry (SIMS). Both well-established methods provide a low detection limit as well as high spatial resolution yet may require elaborate sample orientation or destructive sample preparation. Here we analyze the water content in erupted volcanic clinopyroxene phenocrysts by proton-proton scattering and reproduce water contents measured by FTIR spectroscopy. We show that this technique provides significant advantages over other methods as it can provide a three-dimensional distribution of hydrogen within a crystal, making the identification of potential inclusions possible as well as elimination of surface contamination. The sample analysis is also independent of crystal structure and orientation and independent of matrix effects other than sample density. The results are used to validate the accuracy of wavenumber-dependent vs. mineral-specific molar absorption coefficients in FTIR spectroscopy. In addition, we present a new method for the sample preparation of very thin crystals suitable for proton-proton scattering analysis using relatively low accelerator potentials.

Melamine detection in infant formula powder using near- and mid-infrared spectroscopy.

PubMed

Mauer, Lisa J; Chernyshova, Alona A; Hiatt, Ashley; Deering, Amanda; Davis, Reeta

2009-05-27

Near- and mid-infrared spectroscopy methods (NIR, FTIR-ATR, FTIR-DRIFT) were evaluated for the detection and quantification of melamine in infant formula powder. Partial least-squares (PLS) models were established for correlating spectral data to melamine concentration: R(2) > 0.99, RMSECV ≤ 0.9, and RPD ≥ 12. Factorization analysis of spectra was able to differentiate unadulterated infant formula powder from samples containing 1 ppm melamine with no misclassifications, a confidence level of 99.99%, and selectivity > 2. These nondestructive methods require little or no sample preparation. The NIR method has an assay time of 1 min, and a 2 min total time to detection. The FTIR methods require up to 5 min for melamine detection. Therefore, NIR and FTIR methods enable rapid detection of 1 ppm melamine in infant formula powder.

Spectroscopic and Chemometric Analysis of Binary and Ternary Edible Oil Mixtures: Qualitative and Quantitative Study.

PubMed

Jović, Ozren; Smolić, Tomislav; Primožič, Ines; Hrenar, Tomica

2016-04-19

The aim of this study was to investigate the feasibility of FTIR-ATR spectroscopy coupled with the multivariate numerical methodology for qualitative and quantitative analysis of binary and ternary edible oil mixtures. Four pure oils (extra virgin olive oil, high oleic sunflower oil, rapeseed oil, and sunflower oil), as well as their 54 binary and 108 ternary mixtures, were analyzed using FTIR-ATR spectroscopy in combination with principal component and discriminant analysis, partial least-squares, and principal component regression. It was found that the composition of all 166 samples can be excellently represented using only the first three principal components describing 98.29% of total variance in the selected spectral range (3035-2989, 1170-1140, 1120-1100, 1093-1047, and 930-890 cm(-1)). Factor scores in 3D space spanned by these three principal components form a tetrahedral-like arrangement: pure oils being at the vertices, binary mixtures at the edges, and ternary mixtures on the faces of a tetrahedron. To confirm the validity of results, we applied several cross-validation methods. Quantitative analysis was performed by minimization of root-mean-square error of cross-validation values regarding the spectral range, derivative order, and choice of method (partial least-squares or principal component regression), which resulted in excellent predictions for test sets (R(2) > 0.99 in all cases). Additionally, experimentally more demanding gas chromatography analysis of fatty acid content was carried out for all specimens, confirming the results obtained by FTIR-ATR coupled with principal component analysis. However, FTIR-ATR provided a considerably better model for prediction of mixture composition than gas chromatography, especially for high oleic sunflower oil.

Assessing the shock state of the lunar highlands: Implications for the petrogenesis and chronology of crustal anorthosites.

PubMed

Pernet-Fisher, J F; Joy, K H; Martin, D J P; Donaldson Hanna, K L

2017-07-19

Our understanding of the formation and evolution of the primary lunar crust is based on geochemical systematics from the lunar ferroan anorthosite (FAN) suite. Recently, much effort has been made to understand this suite's petrologic history to constrain the timing of crystallisation and to interpret FAN chemical diversity. We investigate the shock histories of lunar anorthosites by combining Optical Microscope (OM) 'cold' cathodoluminescence (CL)-imaging and Fourier Transform Infrared (FTIR) spectroscopy analyses. In the first combined study of its kind, this study demonstrates that over ~4.5 Ga of impact processing, plagioclase is on average weakly shocked (<15 GPa) and examples of high shock states (>30 GPa; maskelynite) are uncommon. To investigate how plagioclase trace-element systematics are affected by moderate to weak shock (~5 to 30 GPa) we couple REE+Y abundances with FTIR analyses for FAN clasts from lunar meteorite Northwest Africa (NWA) 2995. We observe weak correlations between plagioclase shock state and some REE+Y systematics (e.g., La/Y and Sm/Nd ratios). This observation could prove significant to our understanding of how crystallisation ages are evaluated (e.g., plagioclase-whole rock Sm-Nd isochrons) and for what trace-elements can be used to differentiate between lunar lithologies and assess magma source compositional differences.

Development of an automated method for determining oil in water by direct aqueous supercritical fluid extraction coupled on-line with infrared spectroscopy.

PubMed

Minty, B; Ramsey, E D; Davies, I

2000-12-01

A direct aqueous supercritical fluid extraction (SFE) system was developed which can be directly interfaced to an infrared spectrometer for the determination of oil in water. The technique is designed to provide an environmentally clean, automated alternative to established IR methods for oil in water analysis which require the use of restricted organic solvents. The SFE-FTIR method involves minimum sample handling stages, with on-line analysis of a 500 ml water sample being complete within 15 min. Method accuracy for determining water samples spiked with gasoline, white spirit, kerosene, diesel or engine oil was 81-100% with precision (RSD) ranging from 3 to 17%. An independent evaluation determined a 2 ppm limit of quantification for diesel in industrial effluents. The results of a comparative study involving an established IR method and the SFE-FTIR method indicate that oil levels calculated using an accepted equation which includes coefficients derived from reference hydrocarbon standards may result in significant errors. A new approach permitted the derivation of quantification coefficients for the SFE-FTIR analyses which provided improved results. In situations where the identity of the oil to be analysed is known, a rapid off-line SFE-FTIR system calibration procedure was developed and successfully applied to various oils. An optional in-line silica gel clean-up procedure incorporated within the SFE-FTIR system enables the same water sample to be analysed for total oil content including vegetable oils and selectively for petroleum oil content within a total of 20 min. At the end of an analysis the SFE system is cleaned using an in situ 3 min clean cycle.

[Establishment of the Mathematical Model for PMI Estimation Using FTIR Spectroscopy and Data Mining Method].

PubMed

Wang, L; Qin, X C; Lin, H C; Deng, K F; Luo, Y W; Sun, Q R; Du, Q X; Wang, Z Y; Tuo, Y; Sun, J H

2018-02-01

To analyse the relationship between Fourier transform infrared （FTIR） spectrum of rat's spleen tissue and postmortem interval （PMI） for PMI estimation using FTIR spectroscopy combined with data mining method. Rats were sacrificed by cervical dislocation, and the cadavers were placed at 20 ℃. The FTIR spectrum data of rats' spleen tissues were taken and measured at different time points. After pretreatment, the data was analysed by data mining method. The absorption peak intensity of rat's spleen tissue spectrum changed with the PMI, while the absorption peak position was unchanged. The results of principal component analysis （PCA） showed that the cumulative contribution rate of the first three principal components was 96%. There was an obvious clustering tendency for the spectrum sample at each time point. The methods of partial least squares discriminant analysis （PLS-DA） and support vector machine classification （SVMC） effectively divided the spectrum samples with different PMI into four categories （0-24 h, 48-72 h, 96-120 h and 144-168 h）. The determination coefficient （ R ²） of the PMI estimation model established by PLS regression analysis was 0.96, and the root mean square error of calibration （RMSEC） and root mean square error of cross validation （RMSECV） were 9.90 h and 11.39 h respectively. In prediction set, the R ² was 0.97, and the root mean square error of prediction （RMSEP） was 10.49 h. The FTIR spectrum of the rat's spleen tissue can be effectively analyzed qualitatively and quantitatively by the combination of FTIR spectroscopy and data mining method, and the classification and PLS regression models can be established for PMI estimation. Copyright© by the Editorial Department of Journal of Forensic Medicine.

Application of FTIR-ATR spectroscopy coupled with multivariate analysis for rapid estimation of butter adulteration.

PubMed

Fadzlillah, Nurrulhidayah Ahmad; Rohman, Abdul; Ismail, Amin; Mustafa, Shuhaimi; Khatib, Alfi

2013-01-01

In dairy product sector, butter is one of the potential sources of fat soluble vitamins, namely vitamin A, D, E, K; consequently, butter is taken into account as high valuable price from other dairy products. This fact has attracted unscrupulous market players to blind butter with other animal fats to gain economic profit. Animal fats like mutton fat (MF) are potential to be mixed with butter due to the similarity in terms of fatty acid composition. This study focused on the application of FTIR-ATR spectroscopy in conjunction with chemometrics for classification and quantification of MF as adulterant in butter. The FTIR spectral region of 3910-710 cm⁻¹ was used for classification between butter and butter blended with MF at various concentrations with the aid of discriminant analysis (DA). DA is able to classify butter and adulterated butter without any mistakenly grouped. For quantitative analysis, partial least square (PLS) regression was used to develop a calibration model at the frequency regions of 3910-710 cm⁻¹. The equation obtained for the relationship between actual value of MF and FTIR predicted values of MF in PLS calibration model was y = 0.998x + 1.033, with the values of coefficient of determination (R²) and root mean square error of calibration are 0.998 and 0.046% (v/v), respectively. The PLS calibration model was subsequently used for the prediction of independent samples containing butter in the binary mixtures with MF. Using 9 principal components, root mean square error of prediction (RMSEP) is 1.68% (v/v). The results showed that FTIR spectroscopy can be used for the classification and quantification of MF in butter formulation for verification purposes.

Evaluation of Fourier transform infrared (FT-IR) spectroscopy and chemometrics as a rapid approach for sub-typing Escherichia coli O157:H7 isolates.

PubMed

Davis, R; Paoli, G; Mauer, L J

2012-09-01

The importance of tracking outbreaks of foodborne illness and the emergence of new virulent subtypes of foodborne pathogens have created the need for rapid and reliable sub-typing methods for Escherichia coli O157:H7. Fourier transform infrared (FT-IR) spectroscopy coupled with multivariate statistical analyses was used for sub-typing 30 strains of E. coli O157:H7 that had previously been typed by multilocus variable number tandem repeat analysis (MLVA) and pulsed field gel electrophoresis (PFGE). Hierarchical cluster analysis (HCA) and canonical variate analysis (CVA) of the FT-IR spectra resulted in the clustering of the same or similar MLVA types and separation of different MLVA types of E. coli O157:H7. The developed FT-IR method showed better discriminatory power than PFGE in sub-typing E. coli O157:H7. Results also indicated the spectral relatedness between different outbreak strains. However, the grouping of some strains was not in complete agreement with the clustering based on PFGE and MLVA. Additionally, HCA of the spectra differentiated the strains into 30 sub-clusters, indicating the high specificity and suitability of the method for strain level identification. Strains were also classified (97% correct) based on the type of Shiga toxin present using CVA of the spectra. This study demonstrated that FT-IR spectroscopy is suitable for rapid (≤16 h) and economical sub-typing of E. coli O157:H7 with comparable accuracy to MLVA typing. This is the first report of using an FT-IR-based method for sub-typing E. coli O157:H7. Copyright © 2012 Elsevier Ltd. All rights reserved.

Assessing dysplasia of a bronchial biopsy with FTIR spectroscopic imaging

NASA Astrophysics Data System (ADS)

Foreman, Liberty; Kimber, James A.; Oliver, Katherine V.; Brown, James M.; Janes, Samuel M.; Fearn, Tom; Kazarian, Sergei G.; Rich, Peter

2015-03-01

An FTIR image of an 8 µm section of de-paraffinised bronchial biopsy that shows a histological transition from normal to severe dysplasia/squamous cell carcinoma (SCC) in situ was obtained in transmission by stitching together images of 256 x 256 µm recorded using a 96 x 96 element FPA detector. Each pixel spectrum was calculated from 128 co-added interferograms at 4 cm-1 resolution. In order to improve the signal to noise ratio, blocks of 4x4 adjacent pixels were subsequently averaged. Analyses of this spectral image, after conversion of the spectra to their second derivatives, show that the epithelium and the lamina propria tissue types can be distinguished using the area of troughs at either 1591, 1334, 1275 or 1215 cm-1 or, more effectively, by separation into two groups by hierarchical clustering (HCA) of the 1614-1465 region. Due to an insufficient signal to noise ratio, disease stages within the image could not be distinguished with this extent of pixel averaging. However, after separation of the cell types, disease stages within either the epithelium or the lamina propria could be distinguished if spectra were averaged from larger, manually selected areas of the tissue. Both cell types reveal spectral differences that follow a transition from normal to cancerous histology. For example, spectral changes that occurred in the epithelium over the transition from normal to carcinoma in situ could be seen in the 1200-1000 cm-1 region, particularly as a decrease in the second derivative troughs at 1074 and 1036 cm-1 , consistent with changes in some form of carbohydrate. Spectral differences that indicate a disease transition from normal to carcinoma in the lamina propria could be seen in the 1350-1175 cm-1 and 1125-1030 cm-1 regions. Thus demonstrating that a progression from healthy to severe dysplasia/squamous cell carcinoma (SCC) in situ can be seen using FTIR spectroscopic imaging and multivariate analysis.

Compositional and surface characterization of HULIS by UV-Vis, FTIR, NMR and XPS: Wintertime study in Northern India

NASA Astrophysics Data System (ADS)

Kumar, Varun; Goel, Anubha; Rajput, Prashant

2017-09-01

This study (first attempt) characterizes HULIS (Humic Like Substances) in wintertime aerosols (n = 12 during day and nighttime each) from Indo-Gangetic Plain (IGP, at Kanpur) by using various state-of-the art techniques such as UV-VIS, FTIR, 1H NMR and XPS. Based on UV-Vis analysis the absorption coefficient at 365 nm (babs-365) of HULIS was found to average at 13.6 and 28.8 Mm-1 during day and nighttime, respectively. Relatively high babs-365 of HULIS during the nighttime is attributed to influence of fog-processing. However, the power fit of UV-Vis spectrum provided near similar AAE (absorption Angstrom exponent) value of HULIS centering at 4.9 ± 1.4 and 5.1 ± 1.3 during daytime and nighttime, respectively. FTIR spectra and its double derivative revealed the presence of various functional groups viz. alcohols, ketones aldehydes, carboxylic acids as well as unsaturated and saturated carbon bonds. 1H NMR spectroscopy was applied to quantify relative percentage of various types of hydrogen atoms contained in HULIS, whereas XPS technique provided information on surface composition and oxidation states of various elements present. A significantly high abundance of H‒C‒O group has been observed in HULIS (based on 1H NMR); 41.4± 2.7% and 30.9± 2.4% in day and nighttime, respectively. However, aromatic protons (Ar-H) were higher in nighttime samples (19.3± 1.8%) as compared to that in daytime samples (7.5 ± 1.9). XPS studies revealed presence of various species on the surface of HULIS samples. Carbon existed in 7 different chemical states while total nitrogen and sulfur exhibited 3 and 2 different oxidation states (respectively) on the surface of HULIS. This study reports structural information and absorption properties of HULIS which has implications to their role as cloud condensation nuclei and atmospheric direct radiative forcing.

Attenuated Total Reflection Fourier Transform Infrared (ATR FT-IR) Spectroscopy as an Analytical Method to Investigate the Secondary Structure of a Model Protein Embedded in Solid Lipid Matrices.

PubMed

Zeeshan, Farrukh; Tabbassum, Misbah; Jorgensen, Lene; Medlicott, Natalie J

2018-02-01

Protein drugs may encounter conformational perturbations during the formulation processing of lipid-based solid dosage forms. In aqueous protein solutions, attenuated total reflection Fourier transform infrared (ATR FT-IR) spectroscopy can investigate these conformational changes following the subtraction of spectral interference of solvent with protein amide I bands. However, in solid dosage forms, the possible spectral contribution of lipid carriers to protein amide I band may be an obstacle to determine conformational alterations. The objective of this study was to develop an ATR FT-IR spectroscopic method for the analysis of protein secondary structure embedded in solid lipid matrices. Bovine serum albumin (BSA) was chosen as a model protein, while Precirol AT05 (glycerol palmitostearate, melting point 58 ℃) was employed as the model lipid matrix. Bovine serum albumin was incorporated into lipid using physical mixing, melting and mixing, or wet granulation mixing methods. Attenuated total reflection FT-IR spectroscopy and size exclusion chromatography (SEC) were performed for the analysis of BSA secondary structure and its dissolution in aqueous media, respectively. The results showed significant interference of Precirol ATO5 with BSA amide I band which was subtracted up to 90% w/w lipid content to analyze BSA secondary structure. In addition, ATR FT-IR spectroscopy also detected thermally denatured BSA solid alone and in the presence of lipid matrix indicating its suitability for the detection of denatured protein solids in lipid matrices. Despite being in the solid state, conformational changes occurred to BSA upon incorporation into solid lipid matrices. However, the extent of these conformational alterations was found to be dependent on the mixing method employed as indicated by area overlap calculations. For instance, the melting and mixing method imparted negligible effect on BSA secondary structure, whereas the wet granulation mixing method promoted more changes. Size exclusion chromatography analysis depicted the complete dissolution of BSA in the aqueous media employed in the wet granulation method. In conclusion, an ATR FT-IR spectroscopic method was successfully developed to investigate BSA secondary structure in solid lipid matrices following the subtraction of lipid spectral interference. The ATR FT-IR spectroscopy could further be applied to investigate the secondary structure perturbations of therapeutic proteins during their formulation development.

Water clustering in glassy polymers.

PubMed

Davis, Eric M; Elabd, Yossef A

2013-09-12

In this study, water solubility and water clustering in several glassy polymers, including poly(methyl methacrylate) (PMMA), poly(styrene) (PS), and poly(vinylpyrrolidone) (PVP), were measured using both quartz spring microbalance (QSM) and Fourier transform infrared-attenuated total reflectance (FTIR-ATR) spectroscopy. Specifically, QSM was used to determine water solubility, while FTIR-ATR spectroscopy provided a direct, molecular-level measurement of water clustering. The Flory-Huggins theory was employed to obtain a measure of water-polymer interaction and water solubility, through both prediction and regression, where the theory failed to predict water solubility in both PMMA and PVP. Furthermore, a comparison of water clustering between direct FTIR-ATR spectroscopy measurements and predictions from the Zimm-Lundberg clustering analysis produced contradictory results. The failure of the Flory-Huggins theory and Zimm-Lundberg clustering analysis to describe water solubility and water clustering, respectively, in these glassy polymers is in part due to the equilibrium constraints under which these models are derived in contrast to the nonequilibrium state of glassy polymers. Additionally, FTIR-ATR spectroscopy results were compared to temperature-dependent diffusivity data, where a correlation between the activation energy for diffusion and the measured water clustering was observed.

Phase transition analysis of V-shaped liquid crystal: Combined temperature-dependent FTIR and density functional theory approach

NASA Astrophysics Data System (ADS)

Singh, Swapnil; Singh, Harshita; Karthick, T.; Tandon, Poonam; Prasad, Veena

2018-01-01

Temperature-dependent Fourier transform infrared spectroscopy (FTIR) combined with density functional theory (DFT) is employed to study the mechanism of phase transitions of V-shaped bent-core liquid crystal. Since it has a large number of flexible bonds, one-dimensional potential energy scan (PES) was performed on the flexible bonds and predicted the most stable conformer I. A detailed analysis of vibrational normal modes of conformer I have been done on the basis of potential energy distribution. The good agreement between the calculated spectrum of conformer I and observed FTIR spectrum at room temperature validates our theoretical structure model. Furthermore, the prominent changes observed in the stretching vibrational bands of CH3/CH2, Cdbnd O, ring CC, ring CO, ring CH in-plane bending, and ring CH out-of-plane bending at Iso → nematic phase transition (at 155 °C) have been illustrated. However, the minor changes in the spectral features observed for the other phase transitions might be due to the shape or bulkiness of molecules. Combined FTIR and PES study beautifully explained the dynamics of the molecules, molecular realignment, H-bonding, and conformational changes at the phase transitions.

Differentiation in MALDI-TOF MS and FTIR spectra between two pathovars of Xanthomonas oryzae

NASA Astrophysics Data System (ADS)

Ge, Mengyu; Li, Bin; Wang, Li; Tao, Zhongyun; Mao, Shengfeng; Wang, Yangli; Xie, Guanlin; Sun, Guochang

2014-12-01

Xanthomonas oryzae pv. oryzae (Xoo) and Xanthomonas oryzae pv. oryzicola (Xoc) strains are closely related phenotypically and genetically, which make it difficult to differentiate between the two pathovars based on phenotypic and DNA-based methods. In this study, a fast and accurate method was developed based on the differences in MALDI-TOF MS and FTIR spectra between the two pathovars. MALDI-TOF MS analysis revealed that 9 and 10 peaks are specific to Xoo and Xoc, respectively, which can be used as biomarkers to identify and differentiate the two closely related pathovars. Furthermore, FTIR analysis showed that there is a significant difference in both the band frequencies and absorption intensity of various functional groups between the two pathovars. In particular, the 6 peaks at 3433, 2867, 1273, 1065, 983 and 951 cm-1 were specific to the Xoo strains, while one peak at 1572 cm-1 was specific to the Xoc strains. Overall, this study gives the first attempt to identify and differentiate the two pathovars of X. oryzae based on mass and FTIR spectra, which will be helpful for the early detection and prevention of the two rice diseases caused by both X. oryzae pathovars.

Fourier Transform Infrared Spectroscopy of CF4 on the GEC Reference Cell

NASA Technical Reports Server (NTRS)

Rao, M. V. V. S.; Sharma, S. P.; Meyyappan, M.; Cruden, Brett A.; Arnold, Jim (Technical Monitor)

2001-01-01

Fourier Transform Infrared Spectroscopy (FTIR) has been used to characterize inductively coupled CF4 plasmas in a GEC Reference Cell in-situ In examining these FTIR spectra, several assumptions and approximations of FTIR analysis are addressed. This includes the density dependence of cross-sections, non-linear effects in the addition of overlapping bands and the effect of spatial variations in density and temperature, This analysis demonstrates that temperatures extracted from MR spectra may provide a poor estimate of the true neutral plasma temperature. The FTIR spectra are dominated by unreacted CF, accounting for 40-60% of the gas products. The amount of CF4 consumption is found to have a marked dependence on power, and is nearly independent of pressure in the range of 10-50 mtorr. Small amounts of C2F6 are observed at low power. Also observed are etching products from the quartz window SiF4 COF2 and CO which occur in approximately equal ratios and together account for less than 10% of the gas. The concentrations of these species are nearly independent of pressure. CFx radicals are below the detection limit of this apparatus (approx. 1012/cc).

Propellant's differentiation using FTIR-photoacoustic detection for forensic studies of improvised explosive devices.

PubMed

Álvarez, Ángela; Yáñez, Jorge; Contreras, David; Saavedra, Renato; Sáez, Pedro; Amarasiriwardena, Dulasiri

2017-11-01

The use of propellant for making improvised explosive devices (IED) is an incipient criminal practice. Propellant can be used as initiator in explosive mixtures along with other components such as coal, ammonium nitrate, sulfur, etc. The identification of the propellant's brand used in homemade explosives can provide additional forensic information of this evidence. In this work, four of the most common propellant brands were characterized by Fourier-transform infrared photoacoustic spectroscopy (FTIR-PAS) which is a non-destructive micro-analytical technique. Spectra shows characteristic signals of typical compounds in the propellants, such as nitrocellulose, nitroglycerin, guanidine, diphenylamine, etc. The differentiation of propellant components was achieved by using FTIR-PAS combined with chemometric methods of classification. Principal component analysis (PCA) and soft independent modelling of class analogy (SIMCA) were used to achieve an effective differentiation and classification (100%) of propellant brands. Furthermore, propellant brand differentiation was also assessed using partial least squares discriminant analyses (PLS-DA) by leave one out cross (∼97%) and external (∼100%) validation method. Our results show the ability of FTIR-PAS combined with chemometric analysis to identify and differentiate propellant brands in different explosive formulations of IED. Copyright © 2017 Elsevier B.V. All rights reserved.

A hybrid sensing approach for pure and adulterated honey classification.

PubMed

Subari, Norazian; Mohamad Saleh, Junita; Md Shakaff, Ali Yeon; Zakaria, Ammar

2012-10-17

This paper presents a comparison between data from single modality and fusion methods to classify Tualang honey as pure or adulterated using Linear Discriminant Analysis (LDA) and Principal Component Analysis (PCA) statistical classification approaches. Ten different brands of certified pure Tualang honey were obtained throughout peninsular Malaysia and Sumatera, Indonesia. Various concentrations of two types of sugar solution (beet and cane sugar) were used in this investigation to create honey samples of 20%, 40%, 60% and 80% adulteration concentrations. Honey data extracted from an electronic nose (e-nose) and Fourier Transform Infrared Spectroscopy (FTIR) were gathered, analyzed and compared based on fusion methods. Visual observation of classification plots revealed that the PCA approach able to distinct pure and adulterated honey samples better than the LDA technique. Overall, the validated classification results based on FTIR data (88.0%) gave higher classification accuracy than e-nose data (76.5%) using the LDA technique. Honey classification based on normalized low-level and intermediate-level FTIR and e-nose fusion data scored classification accuracies of 92.2% and 88.7%, respectively using the Stepwise LDA method. The results suggested that pure and adulterated honey samples were better classified using FTIR and e-nose fusion data than single modality data.

Aggregation factor analysis for protein formulation by a systematic approach using FTIR, SEC and design of experiments techniques.

PubMed

Feng, Yan Wen; Ooishi, Ayako; Honda, Shinya

2012-01-05

A simple systematic approach using Fourier transform infrared (FTIR) spectroscopy, size exclusion chromatography (SEC) and design of experiments (DOE) techniques was applied to the analysis of aggregation factors for protein formulations in stress and accelerated testings. FTIR and SEC were used to evaluate protein conformational and storage stabilities, respectively. DOE was used to determine the suitable formulation and to analyze both the main effect of single factors and the interaction effect of combined factors on aggregation. Our results indicated that (i) analysis at a low protein concentration is not always applicable to high concentration formulations; (ii) an investigation of interaction effects of combined factors as well as main effects of single factors is effective for improving conformational stability of proteins; (iii) with the exception of pH, the results of stress testing with regard to aggregation factors would be available for suitable formulation instead of performing time-consuming accelerated testing; (iv) a suitable pH condition should not be determined in stress testing but in accelerated testing, because of inconsistent effects of pH on conformational and storage stabilities. In summary, we propose a three-step strategy, using FTIR, SEC and DOE techniques, to effectively analyze the aggregation factors and perform a rapid screening for suitable conditions of protein formulation. Copyright © 2011 Elsevier B.V. All rights reserved.

Theoretical (in B3LYP/6-3111++G** level), spectroscopic (FT-IR, FT-Raman) and thermogravimetric studies of gentisic acid and sodium, copper(II) and cadmium(II) gentisates.

PubMed

Regulska, E; Kalinowska, M; Wojtulewski, S; Korczak, A; Sienkiewicz-Gromiuk, J; Rzączyńska, Z; Swisłocka, R; Lewandowski, W

2014-11-11

The DFT calculations (B3LYP method with 6-311++G(d,p) mixed with LanL2DZ for transition metals basis sets) for different conformers of 2,5-dihydroxybenzoic acid (gentisic acid), sodium 2,5-dihydroxybenzoate (gentisate) and copper(II) and cadmium(II) gentisates were done. The proposed hydrated structures of transition metal complexes were based on the results of experimental findings. The theoretical geometrical parameters and atomic charge distribution were discussed. Moreover Na, Cu(II) and Cd(II) gentisates were synthesized and the composition of obtained compounds was revealed by means of elemental and thermogravimetric analyses. The FT-IR and FT-Raman spectra of gentisic acid and gentisates were registered and the effect of metals on the electronic charge distribution of ligand was discussed. Copyright © 2014 Elsevier B.V. All rights reserved.

Synthesis of nanocrystalline CdS thin film by SILAR and their characterization

NASA Astrophysics Data System (ADS)

Mukherjee, A.; Satpati, B.; Bhattacharyya, S. R.; Ghosh, R.; Mitra, P.

2015-01-01

Cadmium sulphide (CdS) thin film was prepared by successive ion layer adsorption and reaction (SILAR) technique using ammonium sulphide as anionic precursor. Characterization techniques of XRD, SEM, TEM, FTIR and EDX were utilized to study the microstructure of the films. Structural characterization by x-ray diffraction reveals the polycrystalline nature of the films. Cubic structure is revealed from X-ray diffraction and selected area diffraction (SAD) patterns. The particle size estimated using X-ray line broadening method is approximately 7 nm. Instrumental broadening was taken into account while particle size estimation. TEM shows CdS nanoparticles in the range 5-15 nm. Elemental mapping using EFTEM reveals good stoichiometric composition of CdS. Characteristic stretching vibration mode of CdS was observed in the absorption band of FTIR spectrum. Optical absorption study exhibits a distinct blue shift in band gap energy value of about 2.56 eV which confirms the size quantization.

Material Assessment of L97A1/L96A1 Grenades by Fourier Transform Infrared Spectroscopy and Thermogravimetric Analysis

DTIC Science & Technology

2010-12-01

infrared (FTIR) spectroscopy Differential scanning calorimetry ( DSC ) L97A1/L96A1 grenades Thermogravimetric analysis (TGA) 16. SECURITY CLASSIFICATION OF...Spectroscopy The FTIR scan (fig. 3) shows two baseline materials • The blue spectra represent the Nylon 6 sample • The black spectra represent Nylon 6...The black spectra represent a sample taken from the body of the older grenade body • The relative size and location of all the peaks are identical

Interpretation FTIR spectrum of seawater and sediment in the Ambon Bay (TAD)

NASA Astrophysics Data System (ADS)

Patty, Diana Julaidy; Loupatty, Grace; Sopalauw, Fitria

2017-01-01

Research has done to interpretated FTIR spectrum of seawaters and sediment of the Ambon Bay (TAD). Analysis of samples of sediment and seawater using FTIR spectroscopy. The results showed the sand sediment samples identified Stretch bond OH group (3600-3500 cm-1), N-H Stretch (3400-3300 cm-1), C≡N (2250 cm-1), and NH bending (1640 to 1550 cm-1). And for seawater samples identified bonding group that is N-H Stretch (3400-3350 cm-1), N-H bending (1640 to 1550 cm-1) and C=O (1670-1640 cm-1). The existence of functional groups, carbonyl (C=O), alcohol (OH), carboxyl (COOH) can cause the complexation of metal cations. And the results showed analysis group N-O bond-containing compounds Nitro indicate heavy metal content of Lead (Pb) and group N-H bond-containing compound Amina indicate heavy metal content of Cadmium (Cd).

FTIR, FT-Raman, FT-NMR and quantum chemical investigations of 3-acetylcoumarin

NASA Astrophysics Data System (ADS)

Arjunan, V.; Sakiladevi, S.; Marchewka, M. K.; Mohan, S.

2013-05-01

3-Acetylcoumarin (3AC) was synthesised by a Knoevenagel reaction. Conformational analysis using the B3LYP method was also carried out to determine the most stable conformation of the compound. FTIR and FT-Raman spectra of 3AC have been recorded in the range 4000-400 and 4000-100 cm-1, respectively. 1H and 13C NMR spectra have also been recorded. The complete vibrational assignment and analysis of the fundamental modes of the compound were carried out using the experimental FTIR and FT-Raman data and quantum mechanical studies. The experimental vibrational frequencies were compared with the wavenumbers obtained theoretically from the DFT-B3LYP/B3PW91 gradient calculations employing the standard 6-31G**, high level 6-311++G** and cc-pVTZ basis sets for optimised geometry of the compound. The frontier molecular orbital energies of the compound are determined by DFT method.

Conformational analysis, spectroscopic study (FT-IR, FT-Raman, UV, 1H and 13C NMR), molecular orbital energy and NLO properties of 5-iodosalicylic acid

NASA Astrophysics Data System (ADS)

Karaca, Caglar; Atac, Ahmet; Karabacak, Mehmet

2015-02-01

In this study, 5-iodosalicylic acid (5-ISA, C7H5IO3) is structurally characterized by FT-IR, FT-Raman, NMR and UV spectroscopies. There are eight conformers, Cn, n = 1-8 for this molecule therefore the molecular geometry for these eight conformers in the ground state are calculated by using the ab-initio density functional theory (DFT) B3LYP method approach with the aug-cc-pVDZ-PP basis set for iodine and the aug-cc-pVDZ basis set for the other elements. The computational results identified that the most stable conformer of 5-ISA is the C1 form. The vibrational spectra are calculated DFT method invoking the same basis sets and fundamental vibrations are assigned on the basis of the total energy distribution (TED) of the vibrational modes, calculated with scaled quantum mechanics (SQM) method with PQS program. Total density of state (TDOS) and partial density of state (PDOS) and also overlap population density of state (COOP or OPDOS) diagrams analysis for C1 conformer were calculated using the same method. The energy and oscillator strength are calculated by time-dependent density functional theory (TD-DFT) results complement with the experimental findings. Besides, charge transfer occurring in the molecule between HOMO and LUMO energies, frontier energy gap, molecular electrostatic potential (MEP) are calculated and presented. The NMR chemical shifts (1H and 13C) spectra are recorded and calculated using the gauge independent atomic orbital (GIAO) method. Mulliken atomic charges of the title molecule are also calculated, interpreted and compared with salicylic acid. The optimized bond lengths, bond angles and calculated NMR and UV, vibrational wavenumbers showed the best agreement with the experimental results.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Baybas, Demet, E-mail: dbaybas@cumhuriyet.edu.tr; Ulusoy, Ulvi, E-mail: ulusoy@cumhuriyet.edu.tr

The composite of synthetically produced hydroxyapatite (HAP) and polyacrylamide was prepared (PAAm-HAP) and characterized by BET, FT-IR, TGA, XRD, SEM and PZC analysis. The adsorptive features of HAP and PAAm-HAP were compared for UO{sub 2}{sup 2+} and Th{sup 4+}. The entrapment of HAP into PAAm-HAP did not change the structure of HAP. Both structures had high affinity to the studied ions. The adsorption capacity of PAAm-HAP was than that of HAP. The adsorption dependence on pH and ionic intensity provided supportive evidences for the effect of complex formation on adsorption process. The adsorption kinetics was well compatible to pseudo secondmore » order model. The values of enthalpy and entropy changes were positive. Th{sup 4+} adsorption from the leachate obtained from a regional fluorite rock confirmed the selectivity of PAAm-HAP for this ion. In consequence, PAAm-HAP should be considered amongst favorite adsorbents for especially deposition of nuclear waste containing U and Th, and radionuclide at secular equilibrium with these elements. - Graphical abstract: SEM images of hydroxyapatite (HAP) and polyacrylamide-hydroxyapatite (PAAm-HAP), and the adsorption isotherms for Uranium and Thorium. Highlights: Black-Right-Pointing-Pointer Composite of PAAm-HAP was synthesized from hydroxyapatite and polyacrylamide. Black-Right-Pointing-Pointer The materials were characterized by BET, FT-IR, XRD, SEM, TGA and PZC analysis. Black-Right-Pointing-Pointer HAP and PAAm-HAP had high sorption capacity and very rapid uptake for UO{sub 2}{sup 2+} and Th{sup 4+}. Black-Right-Pointing-Pointer Super porous PAAm was obtained from PAAm-HAP after its removal of HAP content. Black-Right-Pointing-Pointer The composite is potential for deposition of U, Th and its associate radionuclides.« less

Silica nanosphere-supported palladium(II) furfural complex as a highly efficient and recyclable catalyst for oxidative amination of aldehydes.

PubMed

Sharma, R K; Sharma, Shivani

2014-01-21

The present work reports the fabrication of a novel and highly efficient silica nanospheres-based palladium catalyst (SiO2@APTES@Pd-FFR) via immobilization of a palladium complex onto silica nanospheres functionalized with 3-aminopropyltriethoxysilane (APTES), and its catalytic application for the oxidative amination of aldehydes to yield commercially important amides. The structure of the nano-catalyst was confirmed by Solid-state (13)C CPMAS and (29)Si CPMAS NMR spectroscopy, Brunauer-Emmett-Teller (BET) surface area analysis, Fourier transform infrared spectroscopy (FT-IR), Energy dispersive X-ray fluorescence spectroscopy (ED-XRF), Atomic absorption spectroscopy (AAS), Transmission electron microscopy (TEM) and elemental analysis. The nano-catalyst was found to be highly effective for the oxidative amination of aldehydes using hydrogen peroxide as an environmentally benign oxidant to give amides. The effect of various reaction parameters such as temperature, amount of catalyst, reaction time, type of solvent, oxidant used, substrate to oxidant ratio etc. have been demonstrated to achieve high catalytic efficacy. Moreover, this nanostructured catalyst could be recovered with simplicity and reused for several cycles without any significant loss in its catalytic activity. In addition, the stability of the reused nano-catalyst was proved by FT-IR and HRTEM techniques. It is worth noting that the features of mild reaction conditions, simple work-up procedure, high product yield, no use of toxic organic solvents, high turn-over frequency (TOF), and easy recovery and reusability of the present quasi-homogeneous nano-catalyst make this protocol an attractive alternative to the existing catalytic methods for the oxidative amination of aldehydes to furnish industrially important amides.

Synthesis, characterization, and biological activity of some novel Schiff bases and their Co(II) and Ni(II) complexes: A new route for Co3O4 and NiO nanoparticles for photocatalytic degradation of methylene blue dye

NASA Astrophysics Data System (ADS)

Nassar, Mostafa Y.; Aly, Hisham M.; Abdelrahman, Ehab A.; Moustafa, Moustafa E.

2017-09-01

Six novel Co(II) and Ni(II)-triazole Schiff base complexes have been successfully synthesized by refluxing the prepared triazole Schiff bases with CoCl2·6H2O or NiCl2·6H2O. The Schiff base ligands were prepared through condensation of 3-R-4-amino-5-hydrazino-1,2,4-triazole with dibenzoylmethane [Rdbnd H, CH3, and CH2CH3; namely, L1, L2, and L3, respectively]. The prepared Co(II) and Ni(II) complexes have been identified using elemental analysis, FT-IR, UV-Vis, magnetic moment, conductivity, and thermal analysis. On the basis of the conductance results, it was concluded that all the prepared complexes are nonelectrolytes. Interestingly, the prepared Co(II) and Ni(II) complexes were employed as precursors for producing of Co3O4 and NiO nanoparticles, respectively. The produced nanostructures have been identified by XRD, HR-TEM, FT-IR and UV-Vis spectra. The produced nanoparticles revealed good photocatalytic activity for the degradation of methylene blue dye under UV illumination in presence of hydrogen peroxide. The percent of degradation was estimated to be 55.71% in 420.0 min and 90.43% in 360.0 min for Co3O4 and NiO, respectively. Moreover, the synthesized complexes, nano-sized Co3O4, and NiO products have been examined, employing modified Bauer- Kirby method, for antifungal (Candida albicans and Aspergillus flavus) and antibacterial (Staphylococcus aureus and Escherichia coli) activities.

Applications of FT-IR spectrophotometry in cancer diagnostics.

PubMed

Bunaciu, Andrei A; Hoang, Vu Dang; Aboul-Enein, Hassan Y

2015-01-01

This review provides a brief background to the application of infrared spectroscopy, including Fourier transform-infrared spectroscopy, in biological fluids. It is not meant to be complete or exhaustive but to provide the reader with sufficient background for selected applications in cancer diagnostics. Fourier transform-infrared spectroscopy (FT-IR) is a fast and nondestructive analytical method. The infrared spectrum of a mixture serves as the basis to quantitate its constituents, and a number of common clinical chemistry tests have proven to be feasible using this approach. This review focuses on biomedical FT-IR applications, published in the period 2009-2013, used for early detection of cancer through qualitative and quantitative analysis.

ANN-based calibration model of FTIR used in transformer online monitoring

NASA Astrophysics Data System (ADS)

Li, Honglei; Liu, Xian-yong; Zhou, Fangjie; Tan, Kexiong

2005-02-01

Recently, chromatography column and gas sensor have been used in online monitoring device of dissolved gases in transformer oil. But some disadvantages still exist in these devices: consumption of carrier gas, requirement of calibration, etc. Since FTIR has high accuracy, consume no carrier gas and require no calibration, the researcher studied the application of FTIR in such monitoring device. Experiments of "Flow gas method" were designed, and spectrum of mixture composed of different gases was collected with A BOMEM MB104 FTIR Spectrometer. A key question in the application of FTIR is that: the absorbance spectrum of 3 fault key gases, including C2H4, CH4 and C2H6, are overlapped seriously at 2700~3400cm-1. Because Absorbance Law is no longer appropriate, a nonlinear calibration model based on BP ANN was setup to in the quantitative analysis. The height absorbance of C2H4, CH4 and C2H6 were adopted as quantitative feature, and all the data were normalized before training the ANN. Computing results show that the calibration model can effectively eliminate the cross disturbance to measurement.

Comparison of Fourier transform infrared spectrometry and 2,4-dinitrophenylhydrazine impinger techniques for the measurement of formaldehyde in vehicle exhaust

DOE Office of Scientific and Technical Information (OSTI.GOV)

Haack, L.P.; LaCourse, D.L.; Korniski, T.J.

1986-01-01

Experiments were conducted to validate a Fourier transform infrared (FT-IR) sampling and analysis system for measurement of trace gases in vehicle exhaust utilizing gasoline-, gasohol-, diesel-, and methanol-fueled vehicles as the emission source and formaldehyde (HCHO) as the test molecule. The 2,4-dinitrophenylhydrazine impinger method was chosen as the reference method. Diluted exhaust was drawn continuously though the FT-IR cell and measured every 3 s. The FT-IR signals were averaged over a complete driving-test cycle and compared to the concentration determined from concurrent impinger sampling. By impinger measurements it was shown that HCHO losses between the tailpipe and the FT-IR cellmore » were on the order of only 5%, independent of vehicle type or HCHO concentration (0.02-8.5 ppm). Comparisons between FT-IR and impinger measurements on 43 tests of methanol-fueled vehicles under transient conditions (diluted-exhaust HCHO 0.28-8.5 ppm) showed FT-IR/impinger = 1.055 +/- 0.095. 19 references, 5 figures, 5 tables.« less

Determination of trans Fat in Selected Fast Food Products and Hydrogenated Fats of India Using Attenuated Total Reflection Fourier Transform Infrared (ATR-FTIR) Spectroscopy.

PubMed

Khan, Mohd Umar; Hassan, Mohammad Fahimul; Rauf, Abdul

2017-01-01

This paper reports the application of a simple and rapid method for the determination of trans fatty acid (TFA) content in some of the selected Indian fast food products and hydrogenated fats using Fourier transform infrared (FTIR) spectroscopy in conjunction with second derivative procedure. FTIR spectroscopy has been successfully applied to trans measurement using the absorbance bands at or near 966 cm -1 in the FTIR spectra. It was found from the analysis that TFA content of fast food product was ranging from 1.57% to 3.83% of the total fat while for hydrogenated fats, comparatively large quantity of TFA was detected in the range of 3.31% to 4.73%. Since GC-FID is most widely used method for the determination of fatty acid (FA) composition, this method was used for the sake of comparison. Value of regression coefficient was found very close to one (0.99503) with standard deviation of 0.10247 showing a good agreement between GC-FID and proposed ATR-FTIR method.

Distinction of broken cellular wall Ganoderma lucidum spores and G. lucidum spores using FTIR microspectroscopy.

PubMed

Chen, Xianliang; Liu, Xingcun; Sheng, Daping; Huang, Dake; Li, Weizu; Wang, Xin

2012-11-01

In this paper, FTIR microspectroscopy was used to identify broken cellular wall Ganoderma lucidum spores and G. lucidum spores. For IR spectra, broken cellular wall G. lucidum spores and G. lucidum spores were mainly different in the regions of 3000-2800, 1660-1600, 1400-1200 and 1100-1000 cm(-1). For curve fitting, the results showed the differences in the protein secondary structures and the polysaccharide structures/content between broken cellular wall G. lucidum spores and G. lucidum spores. Moreover, the value of A1078/A1741 might be a potentially useful factor to distinguish broken cellular wall G. lucidum spores from G. lucidum spores. Additionally, FTIR microspectroscopy could identify broken cellular wall G. lucidum spores and G. lucidum spores accurately when it was combined with hierarchical cluster analysis. The result suggests FTIR microspectroscopy is very simple and efficient for distinction of broken cellular wall G. lucidum spores and G. lucidum spores. The result also indicates FTIR microspectroscopy may be useful for TCM identification. Copyright © 2012 Elsevier B.V. All rights reserved.

Structural study of Cu(II) complexes with benzo[b]furancarboxylic acids

NASA Astrophysics Data System (ADS)

Kalinowska, Diana; Klepka, Marcin T.; Wolska, Anna; Drzewiecka-Antonik, Aleksandra; Ostrowska, Kinga; Struga, Marta

2017-11-01

Four Cu(II) complexes with 2- and 3-benzo[b]furancarboxylic acids have been synthesized and characterized using combination of two spectroscopic techniques. These techniques were: (i) FTIR and (ii) XAFS. FTIR analysis confirmed that complexes were formed and gave insight into identification of possible coordinating groups to the metallic center. XANES analysis indicated that the oxidation state of Cu is +2. EXAFS analysis allowed to identify that the first coordination sphere is formed by 4-5 oxygen atoms with the Cu-O distances around 2 Å. Combining these techniques it was possible to structurally describe novel Cu(II) complexes with benzo[b]furancarboxylic acids.

Rapid qualitative and quantitative analysis of opiates in extract of poppy head via FTIR and chemometrics: towards in-field sensors.

PubMed

Turner, Nicholas W; Cauchi, Michael; Piletska, Elena V; Preston, Christopher; Piletsky, Sergey A

2009-07-15

Identification and quantification of the opiates morphine and thebaine has been achieved in three commercial poppy cultivars using FTIR-ATR spectroscopy, from a simple and rapid methanolic extraction, suitable for field analysis. The limits of detection were 0.13 mg/ml (0.013%, w/v) and 0.3 mg/ml (0.03%, w/v) respectively. The concentrations of opiates present were verified with HPLC-MS. The chemometrics has been used to identify specific "signature" peaks in the poppy IR spectra for characterisation of cultivar by its unique fingerprint offering a potential forensic application in opiate crop analysis.

Synthesis aspects, structural, spectroscopic, antimicrobial and room temperature ferromagnetism of zinc iodide complex with Schiff based ligand

NASA Astrophysics Data System (ADS)

Shakila, K.; Kalainathan, S.

2015-01-01

In this paper, we report the successful growth of complex compound of zinc iodide with thiocarbamide by slow evaporation method. The single crystal XRD study reveals that the crystal belongs to monoclinic system with centrosymmetric space group and powder XRD analysis shows that the perfect crystalline nature of the crystal. The presence of functional group and element were confirmed from FT-IR and EDAX analysis. Optical absorbance of the grown crystal was studied by UV-Vis spectrophotometer. The optical constants were calculated from the optical absorbance data such as refractive index (n), extinction coefficient (K) and reflectance (R). The optical band gap (Eg) of thiocarbamide zinc iodide crystal is 4.22 eV. The magnetic properties of grown crystal have been determined by Vibrating Sample Magnetometry (VSM). Room temperature magnetization revealed a ferromagnetic behaviour for the grown crystal. The antibacterial and antifungal activities of the title compound were performed by well diffusion method and MIC method against the standard bacteria like Staphylococcus aureus, Escherichia coli, Klebsiella pneumonia and against fungus like Aspergillus niger, Rhizopus sps and Penicillium sps. Thermal behaviour of the crystal has been investigated using thermogravimetric analysis (TGA) and differential thermal analysis (DTA).

Investigation of charge-transfer hydrogen bonding interaction of 1-(2-pyridylazo)-2-naphthol (PAN) and 4-(2-Pyridylazo)resorcinol (PAR) with chloranilic acid through experimental and DFT studies

NASA Astrophysics Data System (ADS)

Karmakar, Animesh; Singh, Bula

2018-07-01

The H-bonding interaction of 1-(2-pyridylazo)-2-naphthol (PAN) and 4-(2-Pyridylazo) resorcinol (PAR) with chloranilic acid (CLA) have been considered spectroscopically in methanol solvent. PAN and PAR were used as a ligand and this two ligands has diverse application in spectrophotometric, chelatometric analysis of different metal ions. However, it is seen as of the literature analysis that no molecular complex of PAN and PAR with CLA was reported. The creation of charge-transfer H-bonded adduct gives a outlook to progress the physico-chemical scenery of the donor. So the complex of PAN and PAR with chloranilic acid was recounted in this work in methanol medium. Both the hydrogen-bonded molecular complexes have been prepared and identified using 1H NMR, FT-IR, and elemental analysis. Spectroscopic data point out that PAN and PAR discretely interact with CLA by a physically potent H-bonding interaction. The thermal constancy of the above molecular complexes has been determined by TGA-DTA analysis. The computational calculation also supported the development of the H-bonded charge-transfer adduct.

Indoor air pollution and its association with poor lung function, microalbuminuria and variations in blood pressure among kitchen workers in India: a cross-sectional study.

PubMed

Singh, Amarnath; Kesavachandran, Chandrasekharan Nair; Kamal, Ritul; Bihari, Vipin; Ansari, Afzal; Azeez, Parappurath Abdul; Saxena, Prem Narain; Ks, Anil Kumar; Khan, Altaf Hussain

2017-04-04

The present study is an attempt to explore the association between kitchen indoor air pollutants and physiological profiles in kitchen workers with microalbuminuria (MAU) in north India (Lucknow) and south India (Coimbatore). The subjects comprised 145 control subjects, 233 kitchen workers from north India and 186 kitchen workers from south India. Information related to the personal and occupational history and health of the subjects at both locations were collected using a custom-made questionnaire. Worker lung function was measured using a spirometer. Blood pressure was monitored using a sphygmomanometer. Urinary MAU was measured using a urine analyzer. Indoor air monitoring in kitchens for particulate matter (PM), total volatile organic compounds (TVOC), carbon dioxide (CO 2 ) and carbon monoxide (CO) was conducted using indoor air quality monitors. The size and shape of PM in indoor air was assessed using a scanning electron microscope (SEM). Fourier transform infrared (FTIR) spectroscopy was used to detect organic or inorganic compounds in the air samples. Particulate matter concentrations (PM 2.5 and PM 1 ) were significantly higher in both north and south Indian kitchens than in non-kitchen areas. The concentrations of TVOC, CO and CO 2 were higher in the kitchens of north and south India than in the control locations (non-kitchen areas). Coarse, fine and ultrafine particles and several elements were also detected in kitchens in both locations by SEM and elemental analysis. The FTIR spectra of kitchen indoor air at both locations show the presence of organic chemicals. Significant declines in systolic blood pressure and lung function were observed in the kitchen workers with MAU at both locations compared to those of the control subjects. A higher prevalence of obstruction cases with MAU was observed among the workers in the southern region than in the controls (p < 0.01). Kitchen workers in south India have lower lung capacities and a greater risk of obstructive and restrictive abnormalities than their north Indian counterparts. The study showed that occupational exposure to multiple kitchen indoor air pollutants (ultrafine particles, PM 2.5 , PM 1 , TVOC, CO, CO 2 ) and FTIR-derived compounds can be associated with a decline in lung function (restrictive and obstructive patterns) in kitchen workers with microalbuminuria. Further studies in different geographical locations in India among kitchen workers on a wider scale are required to validate the present findings.

Synchrotron FTIR microspectroscopy reveals early adipogenic differentiation of human mesenchymal stem cells at single-cell level

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, Zhixiao; University of Chinese Academy of Science, Beijing 100049; Tang, Yuzhao

Human mesenchymal stem cells (hMSCs) have been used as an ideal in vitro model to study human adipogenesis. However, little knowledge of the early stage differentiation greatly hinders our understanding on the mechanism of the adipogenesis processes. In this study, synchrotron radiation-based Fourier transform infrared (SR-FTIR) microspectroscopy was applied to track the global structural and compositional changes of lipids, proteins and nucleic acids inside individual hMSCs along the time course. The multivariate analysis of the SR-FTIR spectra distinguished the dynamic and significant changes of the lipids and nucleic acid at early differentiation stage. Importantly, changes of lipid structure during early daysmore » (Day 1–3) of differentiation might serve as a potential biomarker in identifying the state in early differentiation at single cell level. These results proved that SR-FTIR is a powerful tool to study the stem cell fate determination and early lipogenesis events. - Highlights: • Molecular events occur in the early adipogenic differentiation stage of hMSCs are studied by SR-FTIR. • SR-FTIR data suggest that lipids may play an important role in hMSCs determination. • As potential biomarkers, lipids peaks can identify the state of cell in early differentiation stage at single-cell level.« less

Application of reflectance micro-Fourier Transform infrared analysis to the study of coal macerals: An example from the Late Jurassic to Early Cretaceous coals of the Mist Mountain Formation, British Columbia, Canada

USGS Publications Warehouse

Mastalerz, Maria; Bustin, R.M.

1996-01-01

The applicability of the reflectance micro-Fourier Transform infra-red spectroscopy (FTIR) technique for analyzing the distribution of functional groups in coal macerals is discussed. High quality of spectra, comparable to those obtained using other FTIR techniques (KBr pellet and transmission micro-FTIR), indicate this technique can be applied to characterizing functional groups under most conditions. The ease of sample preparation, the potential to analyze large intact samples, and ability to characterize organic matter in areas as small as 20 ??m are the main advantages of reflectance micro-FTIR. The quantitative aspects of reflectance micro-FTIR require further study. The examples from the coal seams of the Mist Mountain Formation, British Columbia show that at high volatile bituminous rank, reflectance micro-FTIR provides valuable information on the character of aliphatic chains of vitrinite and liptinite macerals. Because the character of aliphatic chains influences bond disassociation energies, such information is useful from a hydrocarbon generation viewpoint. In medium volatile bituminous coal liptinite macerals are usually not detectable but this technique can be used to study the degree of oxidation and reactivity of vitrinite and semifusinite.

Importance of tissue preparation methods in FTIR micro-spectroscopical analysis of biological tissues: 'traps for new users'.

PubMed

Zohdi, Vladislava; Whelan, Donna R; Wood, Bayden R; Pearson, James T; Bambery, Keith R; Black, M Jane

2015-01-01

Fourier Transform Infrared (FTIR) micro-spectroscopy is an emerging technique for the biochemical analysis of tissues and cellular materials. It provides objective information on the holistic biochemistry of a cell or tissue sample and has been applied in many areas of medical research. However, it has become apparent that how the tissue is handled prior to FTIR micro-spectroscopic imaging requires special consideration, particularly with regards to methods for preservation of the samples. We have performed FTIR micro-spectroscopy on rodent heart and liver tissue sections (two spectroscopically very different biological tissues) that were prepared by desiccation drying, ethanol substitution and formalin fixation and have compared the resulting spectra with that of fully hydrated freshly excised tissues. We have systematically examined the spectra for any biochemical changes to the native state of the tissue caused by the three methods of preparation and have detected changes in infrared (IR) absorption band intensities and peak positions. In particular, the position and profile of the amide I, key in assigning protein secondary structure, changes depending on preparation method and the lipid absorptions lose intensity drastically when these tissues are hydrated with ethanol. Indeed, we demonstrate that preserving samples through desiccation drying, ethanol substitution or formalin fixation significantly alters the biochemical information detected using spectroscopic methods when compared to spectra of fresh hydrated tissue. It is therefore imperative to consider tissue preparative effects when preparing, measuring, and analyzing samples using FTIR spectroscopy.

Vibrational (FT-IR, Raman) and DFT analysis on the structure of labile drugs. The case of crystalline tebipenem and its ester

NASA Astrophysics Data System (ADS)

Paczkowska, Magdalena; Mizera, Mikołaj; Dzitko, Jakub; Lewandowska, Kornelia; Zalewski, Przemysław; Cielecka-Piontek, Judyta

2017-04-01

A tebipenem is active form of the first, oral carbapenem antibiotic - tebipenem pivoxyl. The optimized conformations of tebipenem pivoxyl and tebipenem were determinated by quantum-chemical calculations performed with the use of B3LYP functional and 6-31G(d,p) as a basis set. For the most stable conformations of tebipenem and its ester were established theoretical Raman and FT-IR spectra. The theoretical approach in significant part was support for identification of experimental Raman (400-4000 cm-1) and FT-IR (100-4000 cm-1) of tebipenem and tebipenem pivoxil. The geometric structure of molecules, HOMO and LUMO orbitals and molecular electrostatic potential were also determined. The benefits of applying FT-IR and Raman scattering spectroscopy for characterization of tebipenem and its ester consisted in demonstrating differences in their spectral properties.

Comparison of red blood cells from gastric cancer patients and healthy persons using FTIR spectroscopy

NASA Astrophysics Data System (ADS)

Liu, Hui; Su, Qinglong; Sheng, Daping; Zheng, Wei; Wang, Xin

2017-02-01

In this paper, FTIR spectroscopy was used to compare gastric cancer patients' red blood cells (RBCs) with healthy persons' RBCs. IR spectra were acquired with high resolution. The A1653/A1543 (the protein secondary structures), A1543/A2958 (the relative content of proteins and lipids), A1106/A1166 (the structure and content changes of sugars) and A1543/A1106 (the relative content of proteins and sugars) ratios of gastric cancer patients' RBCs were significantly different from those of healthy persons' RBCs. Curve fitting results showed that the protein secondary structures and sugars' structures had differences between gastric cancer patients' and healthy persons' RBCs. Additionally, FTIR spectroscopy could obtain 95% sensitivity, 70% specificity, 84.2% accuracy and 80.9% positive predictive value in combination with canconical discriminant analysis. The above results indicate FTIR spectroscopy may be useful for diagnosing gastric cancer.

A Combined Approach of Infrared Spectroscopy and Multivariate Analysis for the Simultaneous Determination of Sugars and Fructans in Strawberry Juices During Storage.

PubMed

Cassani, Lucía; Santos, Mauricio; Gerbino, Esteban; Del Rosario Moreira, María; Gómez-Zavaglia, Andrea

2018-03-01

In this work, a Fourier transform mid-infrared spectroscopy (FTIR)-based method was developed for simultaneously quantifying simple sugars and exogenously added fructooligosaccharides (FOS) in strawberry juices preserved for up to 14 d using nonthermal techniques (geraniol and vanillin+ultrasound). The main spectral differences were observed in the 1200 to 900 cm -1 region. The presence of FOS was identified by the typical bands at 1134, 1034, and 935 cm -1 . During storage, a significant decrease of sucrose was concomitant to an increase of glucose and fructose in juices stored without any previous preservation treatment, as determined by high-performance liquid chromatography (HPLC). A principal component analysis was performed on the FTIR spectra corresponding to the different treatments. The groups observed explained more than 94% of the variance and were related to changes in the carbohydrate composition during storage. Then, different partial least square models (PLS) were defined to determine the concentrations of glucose, sucrose, fructose, and those of exogenously added FOS with degrees of polymerization within 3 and 5. The carbohydrates' concentrations determined by HPLC were used as reference method. The models were validated with independent sets of data. The mean of predicted values fitted nicely those obtained by HPLC (correlation and R 2  > 0.97), thus supporting the use of the PLS models to monitor the quality of strawberry juices in unknown samples. In conclusion, FTIR spectroscopy appears as an adequate analytical tool to quick assess whether juice formulations meet specifications in terms of authenticity, contamination and/or deterioration. FTIR spectroscopy provided a method potentially transferable to the food industry when associated with the multivariate analysis. The robust 21 PLS models defined in this work provided reliable tools for the rapid monitoring of juices' authenticity and/or deterioration. In this regard, FTIR associated to multivariate analysis enabled the determination of different sugars in a single measurement without the need of pure sugars as standards. This experimental simplicity supports the use of FTIR at the production line, and also contributes to save time in determining carbohydrates' composition and stability, in an environmentally friendly way. © 2017 Institute of Food Technologists®.

The application of ATR-FTIR spectroscopy and multivariate data analysis to study drug crystallisation in the stratum corneum.

PubMed

Goh, Choon Fu; Craig, Duncan Q M; Hadgraft, Jonathan; Lane, Majella E

2017-02-01

Drug permeation through the intercellular lipids, which pack around and between corneocytes, may be enhanced by increasing the thermodynamic activity of the active in a formulation. However, this may also result in unwanted drug crystallisation on and in the skin. In this work, we explore the combination of ATR-FTIR spectroscopy and multivariate data analysis to study drug crystallisation in the skin. Ex vivo permeation studies of saturated solutions of diclofenac sodium (DF Na) in two vehicles, propylene glycol (PG) and dimethyl sulphoxide (DMSO), were carried out in porcine ear skin. Tape stripping and ATR-FTIR spectroscopy were conducted simultaneously to collect spectral data as a function of skin depth. Multivariate data analysis was applied to visualise and categorise the spectral data in the region of interest (1700-1500cm -1 ) containing the carboxylate (COO - ) asymmetric stretching vibrations of DF Na. Spectral data showed the redshifts of the COO - asymmetric stretching vibrations for DF Na in the solution compared with solid drug. Similar shifts were evident following application of saturated solutions of DF Na to porcine skin samples. Multivariate data analysis categorised the spectral data based on the spectral differences and drug crystallisation was found to be confined to the upper layers of the skin. This proof-of-concept study highlights the utility of ATR-FTIR spectroscopy in combination with multivariate data analysis as a simple and rapid approach in the investigation of drug deposition in the skin. The approach described here will be extended to the study of other actives for topical application to the skin. Copyright © 2016 Elsevier B.V. All rights reserved.

UV–Vis and ATR–FTIR spectroscopic investigations of postmortem interval based on the changes in rabbit plasma

PubMed Central

Wang, Qi; He, Haijun; Li, Bing; Lin, Hancheng; Zhang, Yinming; Zhang, Ji

2017-01-01

Estimating PMI is of great importance in forensic investigations. Although many methods are used to estimate the PMI, a few investigations focus on the postmortem redistribution. In this study, ultraviolet–visible (UV–Vis) measurement combined with visual inspection indicated a regular diffusion of hemoglobin into plasma after death showing the redistribution of postmortem components in blood. Thereafter, attenuated total reflection–Fourier transform infrared (ATR–FTIR) spectroscopy was used to confirm the variations caused by this phenomenon. First, full-spectrum partial least-squares (PLS) and genetic algorithm combined with PLS (GA-PLS) models were constructed to predict the PMI. The performance of GA-PLS model was better than that of full-spectrum PLS model based on its root mean square error (RMSE) of cross-validation of 3.46 h (R2 = 0.95) and the RMSE of prediction of 3.46 h (R2 = 0.94). The investigation on the similarity of spectra between blood plasma and formed elements also supported the role of redistribution of components in spectral changes in postmortem plasma. These results demonstrated that ATR-FTIR spectroscopy coupled with the advanced mathematical methods could serve as a convenient and reliable tool to study the redistribution of postmortem components and estimate the PMI. PMID:28753641

Characterizing Aeroallergens by Infrared Spectroscopy of Fungal Spores and Pollen

PubMed Central

Zimmermann, Boris; Tkalčec, Zdenko; Mešić, Armin; Kohler, Achim

2015-01-01

Background Fungal spores and plant pollen cause respiratory diseases in susceptible individuals, such as asthma, allergic rhinitis and hypersensitivity pneumonitis. Aeroallergen monitoring networks are an important part of treatment strategies, but unfortunately traditional analysis is time consuming and expensive. We have explored the use of infrared spectroscopy of pollen and spores for an inexpensive and rapid characterization of aeroallergens. Methodology The study is based on measurement of spore and pollen samples by single reflectance attenuated total reflectance Fourier transform infrared spectroscopy (SR-ATR FTIR). The experimental set includes 71 spore (Basidiomycota) and 121 pollen (Pinales, Fagales and Poales) samples. Along with fresh basidiospores, the study has been conducted on the archived samples collected within the last 50 years. Results The spectroscopic-based methodology enables clear spectral differentiation between pollen and spores, as well as the separation of confamiliar and congeneric species. In addition, the analysis of the scattering signals inherent in the infrared spectra indicates that the FTIR methodology offers indirect estimation of morphology of pollen and spores. The analysis of fresh and archived spores shows that chemical composition of spores is well preserved even after decades of storage, including the characteristic taxonomy-related signals. Therefore, biochemical analysis of fungal spores by FTIR could provide economical, reliable and timely methodologies for improving fungal taxonomy, as well as for fungal identification and monitoring. This proof of principle study shows the potential for using FTIR as a rapid tool in aeroallergen studies. In addition, the presented method is ready to be immediately implemented in biological and ecological studies for direct measurement of pollen and spores from flowers and sporocarps. PMID:25867755

Study of consumer fireworks post-blast residues by ATR-FTIR.

PubMed

Martín-Alberca, Carlos; Zapata, Félix; Carrascosa, Héctor; Ortega-Ojeda, Fernando E; García-Ruiz, Carmen

2016-03-01

Specific analytical procedures are requested for the forensic analysis of pre- and post-blast consumer firework samples, which present significant challenges. Up to date, vibrational spectroscopic techniques such as Fourier transform infrared spectroscopy (FTIR) have not been tested for the analysis of post-blast residues in spite of their interesting strengths for the forensic field. Therefore, this work proposes a simple and fast procedure for the sampling and analysis of consumer firework post-blast residues by a portable FTIR instrument with an Attenuated Total Reflection (ATR) accessory. In addition, the post-blast residues spectra of several consumer fireworks were studied in order to achieve the identification of their original chemical compositions. Hence, this work analysed 22 standard reagents usually employed to make consumer fireworks, or because they are related to their combustion products. Then, 5 different consumer fireworks were exploded, and their residues were sampled with dry cotton swabs and directly analysed by ATR-FTIR. In addition, their pre-blast fuses and charges were also analysed in order to stablish a proper comparison. As a result, the identification of the original chemical compositions of the post-blast samples was obtained. Some of the compounds found were potassium chlorate, barium nitrate, potassium nitrate, potassium perchlorate or charcoal. An additional study involving chemometric tools found that the results might greatly depend on the swab head type used for the sampling, and its sampling efficiency. The proposed procedure could be used as a complementary technique for the analysis of consumer fireworks post-blast residues. Copyright © 2015 Elsevier B.V. All rights reserved.

In-situ preparation of functionalized molecular sieve material and a methodology to remove template

NASA Astrophysics Data System (ADS)

Yadav, Rekha; Ahmed, Maqsood; Singh, Arvind Kumar; Sakthivel, Ayyamperumal

2016-03-01

A series of diaminosilane-functionalized silicoaluminophosphate molecular sieve (SAPO-37) was prepared by in-situ synthesis, and a novel method was developed for the selective removal of structure directing agent (SDA)/template from the functionalized SAPO-37.The complete removal of the SDA was evident according to FT-IR, TGA, 13C MAS-NMR and elemental analysis. The developed method was found to be efficient for removal of template from microporous molecular sieve viz., SAPO-37 and can be applied for other microporous molecular sieves such as SAPO-5, SAPO-40, etc. The powder XRD pattern of the template-removed samples showed a highly crystalline SAPO-37 phase. Argentometric titration revealed that more than 90% of diamine functionality exposed on the surface was accessible for catalytic applications. The resultant materials showed promising activity for ring opening of epoxide with aniline to yield β-amino-alcohol.

Nitrated graphene oxide and its catalytic activity in thermal decomposition of ammonium perchlorate

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhang, Wenwen; Luo, Qingping; Duan, Xiaohui

2014-02-01

Highlights: • The NGO was synthesized by nitrifying homemade GO. • The N content of resulted NGO is up to 1.45 wt.%. • The NGO can facilitate the decomposition of AP and release much heat. - Abstract: Nitrated graphene oxide (NGO) was synthesized by nitrifying homemade GO with nitro-sulfuric acid. Fourier transform infrared spectroscopy (FTIR), laser Raman spectroscopy, CP/MAS {sup 13}C NMR spectra and X-ray photoelectron spectroscopy (XPS) were used to characterize the structure of NGO. The thickness and the compositions of GO and NGO were analyzed by atomic force microscopy (AFM) and elemental analysis (EA), respectively. The catalytic effectmore » of the NGO for the thermal decomposition of ammonium perchlorate (AP) was investigated by differential scanning calorimetry (DSC). Adding 10% of NGO to AP decreases the decomposition temperature by 106 °C and increases the apparent decomposition heat from 875 to 3236 J/g.« less

Research of Co(II) Adsorption on Silica Gel Grafted with Dithiocarbamate (DTC-SiO2) in Aqueous Solution

NASA Astrophysics Data System (ADS)

Yao, Qingxu; Xu, Peng; Huo, Yonggang; Shang, Aiguo; Yu, Fengmei

2018-01-01

Dithiocarbamate grafted silica gel (DTC-SiO2) was prepared following two simple reaction steps. The properties of the composite were characterized by FTIR, SEM and element analysis. Its ability to remove Co2+ ions in aqueous solution with low concentration was also studied by static adsorption experiments. The effects of pH value in solution, contact time and temperature were investigated. The results show that the DTC-SiO2 exhibits excellent adsorption property for Co2+. The adsorption kinetics could be well described by pseudo-second-order model and the adsorption isotherms could be depicted by both Freundlich and Dubinin-Radushkevich models. The adsorption process belongs to chemisorption. The slightly influence of common interfering metal ions (Na+, K+, Ca2+ and Mg2+) on the adsorption capacity revealing the synthesized DTC-SiO2 performs excellent selective adsorption to Co2+.

Synthesis and Spectral Evaluation of Some Unsymmetrical Mesoporphyrinic Complexes

PubMed Central

Boscencu, Rica; Oliveira, Anabela Sousa; Ferreira, Diana P.; Ferreira, Luís Filipe Vieira

2012-01-01

Synthesis and spectral evaluation of new zinc and copper unsymmetrical mesoporphyrinic complexes are reported. Zn(II)-5-(4-acetoxy-3-methoxyphenyl)-10,15,20- tris-(4-carboxymethylphenyl)porphyrin, Zn(II)-5-[(3,4-methylenedioxy)phenyl]-10,15,20- tris-(4-carboxymethylphenyl)porphyrin, Cu(II)-5-(4-acetoxy-3-methoxyphenyl)-10,15,20- tris-(4-carboxymethylphenyl)porphyrin and Cu(II)-5-[(3,4-methylenedioxy)phenyl]-10,15,20- tris-(4-carboxymethylphenyl)porphyrin were synthesized using microwave-assisted synthesis. The complexes were characterized by elemental analysis, FT-IR, UV-Vis, EPR and NMR spectroscopy, which fully confirmed their structure. The spectral absorption properties of the porphyrinic complexes were studied in solvents with different polarities. Fluorescence emission and singlet oxygen formation quantum yields were evaluated for the compounds under study, revealing high yields for the zinc derivatives. The copper complexes are not emissive and only display residual capacity for singlet oxygen formation. PMID:22942693

Biodegradation of lignin by Agaricus Bisporus

DOE Office of Scientific and Technical Information (OSTI.GOV)

Vane, C.H.; Abbott, G.D.; Head, I.M.

The lignolytic activity of Agaricus bisporus will be addressed in this paper. Sound and fungally degraded lignins were characterized by Pyrolysis-Gas Chromatography-Mass Spectrometry (Py-GC-MS), Fourier Transform Infrared Spectroscopy (FnR) and elemental analysis. Fungally degraded lignins displayed increased wt%N, wt%H and wt%O content and decreased wt%C content The FTIR spectrum of decayed lignin showed an increase in the relative intensity of absorption bands assigned to carbonyl and carboxyl functional groups located on the aliphatic side chain and a decrease in absorption bands assigned to aromatic skeletal vibration modes. Semiquantitative Py-GC-MS revealed an 82% decrease in lignin derived pyrolysis products upon biodegradation.more » No significant increase in pyrolysis products with an oxygenated aliphatic side chain were detected in the fungally degraded lignin however shortening of the aliphatic side chain via cleavage at the {alpha}, {beta} and {gamma} positions was observed.« less

Mechanism of Arsenic Adsorption Using Wheat Biomass -- a spectroscopic study

NASA Astrophysics Data System (ADS)

Calvo, Oscar; Manciu, Felicia; Maldonado, Josefina; Gardea-Torresdey, Jorge

2006-10-01

Arsenic is a trace element that is toxic to animals, humans included. Since the current Environmental Protection Agency guidelines regarding water quality standards indicate that arsenic concentrations in excess of 50 ppb are hazardous to welfare of humans, the search for new water remediation methods or improvements of previous methods have been a focus in environmental technology. Investigations of arsenic uptake have used wide range of sorbents including iron oxides and oxyhydroxides, for which it have been proved that arsenic shows high affinity. In this study, we used far-infrared spectroscopy to examine the arsenic reduction using biomaterials. pH dependence analysis by FTIR demonstrates the sorption of iron oxides and oxyhydroxides by the wheat biomass. The splitting of 350 cm-1 amorphous iron oxide vibrations is a direct proof of the arsenic uptake. In addition, there is evidence of sorption of arsenic at sulfhydryl group of cysteine existent in wheat.

Optimization of conditions for thermal treatment of rice bran using an accelerator including an organo-iron compound.

PubMed

Kanno, Hikari; Tachibana, Naoya; Fukushima, Masami

2011-02-01

A method for thermal conversion of raw organic waste (ROW) to a compost-like material (CLM) with higher levels of unsaturated carbohydrates, nitrogen- and oxygen-containing compounds was developed, in which rice bran and an organo-iron compound were employed as a model ROW and the accelerator, respectively. To evaluate the qualities of CLMs, organic substances of an acid insoluble fraction of alkaline extracts (AIAEs) from a CLM were structurally characterized by elemental analysis, pyrolysis-gas chromatography/mass spectrometry and FT-IR. The levels of unsaturated carbohydrates, and nitrogen- and oxygen-containing compounds in the CLM samples were increased by long-term treatment (60°C for 5 days, 170°C for 3 days). In particular, the high lipid content of the AIAEs, which was indicative of inadequate digestion of CLM components, was dramatically reduced in the presence of the accelerator. Copyright © 2010 Elsevier Ltd. All rights reserved.

Efficient catalytic system for the direct transformation of lignocellulosic biomass to furfural and 5-hydroxymethylfurfural.

PubMed

Zhang, Luxin; Xi, Guoyun; Zhang, Jiaxin; Yu, Hongbing; Wang, Xiaochang

2017-01-01

A feasible approach was developed for the co-production of 5-hydroxymethylfurfural (5-HMF) and furfural from corncob via a new porous polytriphenylamine-SO 3 H (SPTPA) solid acid catalyst in lactone solvents. XRD, SEM, XPS, N 2 adsorption-desorption, elemental analysis, TG-DTA, acid-base titration and FTIR spectroscopy techniques were used to characterize the catalyst. This study demonstrates and optimizes the catalytic performance of SPTPA and solvent selection. SPTPA was found to exhibit superior catalytic ability in γ-valerolactone (GVL). Under the optimum reaction conditions, simultaneously encouraging yields of furfural (73.9%) and 5-HMF (32.3%) were achieved at 448K. The main advantages of this process include reasonable yields of both 5-HMF and furfural in the same reaction system, practical simplicity for the raw biomass utilization, and the use of a safe and environmentally benign solvent. Copyright © 2016 Elsevier Ltd. All rights reserved.

GaN@ZIF-8: selective formation of gallium nitride quantum dots inside a zinc methylimidazolate framework.

PubMed

Esken, Daniel; Turner, Stuart; Wiktor, Christian; Kalidindi, Suresh Babu; Van Tendeloo, Gustaaf; Fischer, Roland A

2011-10-19

The microporous zeolitic imidazolate framework [Zn(MeIM)(2); ZIF-8; MeIM = imidazolate-2-methyl] was quantitatively loaded with trimethylamine gallane [(CH(3))(3)NGaH(3)]. The obtained inclusion compound [(CH(3))(3)NGaH(3)]@ZIF-8 reveals three precursor molecules per host cavity. Treatment with ammonia selectively yields the caged cyclotrigallazane intermediate (H(2)GaNH(2))(3)@ZIF-8, and further annealing gives GaN@ZIF-8. This new composite material was characterized with FT-IR spectroscopy, solid-state NMR spectroscopy, powder X-ray diffraction, elemental analysis, (scanning) transmission electron microscopy combined with electron energy-loss spectroscopy, photoluminescence (PL) spectroscopy, and N(2) sorption measurements. The data give evidence for the presence of GaN nanoparticles (1-3 nm) embedded in the cavities of ZIF-8, including a blue-shift of the PL emission band caused by the quantum size effect.

Enhancing the combustible properties of bamboo by torrefaction.

PubMed

Rousset, Patrick; Aguiar, Clarissa; Labbé, Nicole; Commandré, Jean-Michel

2011-09-01

Bamboo has wide range of moisture content, low bulk energy density and is difficult to transport, handle, store and feed into existing combustion and gasification systems. Because of its important fuel characteristics such as low ash content, alkali index and heating value, bamboo is a promising energy crop for the future. The aim of this study was to evaluate the effects of torrefaction on the main energy properties of Bambusa vulgaris. Three different torrefaction temperatures were employed: 220, 250 and 280°C. The elemental characteristics of lignite and coal were compared to the torrefied bamboo. The characteristics of the biomass fuels tend toward those of low rank coals. Principal component analysis of FTIR data showed a clear separation between the samples by thermal treatment. The loadings plot indicated that the bamboo samples underwent chemical changes related to carbonyl groups, mostly present in hemicelluloses, and to aromatic groups present in lignin. Copyright © 2011 Elsevier Ltd. All rights reserved.

Structural analysis of nanocrystalline ZnTe alloys synthesized by melt quenching technique

NASA Astrophysics Data System (ADS)

Singh, Harinder; Singh, Tejbir; Thakur, Anup; Sharma, Jeewan

2018-05-01

Nanocrystalline ZnxTe100-x (x=0, 5, 20, 30, 40, 50) alloys have been synthesized using melt quenching technique. Energy-dispersive X-Ray spectroscopy (EDS) has been used to verify the elemental composition of samples. Various absorption modes are recorded from Fourier transform infrared spectroscopy (FTIR) confirming the formation of ZnTe. The structural study has been performed using X-Ray Diffraction (XRD) method. All synthesized samples have been found to be nanocrystalline in nature with average crystallite size in the range from 49.3 nm to 77.1 nm. Results have shown that Zn0Te100 exhibits hexagonal phase that transforms into a cubic ZnTe phase as the amount of zinc is increased. Pure ZnTe phase has been obtained for x = 50. The texture coefficient (Tc) has been calculated to find the prominent orientations of different planes.

Recycling of pneumatic scrap tyre into nano-crumb rubber by pulsed laser ablation in different pH media

NASA Astrophysics Data System (ADS)

Ezaan Khamsan, Nur; Bidin, Noriah; Islam, Shumaila; Daud, Suzairi; Krishnan, Ganesan; Bakar, Mohamad Aizat A.; Naqiuddin Razali, Muhamad; Khamis, Jamil

2018-05-01

Nano crumb rubber from scrap tyre is synthesized via 1064 nm pulsed Nd:YAG laser ablation in three different pH media i.e. DI-water (pH∼6.45), D-limonene (pH∼3.47) and NaOH solution (pH∼13.41). Field Emission Scanning Electron Microscope (FESEM) results show spherical morphology of crumb rubber with high degree of aggregation in DI-water and in D-limonene. However, dispersion of crumb rubbers is observed in NaOH solution. The smallest particles size is obtained in NaOH solution within the range of 10.9 nm – 74.3 nm. Energy-dispersive X-ray spectroscopy (EDX) and FTIR analysis confirmed the elements distribution and chemical bonding of rubber with DI-water, D-limonene and NaOH solution. The experimental findings shows that pulsed Nd:YAG laser ablation has potential for fabricating nano-crumb rubber in liquid media.

Kinetic modelling for zinc (II) ions biosorption onto Luffa cylindrica

DOE Office of Scientific and Technical Information (OSTI.GOV)

Oboh, I., E-mail: innocentoboh@uniuyo.edu.ng; Aluyor, E.; Audu, T.

The biosorption of Zinc (II) ions onto a biomaterial - Luffa cylindrica has been studied. This biomaterial was characterized by elemental analysis, surface area, pore size distribution, scanning electron microscopy, and the biomaterial before and after sorption, was characterized by Fourier Transform Infra Red (FTIR) spectrometer. The kinetic nonlinear models fitted were Pseudo-first order, Pseudo-second order and Intra-particle diffusion. A comparison of non-linear regression method in selecting the kinetic model was made. Four error functions, namely coefficient of determination (R{sup 2}), hybrid fractional error function (HYBRID), average relative error (ARE), and sum of the errors squared (ERRSQ), were used tomore » predict the parameters of the kinetic models. The strength of this study is that a biomaterial with wide distribution particularly in the tropical world and which occurs as waste material could be put into effective utilization as a biosorbent to address a crucial environmental problem.« less

Cysteine-Functionalized Chitosan Magnetic Nano-Based Particles for the Recovery of Light and Heavy Rare Earth Metals: Uptake Kinetics and Sorption Isotherms

PubMed Central

Galhoum, Ahmed A.; Mafhouz, Mohammad G.; Abdel-Rehem, Sayed T.; Gomaa, Nabawia A.; Atia, Asem A.; Vincent, Thierry; Guibal, Eric

2015-01-01

Cysteine-functionalized chitosan magnetic nano-based particles were synthesized for the sorption of light and heavy rare earth (RE) metal ions (La(III), Nd(III) and Yb(III)). The structural, surface, and magnetic properties of nano-sized sorbent were investigated by elemental analysis, FTIR, XRD, TEM and VSM (vibrating sample magnetometry). Experimental data show that the pseudo second-order rate equation fits the kinetic profiles well, while sorption isotherms are described by the Langmuir model. Thermodynamic constants (ΔG°, ΔH°) demonstrate the spontaneous and endothermic nature of sorption. Yb(III) (heavy RE) was selectively sorbed while light RE metal ions La(III) and Nd(III) were concentrated/enriched in the solution. Cationic species RE(III) in aqueous solution can be adsorbed by the combination of chelating and anion-exchange mechanisms. The sorbent can be efficiently regenerated using acidified thiourea. PMID:28347004

Antimalarial, antimicrobial, cytotoxic, DNA interaction and SOD like activities of tetrahedral copper(II) complexes

NASA Astrophysics Data System (ADS)

Mehta, Jugal V.; Gajera, Sanjay B.; Patel, Mohan N.

2015-02-01

The mononuclear copper(II) complexes with P, O-donor ligand and different fluoroquinolones have been synthesized and characterized by elemental analysis, electronic spectra, TGA, EPR, FT-IR and LC-MS spectroscopy. An antimicrobial efficiency of the complexes has been tested against five different microorganisms in terms of minimum inhibitory concentration (MIC) and displays very good antimicrobial activity. The binding strength and binding mode of the complexes with Herring Sperm DNA (HS DNA) have been investigated by absorption titration and viscosity measurement studies. The studies suggest the classical intercalative mode of DNA binding. Gel electrophoresis assay determines the ability of the complexes to cleave the supercoiled form of pUC19 DNA. Synthesized complexes have been tested for their SOD mimic activity using nonenzymatic NBT/NADH/PMS system and found to have good antioxidant activity. All the complexes show good cytotoxic and in vitro antimalarial activities.

Adsorption of aluminum and lead from wastewater by chitosan-tannic acid modified biopolymers: Isotherms, kinetics, thermodynamics and process mechanism.

PubMed

Badawi, M A; Negm, N A; Abou Kana, M T H; Hefni, H H; Abdel Moneem, M M

2017-06-01

Chitosan was reacted by tannic acid to obtain three modified chitosan biopolymer. Their chemical structures were characterized by FTIR and elemental analysis. The prepared biopolymers were used to adsorb Al(III) and Pb(II) metal ions from industrial wastewater. The factors affecting the adsorption process were biosorbent amount, initial concentration of metal ion and pH of the medium. The adsorption efficiency increased considerably with the increase of the biosorbent amount and pH of the medium. The adsorption process of biosorbent on different metal ions was fitted by Freundlich adsorption model. The adsorption kinetics was followed Pseudo-second-order kinetic model. The adsorption process occurred according to diffusion mechanism which was confirmed by the interparticle diffusion model. The modified biopolymers were efficient biosorbents for removal of Pb(II) and Al(III) metal ions from the medium. Copyright © 2017 Elsevier B.V. All rights reserved.

Novel oxime based flavanone, naringin-oxime: synthesis, characterization and screening for antioxidant activity.

PubMed

Ozyürek, Mustafa; Akpınar, Damla; Bener, Mustafa; Türkkan, Baki; Güçlü, Kubilay; Apak, Reşat

2014-04-05

Recent interest in polyphenolic antioxidants due to their involvement in health benefits has led to the investigation of new polyphenolic compounds with enhanced antioxidant activity. Naringin (4',5,7-trihydroxyflavanone-7-β-l-rhamnoglucoside-(1,2)-α-d-glucopyranoside) is one of the major flavanones in citrus and grapefruit. The present study aimed to synthesize naringin oxime from naringin and to evaluate its antioxidant and anticancer potential using in vitro assay system. The structure of the synthesized compound, naringin oxime, was elucidated by FT-IR, (1)H NMR, elemental analysis and UV-vis spectroscopy. Antioxidant capacity of naringin oxime, as measured by the cupric reducing antioxidant capacity (CUPRAC) method, was found to be higher than that of the parent compound naringin. Other parameters of antioxidant activity (scavenging effects on OH, O2(-), and H2O2) of naringin and naringin oxime were also determined. Copyright © 2014 Elsevier Ireland Ltd. All rights reserved.

Kinetic modelling for zinc (II) ions biosorption onto Luffa cylindrica

NASA Astrophysics Data System (ADS)

Oboh, I.; Aluyor, E.; Audu, T.

2015-03-01

The biosorption of Zinc (II) ions onto a biomaterial - Luffa cylindrica has been studied. This biomaterial was characterized by elemental analysis, surface area, pore size distribution, scanning electron microscopy, and the biomaterial before and after sorption, was characterized by Fourier Transform Infra Red (FTIR) spectrometer. The kinetic nonlinear models fitted were Pseudo-first order, Pseudo-second order and Intra-particle diffusion. A comparison of non-linear regression method in selecting the kinetic model was made. Four error functions, namely coefficient of determination (R2), hybrid fractional error function (HYBRID), average relative error (ARE), and sum of the errors squared (ERRSQ), were used to predict the parameters of the kinetic models. The strength of this study is that a biomaterial with wide distribution particularly in the tropical world and which occurs as waste material could be put into effective utilization as a biosorbent to address a crucial environmental problem.

Surface morphology of chitin highly related with the isolated body part of butterfly (Argynnis pandora).

PubMed

Kaya, Murat; Bitim, Betül; Mujtaba, Muhammad; Koyuncu, Turgay

2015-11-01

This study was conducted to understand the differences in the physicochemical properties of chitin samples isolated from the wings and the other body parts except the wings (OBP) of a butterfly species (Argynnis pandora). The same isolation method was used for obtaining chitin specimens from both types of body parts. The chitin content of the wings (22%) was recorded as being much higher than the OBP (8%). The extracted chitin samples were characterized via FT-IR, TGA, XRD, SEM, and elemental analysis techniques. Results of these characterizations revealed that the chitins from both structures (wings and OBP) were very similar, except for their surface morphologies. SEM results demonstrated one type of surface morphology for the wings and four different surface morphologies for the OBP. Therefore, it can be hypothesized that the surface morphology of the chitin is highly related with the body part. Copyright © 2015 Elsevier B.V. All rights reserved.

Synthesis, spectroscopic characterization, DNA interaction and antibacterial study of metal complexes of tetraazamacrocyclic Schiff base

NASA Astrophysics Data System (ADS)

Shakir, Mohammad; Khanam, Sadiqa; Firdaus, Farha; Latif, Abdul; Aatif, Mohammad; Al-Resayes, Saud I.

The template condensation reaction between benzil and 3,4-diaminotoulene resulted mononuclear 12-membered tetraimine macrocyclic complexes of the type, [MLCl2] [M = Co(II), Ni(II), Cu(II) and Zn(II)]. The synthesized complexes have been characterized on the basis of the results of elemental analysis, molar conductance, magnetic susceptibility measurements and spectroscopic studies viz. FT-IR, 1H and 13C NMR, FAB mass, UV-vis and EPR. An octahedral geometry has been envisaged for all these complexes, while a distorted octahedral geometry has been noticed for Cu(II) complex. Low conductivity data of all these complexes suggest their non-ionic nature. The interactive studies of these complexes with calf thymus DNA showed that the complexes are avid binders of calf thymus DNA. The in vitro antibacterial studies of these complexes screened against pathogenic bacteria proved them as growth inhibiting agents.

Synthesis, characterization, DNA-binding study and anticancer properties of ternary metal(II) complexes of edda and an intercalating ligand.

PubMed

Ng, Chew Hee; Kong, King Chow; Von, Sze Tin; Balraj, Pauline; Jensen, Paul; Thirthagiri, Eswary; Hamada, Hirokazu; Chikira, Makoto

2008-01-28

A series of ternary metal(ii) complexes {M(phen)(edda); 1a (Cu), 1b (Co), 1c (Zn), 1d (Ni); H(2)edda = N,N(')-ethylenediaminediacetic acid} of N,N'-ethylene-bridged diglycine and 1,10-phenanthroline were synthesized and characterized by elemental analysis, FTIR, UV-visible spectroscopy and magnetic susceptibility measurement. The interaction of these complexes with DNA was investigated using CD and EPR spectroscopy. MTT assay results of 1a-1c , screened on MCF-7 cancer cell lines, show that synergy between the metal and ligands results in significant enhancement of their antiproliferative properties. Preliminary results from apoptosis and cell cycle analyses with flow cytometry are reported. seems to be able to induce cell cycle arrest at G(0)/G(1). The crystal structure of 1a is also included.

Deposition of TiOxNy Thin Films with Various Nitrogen Flow Rate:. Growth Behavior and Structural Properties

NASA Astrophysics Data System (ADS)

Cho, S.-J.; Jung, C.-K.; Bae, I.-S.; Song, Y.-H.; Boo, J.-H.

2011-06-01

We have deposited TiOxNy thin films on Si(100) substrates at 500 °C using RF PECVD system. Titanium iso-propoxide was used as precursor with different nitrogen flow rate to control oxygen and nitrogen contents in the films. Changes of chemical states of constituent elements in the deposited films were examined by XPS analysis. The data showed that with increasing nitrogen flow rate, the total amounts of nitrogen and titanium were increased while that of oxygen was decreased, resulting in a binding energy shift toward high energy side. The characteristics of film growth orientation and structure as well as morphology change behavior were also analyzed by XRD, TED, FT-IR, TEM, and SEM. Deposition at higher nitrogen flow rate results in finer clusters with a nanograin size and more effective photocatalytic TiOxNy thin films with hydrophilic surface.

One-pot microwave assisted synthesis and structural elucidation of novel ethyl 3-substituted-7-methylindolizine-1-carboxylates with larvicidal activity against Anopheles arabiensis

NASA Astrophysics Data System (ADS)

Chandrashekharappa, Sandeep; Venugopala, Katharigatta N.; Nayak, Susanta K.; Gleiser, Raquel M.; García, Daniel A.; Kumalo, Hezekiel M.; Kulkarni, Rashmi S.; Mahomoodally, Fawzi M.; Venugopala, Rashmi; Mohan, Mahendra K.; Odhav, Bharti

2018-03-01

In the present investigation a series of novel ethyl 3-substituted-7-methylindolizine-1-carboxylates was achieved by microwave assisted one-pot method. The purity of the compounds was ascertained by HPLC and structural elucidation of the title compounds was achieved by FT-IR, NMR (1H and 13C), LC-MS and elemental analysis. One randomly selected compound from the series was further studied by single crystal X-ray method for intra and intermolecular interactions. Larvicidal properties of the characterized compounds were evaluated against Anopheles arabiensis and it was found that indolizine pharmacophore influences larvicidal activity as we can see larvicidal activity for all the analogues. The synthesized analogues (2j, 2m and 2f) were the most potent compounds based on the functional groups on the indolizine pharmacophore for larvicidal assay.

Azomethine diimides end-capped with anthracene moieties: Experimental and theoretical investigations

NASA Astrophysics Data System (ADS)

Schab-Balcerzak, Ewa; Grucela, Marzena; Malecki, Grzegorz; Kotowicz, Sonia; Siwy, Mariola; Janeczek, Henryk; Golba, Sylwia; Praski, Aleksander

2017-01-01

New arylene bisimide derivatives containing imine linkages and anthracene units were synthesized. Azomethine diimides were prepared via condensation reaction of 9-anthracenecarboxaldehyde and diamines with phthalic diimide or naphthalene diimide core and Schiff base linkers. They were characterized by FTIR spectroscopy, elemental analysis and mass spectrometry (MALDI-TOF-MS). The synthesized compounds exhibited high resistance against thermal decomposition up to 400 °C. Investigated compounds are electrochemically active and undergo reversible electrochemical reduction and irreversible oxidation processes as was found in cyclic voltammetry studies. The photoluminescence measurements of synthesized compounds in solid state as thin film on glass substrate revealed their ability to emission of the blue light with quantum yield efficiency about 2%. The electronic structure and spectroscopic properties of prepared azomethine diimides were also calculated by the density functional theory (DFT). The electrical properties of the diimide derivatives were preliminary investigated by current-voltage measurements.

3-(1,3,4-Thiadiazole-2-yl)quinoline derivatives: synthesis, characterization and anti-microbial activity.

PubMed

Bhat, Abdul R; Tazeem; Azam, Amir; Choi, Inho; Athar, Fareeda

2011-07-01

A new series of thiadiazoles and intermediate thiosemicarbazones were synthesized from the chloroquinone molecule, with an aim to explore their effect on in vitro growth of microorganisms causing microbial infection. The chemical structures of the compound were elucidated by elemental analysis, FTIR, 1H and 13C NMR and ESI-MS spectral data. In vitro anti-microbial activity was performed against Staphylococcusaureus, Streptococcuspyogenes, Salmonellatyphimurium, and Escherichiacoli. The MIC was detected using the double dilution method. The results were compared by calculating percent inhibit area/μg of the compounds and the standard "amoxicillin". The selected compounds were tested for cytotoxic results using MTT assay H9c2 cardiac myoblasts cell line and the results showed that all the compounds offered remarkable >80% viability to a concentration of 200 μg/mL. Copyright © 2011 Elsevier Masson SAS. All rights reserved.

FT-IR, micro-Raman and UV-vis spectroscopic and quantum chemical investigations of free 2,2'-dithiodipyridine and its metal (Co, Cu and Zn) halide complexes.

PubMed

Gökce, Halil; Bahçeli, Semiha

2013-10-01

In this study the elemental analysis results, molecular geometries, vibrational and electronic absorption spectra of free 2,2'-dithiodipyridine(C10H8N2S2), (or DTDP) (with synonym, 2,2'-dipyridyl disulfide) and M(C10H8N2S2)Cl2 (M=Co, Cu and Zn) complexes have been reported. Vibrational wavenumbers of free DTDP and its metal halide complexes have been calculated by using DFT/B3LYP calculation method with 6-31++G(d,p) and Lanl2DZ basis sets, respectively, in the ground state, for the first time. The calculated fundamental vibrational frequencies are in a good agreement with experimental data. The HOMO, LUMO and MEP analyses of all compounds are performed by DFT method. Copyright © 2013. Published by Elsevier B.V.

In-situ preparation of functionalized molecular sieve material and a methodology to remove template.

PubMed

Yadav, Rekha; Ahmed, Maqsood; Singh, Arvind Kumar; Sakthivel, Ayyamperumal

2016-03-10

A series of diaminosilane-functionalized silicoaluminophosphate molecular sieve (SAPO-37) was prepared by in-situ synthesis, and a novel method was developed for the selective removal of structure directing agent (SDA)/template from the functionalized SAPO-37.The complete removal of the SDA was evident according to FT-IR, TGA, (13)C MAS-NMR and elemental analysis. The developed method was found to be efficient for removal of template from microporous molecular sieve viz., SAPO-37 and can be applied for other microporous molecular sieves such as SAPO-5, SAPO-40, etc. The powder XRD pattern of the template-removed samples showed a highly crystalline SAPO-37 phase. Argentometric titration revealed that more than 90% of diamine functionality exposed on the surface was accessible for catalytic applications. The resultant materials showed promising activity for ring opening of epoxide with aniline to yield β-amino-alcohol.

Stabilization of Co{sup 2+} in layered double hydroxides (LDHs) by microwave-assisted ageing

DOE Office of Scientific and Technical Information (OSTI.GOV)

Herrero, M.; Benito, P.; Labajos, F.M.

2007-03-15

Co-containing layered double hydroxides at different pH have been prepared, and aged following different routes. The solids prepared have been characterized by element chemical analysis, powder X-ray diffraction, thermogravimetric and differential thermal analyses (both in nitrogen and in oxygen), FT-IR and Vis-UV spectroscopies, temperature-programmed reduction and surface area assessment by nitrogen adsorption at -196 deg. C. The best conditions found to preserve the cobalt species in the divalent oxidation state are preparing the samples at controlled pH, and then submit them to ageing under microwave irradiation. - Graphical abstract: The use of microwave-hydrothermal treatment, controlling both temperature and ageing time,more » permits to synthesize well-crystallized nanomaterials with controlled surface properties. An enhancement in the crystallinity degree and an increase in the particle size are observed when the irradiation time is prolonged.« less

Synthesis and characterization of dithiocarbamate chitosan derivatives with enhanced antifungal activity.

PubMed

Qin, Yukun; Liu, Song; Xing, Ronge; Yu, Huahua; Li, Kecheng; Meng, Xiangtao; Li, Rongfeng; Li, Pengcheng

2012-06-20

In this study, ammonium dithiocarbamate chitosan (ADTCCS) and triethylene diamine dithiocarbamate chitosan (TEDADTCCS) derivatives were obtained respectively by mixing chitosan with carbon disulfide and ammonia (triethylenediamine). Their structures were confirmed by FT-IR, 1H NMR, XRD, DSC, SEM, and elemental analysis. Antifungal properties of them against the plant pathogenic fungi Fusarium oxysporum and Alternaria porri were investigated at concentrations ranged from 31.25 to 500 mg/L. The dithiocarbamate chitosan derivatives had enhanced antifungal activity compared with chitosan. Particularly, they showed obvious inhibitory effect on Fusarium oxysporum. At 500 mg/L, TEDADTCCS inhibited growth of F. oxysporum at 60.4%, stronger than polyoxin and triadimefon whose antifungal indexes were found to be 25.3% and 37.7%. The chitosan derivatives described here deserve further study for use in crop protection. Crown Copyright © 2012. Published by Elsevier Ltd. All rights reserved.

Amination of black liquor and the application in the ready-mixed wet mortar.

PubMed

Zheng, Dafeng; Zheng, Tao; Chen, Ran; Li, Xiaokang; Qiu, Xueqing

2018-01-01

In order to extend the application of black liquor (BL), amino group was introduced in lignin through Mannich reaction. The structure of the aminated black liquor (ABL) was characterized with FT-IR, elemental analysis, the zeta potential and the inherent viscosity. The foam generated by ABL was more stable, for the surface tension was lower. The results of the mortar test indicated that the water-retention rate of the fresh mortar incorporated with 0.3 wt% ABL was 89.1%; the consistency loss was about 39.7% after 4 h. When the dosage was less than 0.3 wt%, ABL could increase the bond strength of the hardened mortars. The results showed that ABL could be used as an effective ready-mixed wet mortar admixture. This study not only provided a new method to develop new mortar admixture, but also alleviated the pollution of BL.

The employment of FTIR spectroscopy in combination with chemometrics for analysis of rat meat in meatball formulation.

PubMed

Rahmania, Halida; Sudjadi; Rohman, Abdul

2015-02-01

For Indonesian community, meatball is one of the favorite meat food products. In order to gain economical benefits, the substitution of beef meat with rat meat can happen due to the different prices between rat meat and beef. In this present research, the feasibility of FTIR spectroscopy in combination with multivariate calibration of partial least square (PLS) was used for the quantitative analysis of rat meat in the binary mixture of beef in meatball formulation. Meanwhile, the chemometrics of principal component analysis (PCA) was used for the classification between rat meat and beef meatballs. Some frequency regions in mid infrared region were optimized, and finally, the frequency region of 750-1000 cm(-1) was selected during PLS and PCA modeling.For quantitative analysis, the relationship between actual values (x-axis) and FTIR predicted values (y-axis) of rat meat is described by the equation of y= 0.9417x+ 2.8410 with coefficient of determination (R2) of 0.993, and root mean square error of calibration (RMSEC) of 1.79%. Furthermore, PCA was successfully used for the classification of rat meat meatball and beef meatball.

FIM, a Novel FTIR-Based Imaging Method for High Throughput Locomotion Analysis

PubMed Central

Otto, Nils; Löpmeier, Tim; Valkov, Dimitar; Jiang, Xiaoyi; Klämbt, Christian

2013-01-01

We designed a novel imaging technique based on frustrated total internal reflection (FTIR) to obtain high resolution and high contrast movies. This FTIR-based Imaging Method (FIM) is suitable for a wide range of biological applications and a wide range of organisms. It operates at all wavelengths permitting the in vivo detection of fluorescent proteins. To demonstrate the benefits of FIM, we analyzed large groups of crawling Drosophila larvae. The number of analyzable locomotion tracks was increased by implementing a new software module capable of preserving larval identity during most collision events. This module is integrated in our new tracking program named FIMTrack which subsequently extracts a number of features required for the analysis of complex locomotion phenotypes. FIM enables high throughput screening for even subtle behavioral phenotypes. We tested this newly developed setup by analyzing locomotion deficits caused by the glial knockdown of several genes. Suppression of kinesin heavy chain (khc) or rab30 function led to contraction pattern or head sweeping defects, which escaped in previous analysis. Thus, FIM permits forward genetic screens aimed to unravel the neural basis of behavior. PMID:23349775

[Identification of different Citrus sinensis (L.) Osbeck trees varieties using Fourier transform infrared spectroscopy and hierarchical cluster analysis].

PubMed

Yi, Shi-Lai; Deng, Lie; He, Shao-Lan; Shi, You-Ming; Zheng, Yong-Qiang; Lu, Qiang; Xie, Rang-Jin; Wei, Xian-Guoi; Li, Song-Wei; Jian, Shui-Xian

2012-11-01

Researched on diversity of the spring leaf samples of seven different Citrus sinensis (L.) Osbeck varieties by Fourier transform infrared (FTIR) spectroscopy technology, the results showed that the Fourier transform infrared spectra of seven varieties leaves was composited by the absorption band of cellulose and polysaccharide mainly, the wave number of characteristics absorption peaks were similar at their FTIR spectra. However, there were some differences in shape of peaks and relatively absorption intensity. The conspicuous difference was presented at the region between 1 500 and 700 cm(-1) by second derivative spectra. Through the hierarchical cluster analysis (HCA) of second derivative spectra between 1 500 and 700 cm(-1), the results showed that the clustering of the different varieties of Citrus sinensis (L.) Osbeck varieties was classification according to genetic relationship. The results showed that FTIR spectroscopy combined with hierarchical cluster analysis could be used to identify and classify of citrus varieties rapidly, it was an extension method to study on early leaves of varieties orange seedlings.

Radiation grafting of various water-soluble monomers on ultra-high molecular weight polyethylene powder. Part II: Thermal, FTIR and morphological characterisation

NASA Astrophysics Data System (ADS)

Aydınlı, Bahattin; Tin c̡er, Teoman

2001-10-01

Radiation induced grafted polyacrylic acid (PAA), polymethacrylic acid (PMAA), polyacrylamide (PAAm), poly N,N-dimethyl acrylamide (PNDAAm) and poly 1-vinyl-2 pyrrolidone (PVP) on ultra-high molecular weight polyethylene (UHMWPE) were characterised by DSC, FTIR and SEM analysis. While the effect of irradiation on pure UHMWPE was found to increase crystallinity and cause higher enthalpy of crystallisation, grafted UHMWPE powders showed lower crystallinity and enthalpy of crystallisation. In all grafted UHMWPE there existed secondary transitions corresponding to grafting polymers in the first run of DSC above 60°C and they became clearer at a higher grafting level. In the second run of DSC some Tg values appeared to shift to higher temperatures while some were not detected. FTIR analysis indicated the presence of water-soluble polymers in the grafted UHMWPE. The characteristic peaks of water-soluble polymers became sharper in the grafted UHMWPE. SEM analysis revealed that the grafting occurs both on fiber and microparticles of UHMWPE while flowing characteristic of powder is retained.

Novel nanohybrids of cobalt(III) Schiff base complexes and clay: synthesis and structural determinations.

PubMed

Kianfar, Ali Hossein; Mahmood, Wan Ahmad Kamil; Dinari, Mohammad; Azarian, Mohammad Hossein; Khafri, Fatemeh Zare

2014-06-05

The [Co(Me(2)Salen)(PBu(3))(OH(2))]BF4 and [Co(Me(2)Salen)(PPh(3))(Solv)]BF(4), complexes were synthesized and characterized by FT-IR, UV-Vis, (1)H NMR spectroscopy and elemental analysis techniques. The coordination geometry of [Co(Me(2)Salen)(PPh(3))(H(2)O)]BF(4) was determined by X-ray crystallography. It has been found that the complex is containing [Co(Me(2)Salen)(PPh(3))(H(2)O)]BF(4) and [Co(Me(2)Salen)(PPh(3))(EtOH)]BF(4) hexacoordinate species in the solid state. Cobalt atom exhibits a distorted octahedral geometry and the Me(2)Salen ligand has the N2O2 coordinated environment in the equatorial plane. The [Co(Me(2)Salen)(PPh(3))(H(2)O)]BF(4) complex shows a dimeric structure via hydrogen bonding between the phenolate oxygen and hydrogens of coordinated H2O molecule. These complexes were incorporated into Montmorillonite-K10 nanoclay. The modified clays were identified by FT-IR, XRD, EDX, TGA/DTA, SEM and TEM techniques. According to the XRD results of the new nanohybrid materials, the Schiff base complexes are intercalated in the interlayer spaces of the clay. SEM and TEM micrographs show that the resulting hybrid nanomaterials have layer structures. Also, TGA/DTG results show that the intercalation reaction was taken place successfully. Copyright © 2014. Published by Elsevier B.V.

Ligand-tailored single-site silica supported titanium catalysts: Synthesis, characterization and towards cyanosilylation reaction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Xu, Wei; Li, Yani; Yu, Bo

2015-01-15

A successive anchoring of Ti(NMe{sub 2}){sub 4}, cyclopentadiene and a O-donor ligand, 1-hydroxyethylbenzene (PEA), 1,1′-bi-2-naphthol (Binol) or 2,3-dihydroxybutanedioic acid diethyl ester (Tartrate), on silica was conducted by SOMC strategy in moderate conditions. The silica, monitored by in-situ Fourier transform infrared spectroscopy (in-situ FT-IR), was pretreated at different temperatures (200, 500 and 800 °C). The ligand tailored silica-supported titanium complexes were characterized by in-situ FT-IR, {sup 13}C CP MAS-NMR, X-ray photoelectron spectroscopy (XPS), X-ray absorption near edge structure (XANES) and elemental analysis in detail, verifying that the surface titanium species are single sited. The catalytic activity of the ligand tailored single-sitemore » silica supported titanium complexes was evaluated by a cyanosilylation of benzaldehyde. The results showed that the catalytic activity is dependent strongly on the dehydroxylation temperatures of silica and the configuration of the ligands. - Graphical abstract: The ligand-tailored silica supported “single site” titanium complexes were synthesized by SOMC strategy and fully characterized. Their catalytic activity were evaluated by benzaldehyde silylcyanation. - Highlights: • Single-site silica supported Ti active species was prepared by SOMC technique. • O-donor ligand tailored Ti surface species was synthesized. • The surface species was characterized by XPS, {sup 13}C CP-MAS NMR, XANES etc. • Catalytic activity of the Ti active species in silylcyanation reaction was evaluated.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kaus, Noor Haida Mohd., E-mail: noorhaida@usm.my; Collins, A. M.; Mann, S.

In this paper, we present a facile method for production stable aqueous dispersion of ferrocene (FO) nanoparticles. Ferrocene compounds were employed to achieve stable nanodispersions, stabilized with three different biopolymers namely, alginate, CM-dextran and chitosan. The nanoparticles produce are spherical, less than 10 nm in mean diameter and highly stable without any sedimentation. Fourier infrared transform (FTIR) and X-ray diffraction (XRD) studies confirmed the purity of ferrocene nanoparticles there is no modifications occur during the preparation route. FTIR spectra results were consistent with the presence of absorption band of cyclopentadienyl ring (C{sub 5}H{sub 5}{sup −} ion) which assigned to ν(C-C)more » vibrations (1409 cm-1), δ(C-H) stretching at 1001 cm{sup −1} and π(C-H) vibrations at 812 cm{sup −1}. Furthermore, all functional group for biopolymers such as CO from carboxyl group of CM-dextran and sodium alginate appears at 1712 cm{sup −1} and 1709 cm{sup −1} respectively, indicating there are steric repulsion interactions for particles stabilization. Powder X-ray diffraction patterns of sedimented samples of the biopolymers-stabilized ferrocene (FO) showed all reflections which were indexed respectively to the (−110), (001), (−201), (−111), (200), (−211), (210), (120) and (111) according to the monoclinic phase ferrocene. This confirmed that the products obtained were of high purity of Fe and EDAX analysis also suggests that the presence of the Fe element in the colloidal dispersion.« less

Synthesis and characterization of high quantum yield and oscillator strength 6-chloro-2-(4-cynophenyl)-4-phenyl quinoline (cl-CN-DPQ) organic phosphor for solid-state lighting.

PubMed

Ghate, Minakshi; Dahule, H K; Thejo Kalyani, N; Dhoble, S J

2018-03-01

A novel blue luminescent 6-chloro-2-(4-cynophenyl) substituted diphenyl quinoline (Cl-CN DPQ) organic phosphor has been synthesized by the acid-catalyzed Friedlander reaction and then characterized to confirm structural, optical and thermal properties. Structural properties of Cl-CN-DPQ were analyzed by Fourier transform infrared (FTIR), nuclear magnetic resonance (NMR) spectroscopy, X-ray diffraction technique (XRD) and scanning electron microscopy (SEM) and energy dispersive analysis of X-ray (EDAX) spectroscopy. FTIR spectra confirmed the presence of different functional groups and bond stretching. 1 H-NMR and 13 C-NMR confirmed the formation of an organic Cl-CN-DPQ compound. X-ray diffraction study provided its crystalline nature. The surface morphology of Cl-CN-DPQ was analyzed by SEM, while EDAX spectroscopy revealed the elemental analysis. Differential thermal analysis (TGA/DTA) disclosed its thermal stability up to 250°C. The optical properties of Cl-CN-DPQ were investigated by UV-vis absorption and photoluminescence (PL) measurements. Cl-CN-DPQ exhibits intense blue emission at 434 nm in a solid-state crystalline powder with CIE co-ordinates (0.157, 0.027), when excited at 373 nm. Cl-CN-DPQ shows remarkable Stokes shift in the range 14800-5100 cm -1 , which is the characteristic feature of intense light emission. A narrow full width at half-maximum (FWHM) value of PL spectra in the range 42-48 nm was observed. Oscillator strength, energy band gap, quantum yield, and fluorescence energy yield were also examined using UV-vis absorption and photoluminescence spectra. These results prove its applications towards developing organic luminescence devices and displays, organic phosphor-based solar cells and displays, organic lasers, chemical sensors and many more. Copyright © 2017 John Wiley & Sons, Ltd.

IRIS: A database application system for diseases identification using FTIR spectroscopy

NASA Astrophysics Data System (ADS)

Arshad, Ahmad Zulhilmi; Munajat, Yusof; Ibrahim, Raja Kamarulzaman Raja; Mahmood, Nasrul Humaimi

2015-05-01

Infrared information on diseases identification system (IRIS) is an application for diseases identification and analysis by using Fourier transform infrared (FTIR) spectroscopy. This is the preliminary step to gather information from the secondary data which was extracted from recognized various research and scientific paper, which are combined into a single database as in IRIS for our purpose of study. The importance of this database is to examine the fingerprint differences between normal and diseases cell or tissue. With the implementation of this application is it hopes that the diseases identification using FTIR spectroscopy would be more reliable and may assist either physicians, pathologists, or researchers to diagnose the certain type of disease efficiently.

Wintertime Experimental investigation of Morphology, Mixing States and Columnar Optical Properties of Aerosols over a Desert location in India

NASA Astrophysics Data System (ADS)

Mishra, S.; Kumar, T.; Sharma, C.; Prasad, M. V. S. N.; Singh, S.; Agnihotri, R.; Arya, B. C.; Gupta, B.; Naaraayanan, T.; Gautam, S.; Kumar, D.; Sood, K. N.; Tawale, J. S.; Sharma, A. K.; Mitra, A. K.

2014-12-01

Indian Desert (The Thar Desert) is considered as the source of mineral dust in the Indo-Gangetic Plain (IGP) especially in pre-monsoon period due to large scale convective activities during hot summer. To study the physico-chemical characteristics of aerosols over the Thar Desert (Jaisalmer, Rajasthan) during winter (December, 2013), a field campaign has been carried out in Jaisalmer in Rajasthan state. Experiments were conducted inside the city as well as far from the city. The faraway location is close to international border of another country i.e. Pakistan. PM2.5 and PM10 were collected within the city while PM5 was collected far from the city. Particles were collected on Teflon filters for bulk analysis with Fourier Transform Infrared Spectroscopy (FTIR), on Tin substrate for individual particle morphology and elemental composition analysis with Scanning Electron Microscope (SEM) equipped with Energy Dispersive Spectrometer (EDS) and on the Cu-TEM grid for individual particle morphology and mixing state characterization using High Resolution-Transmission Electron Microscope (HRTEM). Together with this, aerosol size distribution observation and columnar spectral aerosol optical properties have been carried out with OPC (Optical Particle Counter, GRIMM Model 1.108) and hand held Microtops-II, respectively. HRTEM analysis reveals occurrence of carbonaceous fractals found in various mixing states 1) aged with some hygroscopic species 2) embedded in sulfate host 3) semi-externally mixed with sulfate and other species. Core-shell particles were also observed with varying core composition (carbon, typical mineral dust, and calcite) and shell thickness (shell comprising of water). The back trajectory analysis reveals the source of wind from Karachi and Islamabad from Pakistan which may be the potential source of carbonaceous species over the sampling site. SEM-EDS analysis reveals occurrence of mineral dust 1) pure mineral dust (Ca and Si rich) 2) polluted mineral dust (mixed with carbon and Cr) together with some pollutants (rich in carbon, S, K, Cl, Mo and Nb). Signatures of various organics were traced using FTIR. Aerosol columnar spectral optical properties, size distribution and meteorology in tandem with aforementioned aerosol properties will be discussed in detail during the presentation.

Supervision of Ethylene Propylene Diene M-Class (EPDM) Rubber Vulcanization and Recovery Processes Using Attenuated Total Reflection Fourier Transform Infrared (ATR FT-IR) Spectroscopy and Multivariate Analysis.

PubMed

Riba Ruiz, Jordi-Roger; Canals, Trini; Cantero, Rosa

2017-01-01

Ethylene propylene diene monomer (EPDM) rubber is widely used in a diverse type of applications, such as the automotive, industrial and construction sectors among others. Due to its appealing features, the consumption of vulcanized EPDM rubber is growing significantly. However, environmental issues are forcing the application of devulcanization processes to facilitate recovery, which has led rubber manufacturers to implement strict quality controls. Consequently, it is important to develop methods for supervising the vulcanizing and recovery processes of such products. This paper deals with the supervision process of EPDM compounds by means of Fourier transform mid-infrared (FT-IR) spectroscopy and suitable multivariate statistical methods. An expedited and nondestructive classification approach was applied to a sufficient number of EPDM samples with different applied processes, that is, with and without application of vulcanizing agents, vulcanized samples, and microwave treated samples. First the FT-IR spectra of the samples is acquired and next it is processed by applying suitable feature extraction methods, i.e., principal component analysis and canonical variate analysis to obtain the latent variables to be used for classifying test EPDM samples. Finally, the k nearest neighbor algorithm was used in the classification stage. Experimental results prove the accuracy of the proposed method and the potential of FT-IR spectroscopy in this area, since the classification accuracy can be as high as 100%.

Optical diagnosis of actinic cheilitis by infrared spectroscopy.

PubMed

das Chagas E Silva de Carvalho, Luis Felipe; Pereira, Thiago Martini; Magrini, Taciana Depra; Cavalcante, Ana Sueli Rodrigues; da Silva Martinho, Herculano; Almeida, Janete Dias

2016-12-01

Actinic cheilitis (AC) is considered a potentially malignant disorder of the lip. Biomolecular markers study is important to understand malignant transformation into squamous cell carcinoma. Fourier transform infra red (FT-IR) spectroscopy was used to analyze AC in this study. The aim of the study was to evaluate if FT-IR spectral regions of nucleic acids and collagen can help in early diagnosis of malignant transformation. Tissues biopsies of 14 patients diagnosed with AC and 14 normal tissues were obtained. FT-IR spectra were measured at five different points resulting in 70 spectra of each. Analysis of Principal components analysis (PCA) and linear discrimination analysis (LDA) model were also used. In order to verify the statistical difference in the spectra, Mann-Whitney U test was performed in each variable (wavenumber) with p-value <0.05. After the Mann-Whitney U test the vibrational modes of CO (Collagen 1), PO2 (Nucleic Acids) and CO asymmetric (Triglycerides/Lipids) were observed as a possible spectral biomarker. These bands were chosen because they represent the vibrational modes related to collagen and DNA, which are supposed to be changed in AC samples. Based on the PCA-LDA results, the predictive model corresponding to the area under the curve was 0.91 for the fingerprint region and 0.83 for the high wavenumber region, showing the greater accuracy of the test. FT-IR changes in collagen and nucleic acids could be used as molecular biomarkers for malignant transformation. Copyright © 2016 Elsevier B.V. All rights reserved.

The pituitary gland under infrared light - in search of a representative spectrum for homogeneous regions.

PubMed

Banas, A; Banas, K; Furgal-Borzych, A; Kwiatek, W M; Pawlicki, B; Breese, M B H

2015-04-07

The pituitary gland is a small but vital organ in the human body. It is located at the base of the brain and is often described as the master gland due to its multiple functions. The pituitary gland secretes and stores hormones, such as the thyroid-stimulating hormone (TSH), adrenocorticotropic hormone (ACTH), growth hormone (hGH), prolactin, gonadotropins, and luteinizing hormones, as well as the antidiuretic hormone (ADH). A proper diagnosis of pituitary disorders is of utmost importance as this organ participates in regulating a variety of body functions. Typical histopathological analysis provides much valuable information, but it gives no insight into the biochemical background of the changes that occur within the gland. One approach that could be used to evaluate the biochemistry of tissue sections obtained from pituitary disorders is Fourier Transform Infra-Red (FTIR) spectromicroscopy. In order to collect diagnostically valuable information large areas of tissue must be investigated. This work focuses on obtaining a unique and representative FTIR spectrum characteristic of one type of cell architecture within a sample. The idea presented is based on using hierarchical cluster analysis (HCA) for data evaluation to search for uniform patterns within samples from the perspective of FTIR spectra. The results obtained demonstrate that FTIR spectromicroscopy, combined with proper statistical evaluation, can be treated as a complementary method for histopathological analysis and ipso facto can increase the sensitivity and specificity for detecting various disorders not only for the pituitary gland, but also for other human tissues.

Assignment of far-infrared laser lines of O-17 methanol by synchrotron FTIR spectroscopy and laser frequency measurements

NASA Astrophysics Data System (ADS)

Lees, R. M.; Jackson, M.; Moruzzi, G.; Predoi-Cross, Adriana; Billinghurst, B. E.

2015-09-01

Analysis of synchrotron FTIR spectra has revealed new assignments for a number of optically pumped far-infrared laser lines from the CH317OH isotopologue of methanol, with definitive confirmation provided by recent accurate measurements of the laser frequencies. In this Note the lasing energy level systems are discussed, and the spectroscopic evidence for the assignments is presented.

Rapid authentication of edible bird's nest by FTIR spectroscopy combined with chemometrics.

PubMed

Guo, Lili; Wu, Yajun; Liu, Mingchang; Ge, Yiqiang; Chen, Ying

2018-06-01

Edible bird's nests (EBNs) have been traditionally regarded as a kind of medicinal and healthy food in China. For economic reasons, they are frequently subjected to adulteration with some cheaper substitutes, such as Tremella fungus, agar, fried pigskin, and egg white. As a kind of precious and functional product, it is necessary to establish a robust method for the rapid authentication of EBNs with small amounts of samples by simple processes. In this study, the Fourier transform infrared spectroscopy (FTIR) system was utilized and its feasibility for identification of EBNs was verified. FTIR spectra data of authentic and adulterated EBNs were analyzed by chemometrics analyses including principal component analysis, linear discriminant analysis (LDA), support vector machine (SVM) and one-class partial least squares (OCPLS). The results showed that the established LDA and SVM models performed well and had satisfactory classification ability, with the former 94.12% and the latter 100%. The OCPLS model was developed with prediction sensitivity of 0.937 and specificity of 0.886. Further detection of commercial EBN samples confirmed these results. FTIR is applicable in the scene of rapid authentication of EBNs, especially for quality supervision departments, entry-exit inspection and quarantine, and customs administration. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

Diagnosis of Cell Death by Means of Infrared Spectroscopy

PubMed Central

Zelig, Udi; Kapelushnik, Joseph; Moreh, Raymond; Mordechai, Shaul; Nathan, Ilana

2009-01-01

Abstract Fourier transform infrared (FTIR) spectroscopy has been established as a fast spectroscopic method for biochemical analysis of cells and tissues. In this research we aimed to investigate FTIR's utility for identifying and characterizing different modes of cell death, using leukemic cell lines as a model system. CCRF-CEM and U937 leukemia cells were treated with arabinoside and doxorubicin apoptosis inducers, as well as with potassium cyanide, saponin, freezing-thawing, and H2O2 necrosis inducers. Cell death mode was determined by various gold standard biochemical methods in parallel with FTIR-microscope measurements. Both cell death modes exhibit large spectral changes in lipid absorbance during apoptosis and necrosis; however, these changes are similar and thus cannot be used to distinguish apoptosis from necrosis. In contrast to the above confounding factor, our results reveal that apoptosis and necrosis can still be distinguished by the degree of DNA opaqueness to infrared light. Moreover, these two cell death modes also can be differentiated by their infrared absorbance, which relates to the secondary structure of total cellular protein. In light of these findings, we conclude that, because of its capacity to monitor multiple biomolecular parameters, FTIR spectroscopy enables unambiguous and easy analysis of cell death modes and may be useful for biochemical and medical applications. PMID:19804743

A Hybrid Sensing Approach for Pure and Adulterated Honey Classification

PubMed Central

Subari, Norazian; Saleh, Junita Mohamad; Shakaff, Ali Yeon Md; Zakaria, Ammar

2012-01-01

This paper presents a comparison between data from single modality and fusion methods to classify Tualang honey as pure or adulterated using Linear Discriminant Analysis (LDA) and Principal Component Analysis (PCA) statistical classification approaches. Ten different brands of certified pure Tualang honey were obtained throughout peninsular Malaysia and Sumatera, Indonesia. Various concentrations of two types of sugar solution (beet and cane sugar) were used in this investigation to create honey samples of 20%, 40%, 60% and 80% adulteration concentrations. Honey data extracted from an electronic nose (e-nose) and Fourier Transform Infrared Spectroscopy (FTIR) were gathered, analyzed and compared based on fusion methods. Visual observation of classification plots revealed that the PCA approach able to distinct pure and adulterated honey samples better than the LDA technique. Overall, the validated classification results based on FTIR data (88.0%) gave higher classification accuracy than e-nose data (76.5%) using the LDA technique. Honey classification based on normalized low-level and intermediate-level FTIR and e-nose fusion data scored classification accuracies of 92.2% and 88.7%, respectively using the Stepwise LDA method. The results suggested that pure and adulterated honey samples were better classified using FTIR and e-nose fusion data than single modality data. PMID:23202033

Fourier-transform infrared spectroscopy as a novel approach to providing effect-based endpoints in duckweed toxicity testing.

PubMed

Hu, Li-Xin; Ying, Guang-Guo; Chen, Xiao-Wen; Huang, Guo-Yong; Liu, You-Sheng; Jiang, Yu-Xia; Pan, Chang-Gui; Tian, Fei; Martin, Francis L

2017-02-01

Traditional duckweed toxicity tests only measure plant growth inhibition as an endpoint, with limited effects-based data. The present study aimed to investigate whether Fourier-transform infrared (FTIR) spectroscopy could enhance the duckweed (Lemna minor L.) toxicity test. Four chemicals (Cu, Cd, atrazine, and acetochlor) and 4 metal-containing industrial wastewater samples were tested. After exposure of duckweed to the chemicals, standard toxicity endpoints (frond number and chlorophyll content) were determined; the fronds were also interrogated using FTIR spectroscopy under optimized test conditions. Biochemical alterations associated with each treatment were assessed and further analyzed by multivariate analysis. The results showed that comparable x% of effective concentration (ECx) values could be achieved based on FTIR spectroscopy in comparison with those based on traditional toxicity endpoints. Biochemical alterations associated with different doses of toxicant were mainly attributed to lipid, protein, nucleic acid, and carbohydrate structural changes, which helped to explain toxic mechanisms. With the help of multivariate analysis, separation of clusters related to different exposure doses could be achieved. The present study is the first to show successful application of FTIR spectroscopy in standard duckweed toxicity tests with biochemical alterations as new endpoints. Environ Toxicol Chem 2017;36:346-353. © 2016 SETAC. © 2016 SETAC.

Study on Senna alata and its different extracts by Fourier transform infrared spectroscopy and two-dimensional correlation infrared spectroscopy

NASA Astrophysics Data System (ADS)

Adiana, M. A.; Mazura, M. P.

2011-04-01

Senna alata L. commonly known as candle bush belongs to the family of Fabaceae and the plant has been reported to possess anti-inflammatory, analgesic, laxative and antiplatelet-aggregating activity. In order to develop a rapid and effective analysis method for studying integrally the main constituents in the medicinal materials and their extracts, discriminating the extracts from different extraction process, comparing the categories of chemical constituents in the different extracts and monitoring the qualities of medicinal materials, we applied Fourier transform infrared spectroscopy (FT-IR) associated with second derivative infrared spectroscopy and two-dimensional infrared correlation spectroscopy (2D-IR) to study the main constituents of S. alata and its different extracts (extracted by hexane, dichloromethane, ethyl acetate and methanol in turn). The findings indicated that FT-IR and 2D-IR can provide many holistic variation rules of chemical constituents. Use of the macroscopical fingerprint characters of FT-IR and 2D-IR spectrum can identify the main chemical constituents in medicinal materials and their extracts, but also compare the components differences among similar samples. In a conclusion, FT-IR spectroscopy combined with 2D correlation analysis provides a powerful method for the quality control of traditional medicines.

Proteolytically-induced changes of secondary structural protein conformation of bovine serum albumin monitored by Fourier transform infrared (FT-IR) and UV-circular dichroism spectroscopy

NASA Astrophysics Data System (ADS)

Güler, Günnur; Vorob'ev, Mikhail M.; Vogel, Vitali; Mäntele, Werner

2016-05-01

Enzymatically-induced degradation of bovine serum albumin (BSA) by serine proteases (trypsin and α-chymotrypsin) in various concentrations was monitored by means of Fourier transform infrared (FT-IR) and ultraviolet circular dichroism (UV-CD) spectroscopy. In this study, the applicability of both spectroscopies to monitor the proteolysis process in real time has been proven, by tracking the spectral changes together with secondary structure analysis of BSA as proteolysis proceeds. On the basis of the FTIR spectra and the changes in the amide I band region, we suggest the progression of proteolysis process via conversion of α-helices (1654 cm- 1) into unordered structures and an increase in the concentration of free carboxylates (absorption of 1593 and 1402 cm- 1). For the first time, the correlation between the degree of hydrolysis and the concentration of carboxylic groups measured by FTIR spectroscopy was revealed as well. The far UV-CD spectra together with their secondary structure analysis suggest that the α-helical content decreases concomitant with an increase in the unordered structure. Both spectroscopic techniques also demonstrate that there are similar but less spectral changes of BSA for the trypsin attack than for α-chymotrypsin although the substrate/enzyme ratio is taken the same.

Organic Matter Detection on Mars by Pyrolysis-FTIR: An Analysis of Sensitivity and Mineral Matrix Effects

NASA Astrophysics Data System (ADS)

Gordon, Peter R.; Sephton, Mark A.

2016-11-01

Returning samples from Mars will require an effective method to assess and select the highest-priority geological materials. The ideal instrument for sample triage would be simple in operation, limited in its demand for resources, and rich in produced diagnostic information. Pyrolysis-Fourier infrared spectroscopy (pyrolysis-FTIR) is a potentially attractive triage instrument that considers both the past habitability of the sample depositional environment and the presence of organic matter that may reflect actual habitation. An important consideration for triage protocols is the sensitivity of the instrumental method. Experimental data indicate pyrolysis-FTIR sensitivities for organic matter at the tens of parts per million level. The mineral matrix in which the organic matter is hosted also has an influence on organic detection. To provide an insight into matrix effects, we mixed well-characterized organic matter with a variety of dry minerals, to represent the various inorganic matrices of Mars samples, prior to analysis. During pyrolysis-FTIR, serpentinites analogous to those on Mars indicative of the Phyllocian Era led to no negative effects on organic matter detection; sulfates analogous to those of the Theiikian Era led, in some instances, to the combustion of organic matter; and palagonites, which may represent samples from the Siderikian Era, led, in some instances, to the chlorination of organic matter. Any negative consequences brought about by these mineral effects can be mitigated by the correct choice of thermal extraction temperature. Our results offer an improved understanding of how pyrolysis-FTIR can perform during sample triage on Mars.

Organic geochemistry of resins from modern Agathis australis and Eocene resins from New Zealand: Diagenetic and taxonomic implications

USGS Publications Warehouse

Lyons, P.C.; Mastalerz, Maria; Orem, W.H.

2009-01-01

A maturation series of resins and fossil resins from New Zealand, ranging in age from Modern to Eocene and ranging from uncoalified to high volatile C bituminous coal, were analyzed by elemental, pyrolysis-gas chromatography (Py-GC), Fourier Transform infrared (FTir), and solid-state 13C nuclear magnetic resonance (13C NMR) techniques. For comparison, four resin samples from the Latrobe Valley, Australia, were analyzed. All of the resins and fossil resins of this study show very high H/C atomic ratios, and are characterized by dominant peaks in the 10-60??ppm range of solid-state 13C NMR spectra and prominent bands in the aliphatic stretching region (2800-3000??cm- 1) of FTir spectra, all indicating a highly aliphatic molecular structure. The 13C NMR and FTir data indicate a diterpenoid structure for these resins. There is an abrupt loss of oxygen that occurs at the Lignite A/Subbituminous C stage, which is attributed to a dramatic loss of carboxyl (COOH) from the diterpenoid molecule. This is a new finding in the diagenesis of resins. This important loss in oxygenated functional groups is attributed to a maturation change. Also, there is a progressive loss of exomethylene (CH2) groups with increasing degree of maturation, as shown by both 13C NMR and FTir data. This change has been noted by previous investigators. Exomethylene is absent in the fossil resins from the Eocene high volatile C bituminous coals. This progressive loss is characteristic of Class I resinites. FTir data indicate that the oxygenated functional groups are strong in all the resin samples except the fossil resin from high volatile C bituminous coal. This important change in oxygenated functional groups is attributed to maturation changes. The 13C NMR and FTir data indicate there are minor changes in the Agathis australis resin from the living tree and soil, which suggests that alteration of A. australis resins begins shortly after deposition in the soil for as little as 1000??years. The Morwell and Yallourn fossil resins from brown coal (lignite B) Australia do not have some of the FTir characteristics of the New Zealand resins, which most likely indicates they have a different plant source because different degrees of oxidation and weathering and changes due to fires (i.e., charring) can be ruled out. Our results have implications for studies of the maturation, provenance, and botanical sources of fossil resins and resinites in Eocene and Miocene coals and sediments of New Zealand and Australia. ?? 2009 Elsevier B.V. All rights reserved.

Serum-based diagnostic prediction of oral submucous fibrosis using FTIR spectrometry

NASA Astrophysics Data System (ADS)

Rai, Vertika; Mukherjee, Rashmi; Routray, Aurobinda; Ghosh, Ananta Kumar; Roy, Seema; Ghosh, Barnali Paul; Mandal, Puspendu Bikash; Bose, Surajit; Chakraborty, Chandan

2018-01-01

Oral submucous fibrosis (OSF) is found to have the highest malignant potentiality among all other pre-cancerous lesions. However, its detection prior to tissue biopsy can be challenging in clinics. Moreover, biopsy examination is invasive and painful. Hence, there is an urgent need of new technology that facilitates accurate diagnostic prediction of OSF prior to biopsy. Here, we used FTIR spectroscopy coupled with chemometric techniques to distinguish the serum metabolic signatures of OSF patients (n = 30) and healthy controls (n = 30). Serum biochemical analyses have been performed to further support the FTIR findings. Absorbance intensities of 45 infrared wavenumbers differed significantly between OSF and normal serum FTIR spectra representing alterations in carbohydrates, proteins, lipids and nucleic acids. Nineteen prominent significant wavenumbers (P ≤ 0.001) at 1020, 1025, 1035, 1039, 1045, 1078, 1055, 1100, 1117, 1122, 1151, 1169, 1243, 1313, 1398, 1453, 1544, 1650 and 1725 cm- 1 provided excellent segregation of OSF spectra from normal using multivariate statistical techniques. These findings provided essential information on the metabolic features of blood serum of OSF patients and established that FTIR spectroscopy coupled with chemometric analysis can be potentially useful in the rapid and accurate preoperative screening/diagnosis of OSF.

Characterization and cytotoxic activity of sulfated derivatives of polysaccharides from Agaricus brasiliensis

PubMed Central

Cardozo, F. T. G. S.; Camelini, C. M.; Cordeiro, M. N. S.; Mascarello, A.; Malagoli, B. G.; Larsen, I.; Rossi, M. J.; Nunes, R. J.; Braga, F. C.; Brandt, C.R.; Simões, C. M. O.

2014-01-01

Agaricus brasiliensis cell-wall polysaccharides isolated from fruiting body (FR) and mycelium (MI) and their respective sulfated derivatives (FR-S and MI-S) were chemically characterized using elemental analysis, TLC, FT-IR, NMR, HPLC, and thermal analysis. Cytotoxic activity was evaluated against A549 tumor cells by MTT and sulforhodamine assays. The average molecular weight (Mw) of FR and MI was estimated to be 609 and 310 kDa, respectively. FR-S (127 kDa) and MI-S (86 kDa) had lower Mw, probably due to hydrolysis occurred during the sulfation reaction. FR-S and MI-S presented ~14 % sulfur content in elemental analysis. Sulfation of samples was characterized by the appearance of two new absorption bands at 1253 and 810 cm−1 in the infrared spectra, related to S=O and C-S-O sulfate groups, respectively. Through 1H and 13C NMR analysis FR-S was characterized as a (1→6)-(1→3)-β-D-glucan fully sulfated at C-4 and C-6 terminal and partially sulfated at C-6 of (1→3)-β-D-glucan moiety. MI-S was shown to be a (1→3)-β-D-gluco-(1→2)-β-D-mannan, partially sulfated at C-2, C-3, C-4, and C-6, and fully sulfated at C-6 of the terminal residues. The combination of high degree of sulfation and low molecular weight was correlated with the increased cytotoxic activity (48 h of treatment) of both FR-S (EC50=605.6 μg/mL) and MI-S (EC50=342.1 μg/mL) compared to the non-sulfated polysaccharides FR and MI (EC50>1500 μg/mL). PMID:23511057

In situ hydrothermal syntheses, structures and photoluminescent properties of four novel metal-organic frameworks constructed by lanthanide (Ln=Ce(III), Pr(III), Eu(III)) and Cu(I) metals with flexible dicarboxylate acids and piperazine-based ligands

NASA Astrophysics Data System (ADS)

Ay, Burak; Karaca, Serkan; Yildiz, Emel; Lopez, Valerie; Nanao, Max H.; Zubieta, Jon

2016-01-01

Four novel metal-organic frameworks,[Cu2Cl2(pyrz)]n (1) and (H2pip)n[Ln2(pydc)4(H2O)2]n (Ln=Ce (2), Pr (3) and Eu (4), H2pzdc=2,3-pyrazinedicarboxylic acid, pyrz=pyrazine, H2pydc=2,6-pyridinedicarboxylic acid, H2pip=piperazine) have been synthesized under hydrothermal conditions and characterized by the elemental analysis, ICP, Far IR (FIR), FT-IR spectra, TGA, single crystal X-ray diffraction analysis and powder X-ray diffraction (PXRD). Compound 1 is two-dimensional containing Cl-Cu-Cl sites, while the lanthanide complexes contain one-dimensional infinite Ln-O-Ln chains. All the complexes show high thermal stability. The complexes 1-3 exhibit luminescence emission bands at 584, 598 and 614 nm at room temperature when excited at 300 nm. Complex 4 exhibits bright red solid-state phosphorescence upon exposure to UV radiation at room temperature.

Production of 5-hydroxymethylfurfural from starch-rich food waste catalyzed by sulfonated biochar.

PubMed

Cao, Leichang; Yu, Iris K M; Chen, Season S; Tsang, Daniel C W; Wang, Lei; Xiong, Xinni; Zhang, Shicheng; Ok, Yong Sik; Kwon, Eilhann E; Song, Hocheol; Poon, Chi Sun

2018-03-01

Sulfonated biochar derived from forestry wood waste was employed for the catalytic conversion of starch-rich food waste (e.g., bread) into 5-hydroxymethylfurfural (HMF). Chemical and physical properties of catalyst were characterized by Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), scanning electron microscopy (SEM), Brunauer-Emmett-Teller (BET) surface area, and elemental analysis. The conversion of HMF was investigated via controlling the reaction parameters such as catalyst loading, temperature, and reaction time. Under the optimum reaction conditions the HMF yield of 30.4 Cmol% (i.e., 22 wt% of bread waste) was achieved in the mixture of dimethylsulfoxide (DMSO)/deionized-water (DIW) at 180 °C in 20 min. The effectiveness of sulfonated biochar catalyst was positively correlated to the density of strong/weak Brønsted acidity (SO 3 H, COOH, and OH groups) and inversely correlated to humins content on the surface. With regeneration process, sulfonated biochar catalyst displayed excellent recyclability for comparable HMF yield from bread waste over five cycles. Copyright © 2017 Elsevier Ltd. All rights reserved.

One-Pot Green Synthesis of Graphene Nanosheets Encapsulated Gold Nanoparticles for Sensitive and Selective Detection of Dopamine

PubMed Central

Thirumalraj, Balamurugan; Rajkumar, Chellakannu; Chen, Shen-Ming; Palanisamy, Selvakumar

2017-01-01

We report a simple new approach for green preparation of gallic acid supported reduced graphene oxide encapsulated gold nanoparticles (GA-RGO/AuNPs) via one-pot hydrothermal method. The as-prepared composites were successfully characterized by using Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, X-ray powder diffraction techniques (XRD), scanning electron microscope (SEM), high resolution transmission electron microscopy (HRTEM) and elemental analysis. The GA-RGO/AuNPs modified electrode behaves as a hybrid electrode material for sensitive and selective detection of dopamine (DA) in presence of ascorbic acid (AA) and uric acid (UA). The GA-RGO/AuNPs modified electrode displays an excellent electrocatalytic activity towards the oxidation of DA and exhibits a wide linear response range over the DA concentrations from 0.01–100.3 μM with a detection limit (LOD) of 2.6 nM based on S/N = 3. In addition, the proposed sensor could be applied for the determination of DA in human serum and urine samples for practical analysis. PMID:28128225

Chitin-Lignin Material as a Novel Matrix for Enzyme Immobilization

PubMed Central

Zdarta, Jakub; Klapiszewski, Łukasz; Wysokowski, Marcin; Norman, Małgorzata; Kołodziejczak-Radzimska, Agnieszka; Moszyński, Dariusz; Ehrlich, Hermann; Maciejewski, Hieronim; Stelling, Allison L.; Jesionowski, Teofil

2015-01-01

Innovative materials were made via the combination of chitin and lignin, and the immobilization of lipase from Aspergillus niger. Analysis by techniques including FTIR, XPS and 13C CP MAS NMR confirmed the effective immobilization of the enzyme on the surface of the composite support. The electrokinetic properties of the resulting systems were also determined. Results obtained from elemental analysis and by the Bradford method enabled the determination of optimum parameters for the immobilization process. Based on the hydrolysis reaction of para-nitrophenyl palmitate, a determination was made of the catalytic activity, thermal and pH stability, and reusability. The systems with immobilized enzymes were found to have a hydrolytic activity of 5.72 mU, and increased thermal and pH stability compared with the native lipase. The products were also shown to retain approximately 80% of their initial catalytic activity, even after 20 reaction cycles. The immobilization process, using a cheap, non-toxic matrix of natural origin, leads to systems with potential applications in wastewater remediation processes and in biosensors. PMID:25903282

Synthesis and Characterization of Molybdenum Based Colloidal Particles.

PubMed

Moreno; Vidoni; Ovalles; Chaudret; Urbina; Krentzein

1998-11-15

The synthesis and characterization of molybdenum colloidal particles were evaluated using thermal and sonochemical methods and starting from different metal precursors, Mo(CO)6 and (NH4)2MoS4. The products were characterized by elemental analysis, spectroscopic (UV, FTIR), and surface analysis (XPS) techniques, as well as by transmission electron microscopy (TEM) for determining the particle sizes. Using Mo(CO)6 as metal source, particle sizes with an average diameter of 1.5 nm can be obtained using tert-amyl alcohol as solvent and tetrahydrothiophene as sulfurating ligand. The characterization of these particles showed that they are composed of molybdenum oxide MoO3. Using (NH4)2MoS4 as metal precursor, particles with average diameters of 4.7 and 2.5 nm were synthesized using thermal and sonochemical methods, respectively. The characterization of these particles showed them to be composed of molybdenum sulfide, MoS2. The sonochemical method proved to be the fastest and most convenient synthetic pathway of obtaining small colloidal particles at low temperatures and with control of the average size. Copyright 1998 Academic Press.

Green synthesis of silver nanoparticles using Coffea arabica seed extract and its antibacterial activity.

PubMed

Dhand, Vivek; Soumya, L; Bharadwaj, S; Chakra, Shilpa; Bhatt, Deepika; Sreedhar, B

2016-01-01

A novel green source was opted to synthesize silver nanoparticles using dried roasted Coffea arabica seed extract. Bio-reduction of silver was complete when the mixture (AgNO3+extract) changed its color from light to dark brown. UV-vis spectroscopy result showed maximum adsorption at 459 nm, which represents the characteristic surface plasmon resonance of nanosilver. X-ray crystal analysis showed that the silver nanoparticles are highly crystalline and exhibit a cubic, face centered lattice with characteristic (111), (200), (220) and (311) orientations. Particles exhibit spherical and ellipsoidal shaped structures as observed from TEM. Composition analysis obtained from SEM-EDXA confirmed the presence of elemental signature of silver. FTIR results recorded a downward shift of absorption bands between 800-1500 cm(-1) indicting the formation of silver nanoparticles. The mean particle size investigated using DLS was found to be in between 20-30 nm respectively. Anti-bacterial activity of silver nanoparticles on E. coli and S. aureus demonstrated diminished bacterial growth with the development of well-defined inhibition zones. Copyright © 2015 Elsevier B.V. All rights reserved.

One-Pot Green Synthesis of Graphene Nanosheets Encapsulated Gold Nanoparticles for Sensitive and Selective Detection of Dopamine

NASA Astrophysics Data System (ADS)

Thirumalraj, Balamurugan; Rajkumar, Chellakannu; Chen, Shen-Ming; Palanisamy, Selvakumar

2017-01-01

We report a simple new approach for green preparation of gallic acid supported reduced graphene oxide encapsulated gold nanoparticles (GA-RGO/AuNPs) via one-pot hydrothermal method. The as-prepared composites were successfully characterized by using Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, X-ray powder diffraction techniques (XRD), scanning electron microscope (SEM), high resolution transmission electron microscopy (HRTEM) and elemental analysis. The GA-RGO/AuNPs modified electrode behaves as a hybrid electrode material for sensitive and selective detection of dopamine (DA) in presence of ascorbic acid (AA) and uric acid (UA). The GA-RGO/AuNPs modified electrode displays an excellent electrocatalytic activity towards the oxidation of DA and exhibits a wide linear response range over the DA concentrations from 0.01-100.3 μM with a detection limit (LOD) of 2.6 nM based on S/N = 3. In addition, the proposed sensor could be applied for the determination of DA in human serum and urine samples for practical analysis.

Immobilization of kojic acid in ZnAl-hydrotalcite like compounds

NASA Astrophysics Data System (ADS)

Ambrogi, Valeria; Perioli, Luana; Nocchetti, Morena; Latterini, Loredana; Pagano, Cinzia; Massetti, Elena; Rossi, Carlo

2012-01-01

Kojic acid (KOJ) is a melanin synthesis inhibitor widely used as skin lightening agent in topical preparations. Unfortunately it is easily susceptible to photo-oxidation, phenomenon responsible for chemical and organoleptic modifications. The aim of this work was the intercalation of KOJ in hydrotalcite-like compounds (HTlc) in order to stabilize KOJ and to reduce its photolability. Hydrotalcite containing Zn and Al (ZnAl-HTlc) was used as host to obtain the final compound ZnAl-HTlc-KOJ. The intercalation was carried out, after many attempts, by ionic exchange mechanism by means of the strong base EtO- in anhydrous ethanol/dimethylsulfoxide (DMSO) mixture as solvent in order to generate KOJ- anions. The final product was characterized by the X-ray powder diffraction (XRPD), FT-IR spectroscopy, thermogravimetric analysis (TGA), differential scanning calorimetry (DSC) and elemental analysis. The intercalated compound was formulated in a siliconic water free self-emulsifying ointment and the in vitro release profile was evaluated. All samples (intercalation compound and its formulation) were submitted also to spectrophotometric assays in order to evaluate the matrix protective effect towards ultraviolet rays.

A facile access to new diazepines derivatives: Spectral characterization and crystal structures of 7-(thiophene-2-yl)-5-(trifluoromethyl)-2,3-dihydro-1H-1,4-diazepine and 2-thiophene-4-trifluoromethyl-1,5-benzodiazepine

NASA Astrophysics Data System (ADS)

Ahumada, Guillermo; Carrillo, David; Manzur, Carolina; Fuentealba, Mauricio; Roisnel, Thierry; Hamon, Jean-René

2016-12-01

The one-pot double condensation reaction of 2-thenoyltrifluoroacetone (2-TTA) with ethylendiamine or o-phenylenediamine, in a 2:1 stoichiometric molar ratio, leads to the formation of 7-(thiophene-2-yl)-5-(trifluoromethyl)-2,3-dihydro-1H-1,4-diazepine 2 and 2-thiophene-4-trifluoromethyl-1,5-benzodiazepine 3, that were isolated in 56 and 53% yields, respectively. The bis(trifluoroacetamide)ethylene derivative 1 was also isolated in 32% yield as a side-product in the reaction of 2-TTA and ethylenediamine. Compounds 1-3 were fully characterized by elemental analysis, FT-IR and multinuclear (1H, 13C and 19F) NMR spectroscopy. In addition, their molecular identities and geometries have been authenticated by single-crystal X-ray diffraction analysis. The spectroscopic and structural data confirm that the 1,4-diazepine 2 and the 1,5-benzodiazepine 3 exist in the imine-enamine and diimine tautomeric forms, respectively, both in solution and in the solid-state.

Characterization of Sintering Dust, Blast Furnace Dust and Carbon Steel Electric Arc Furnace Dust

NASA Astrophysics Data System (ADS)

Chang, Feng; Wu, Shengli; Zhang, Fengjie; Lu, Hua; Du, Kaiping

In order to make a complete understanding of steel plant metallurgical dusts and to realize the goal of zero-waste, a study of their properties was undertaken. For these purposes, samples of two sintering dusts (SD), two blast furnace dusts (BFD), and one electric arc furnace dust (EAFD) taken from the regular production process were subjected to a series of tests. The tests were carried out by using granulometry analysis, chemical analysis, X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectroscopy via SEM (EDS), and Fourier transform infrared spectroscopy (FTIR). The dominant elements having an advantage of reuse are Fe, K, Cl, Zn, C. The dominant mineralogical phases identified in sintering dust are KCl, Fe2O3, CaCO3, CaMg(CO3)2, NaCl, SiO2. Mineralogical phases exist in blast furnace dust are Fe2O3, Fe3O4, with small amount of KCl and kaolinite coexist. While in electric arc furnace dust, Fe3O4, ZnFe2O4, CaCO3, CaO, Ca(OH)2 are detected.

Synthesis, characterization and anti-bacterial activities of pure and Co-doped BaSO4 nanoparticles via chemical precipitation route

NASA Astrophysics Data System (ADS)

Sivakumar, S.; Soundhirarajan, P.; Venkatesan, A.; Khatiwada, Chandra Prasad

2015-02-01

In the present study, we reported that the synthesis and characterization of pure and diverse mole Co-doped BaSO4 nanoparticles have been synthesized by chemical precipitation technique. X-ray diffraction analysis (XRD) brought out the information about the synthesized products is orthorhombic structure and highly crystalline in nature. The average grain size of the samples was determined by using the Debye-Scherer's equation. The existence of functional groups and band area of the samples were confirmed by Fourier transform infrared (FTIR) spectroscopy. The direct and indirect band gap energy of pure and doped samples was carried out using UV-VIS-DRS. The surface micrograph, morphological distribution and elemental compositions of the synthesized products were assessed by scanning electron microscopy (SEM) and Energy dispersive X-ray (EDS). Thermo gravimetric and differential thermal analysis (TG-DTA) techniques were analyzed thermal behaviour of pure and Co-doped samples. Finally, antibacterial activities found the Gram-positive and Gram-negative bacteria are more active in transporter, dehydrogenize and periplasmic enzymatic activities of pure and doped samples.

Equilibrium, kinetic and thermodynamic studies for adsorption of BTEX onto Ordered Mesoporous Carbon (OMC).

PubMed

Konggidinata, Mas Iwan; Chao, Bing; Lian, Qiyu; Subramaniam, Ramalingam; Zappi, Mark; Gang, Daniel Dianchen

2017-08-15

Chemical and petrochemical industries produce substantial amounts of wastewater everyday. This wastewater contains organic pollutants such as benzene, toluene, ethylbenzene and xylenes (BTEX) that are toxic to human and aquatic life. Ordered Mesoporous Carbon (OMC), the adsorbent that possesses the characteristics of an ideal adsorbent was investigated to understand its properties and suitability for BTEX removal. Adsorption isotherms, adsorption kinetics, the effects of initial BTEX concentrations and temperatures on the adsorption process were studied. The OMCs were characterized using surface area and pore size analyzer, transmission electron microscopy (TEM), elemental analysis, thermogravimetric analysis (TGA) and fourier transform infrared spectroscopy (FTIR). The results suggested that the Langmuir Isotherm and Pseudo-Second-Order Models described the experimental data well. The thermodynamic parameters, Gibbs free energy (ΔG°), the enthalpy change (ΔH°) and the entropy change (ΔS°) of adsorption indicated that the adsorption processes were physical, endothermic, and spontaneous. In addition, OMC had 27% higher overall adsorption capacities compared to granular activated carbon (GAC). Copyright © 2017 Elsevier B.V. All rights reserved.

One Step Synthesis of NiO Nanoparticles via Solid-State Thermal Decomposition at Low-Temperature of Novel Aqua(2,9-dimethyl-1,10-phenanthroline)NiCl2 Complex

PubMed Central

Barakat, Assem; Al-Noaimi, Mousa; Suleiman, Mohammed; Aldwayyan, Abdullah S.; Hammouti, Belkheir; Ben Hadda, Taibi; Haddad, Salim F.; Boshaala, Ahmed; Warad, Ismail

2013-01-01

[NiCl2(C14H12N2)(H2O)] complex has been synthesized from nickel chloride hexahydrate (NiCl2·6H2O) and 2,9-dimethyl-1,10-phenanthroline (dmphen) as N,N-bidentate ligand. The synthesized complex was characterized by elemental analysis, infrared (IR) spectroscopy, ultraviolet-visible (UV-vis) spectroscopy and differential thermal/thermogravimetric analysis (TG/DTA). The complex was further confirmed by single crystal X-ray diffraction (XRD) as triclinic with space group P-1. The desired complex, subjected to thermal decomposition at low temperature of 400 ºC in an open atmosphere, revealed a novel and facile synthesis of pure NiO nanoparticles with uniform spherical particle; the structure of the NiO nanoparticles product was elucidated on the basis of Fourier transform infrared (FT-IR), UV-vis spectroscopy, TG/DTA, XRD, scanning electron microscopy (SEM), energy-dispersive X-ray spectrometry (EDXS) and transmission electron microscopy (TEM). PMID:24351867

Host-guest interaction of ZnBDC-MOF + doxorubicin: A theoretical and experimental study

NASA Astrophysics Data System (ADS)

Vasconcelos, Iane B.; Wanderley, Kaline A.; Rodrigues, Nailton M.; da Costa, Nivan B.; Freire, Ricardo O.; Junior, Severino A.

2017-03-01

The incorporation of drugs in biodegradable polymeric particles is one of many processes that controllably and significantly increase their release and action. In this paper, we describe the synthesis and physicochemical characterization of ZnBDC-MOF + doxorubicin (DOXO@ZnBDC) and the system's effectiveness in the sustained release of the drug doxorubicin. An experimental and theoretical study is presented of the interaction between the [Zn(BDC)(H2O)2]n MOF and the drug doxorubicin (DOXO). The synthesis was characterized by elemental analysis and X-ray powder diffraction (XRPD). The experimental incorporation was accomplished and analyzed by Fourier transform infrared spectroscopy (FTIR), XRPD and UV-Vis (ultraviolet-visible) spectrophotometry. Based on an analysis of the doxorubicin release profile, our results suggest that the drug delivery system showed slower release than other systems under development. Studies of cytotoxicity by the MTT method showed good results for the system developed with antineoplastic doxorubicin, and together with the other results of this study, suggest the successful development of a MOF-based drug delivery system.

Synthesis, characterization and solid-state properties of [Zn(Hdmmthiol)2]\\cdot2H2O complex

NASA Astrophysics Data System (ADS)

Dagdelen, Fethi; Aydogdu, Yildirim; Dey, Kamalendu; Biswas, Susobhan

2016-05-01

The zinc(II) complex with tridentate thiohydrazone ligand have been prepared by metal template reaction. The metal template reaction was used to prepare the zinc (II) complex with tridentate thiohydrazone ligand. The reaction of diacetylmonoxime and, morpholine N-thiohydrazidewith Zn(OAc)2 \\cdot2H2O under reflux yielded the formation of the [Zn(Hdmmthiol )2]\\cdot2H2O complex. The complex was characterized by a combination of protocols including elemental analysis, UV+vis, FT-IR, TG and PXRD. The temperature dependence of the electrical conductivity and the optical property of the [Zn(Hdmmthiol )2] \\cdot2H2O complex is called H2dammthiol was studied. Powder X-ray diffraction (PXRD) method was used to investigate the crystal structure of the sample. The zinc complex was shown to be a member of the triclinic system. The zinc complex was determined to have n-type conductivity as demonstrated in the hot probe measurements. The complex was determined to display direct optical transition with band gaps of 2.52eV as determined by the optical absorption analysis.

Biologically active and thermally stable polymeric Schiff base and its metal polychelates: Their synthesis and spectral aspects

NASA Astrophysics Data System (ADS)

Rasool, Raza; Hasnain, Sumaiya

2015-09-01

New metal polychelates of Mn(II), Co(II), Ni(II), Cu(II) and Zn(II) obtained by the interaction of metal acetates with polymeric Schiff base containing formaldehyde and piperazine, have been investigated. Structural and spectroscopic properties have been evaluated by elemental analysis, FT-IR and 1H-NMR. Geometry of the chelated polymers was confirmed by magnetic susceptibility measurements, UV-Visible spectroscopy and Electron Spin Resonance. The molecular weight of the polymer was determined by gel permeation chromatography (GPC). Thermogravimetric analysis indicated that metal polychelates were more thermally stable than their corresponding ligand. All compounds were screened for their antimicrobial activities against Escherichia coli, Staphylococcus aureus, Bacillus subtilis, (bacteria) and Candida albicans, Microsporum canis, Cryptococcus neoformans (fungi) by agar well diffusion method. Interestingly, the polymeric Schiff base was found to be antimicrobial in nature but less effective as compared to the metal polychelates. On the basis of thermal and antimicrobial behavior, these polymers hold potential applications as thermally resistant antimicrobial and antifouling coating materials as well as antimicrobial packaging materials.

Preparation and characterization of multi stimuli-responsive photoluminescent nanocomposites of graphene quantum dots with hyperbranched polyethylenimine derivatives

NASA Astrophysics Data System (ADS)

Liu, Xing; Liu, Hua-Ji; Cheng, Fa; Chen, Yu

2014-06-01

Oxidized graphene sheets (OGS) were treated with a hyperbranched polyethylenimine (PEI) under hydrothermal conditions to generate nanocomposites of graphene quantum dots (GQDs) functionalized with PEI (GQD-PEIs). The influence of the reaction temperature and the PEI/OGS feed ratio on the photoluminescence properties of the GQD-PEIs was studied. The obtained GQD-PEIs were characterized by TEM, dynamic light scattering, elemental analysis, FTIR, zeta potential measurements and 1H NMR spectroscopy, from which their structural information was inferred. Subsequently, isobutyric amide (IBAm) groups were attached to the GQD-PEIs through the amidation reaction of isobutyric anhydride with the PEI moieties, which resulted in GQD-PEI-IBAm nanocomposites. GQD-PEI-IBAm was not only thermoresponsive, but also responded to other stimuli, including inorganic salts, pH, and loaded organic guests. The cloud point temperature (Tcp) of aqueous solutions of GQD-PEI-IBAm could be modulated through changing the number of IBAm units in GQD-PEI-IBAm, by varying the type and concentration of the inorganic salts and loaded organic guests, or by varying the pH. All the obtained GQD-PEI-IBAm nanocomposites were photoluminescent, and their maximum emission wavelengths were not influenced by outside stimuli. Their emission intensities were influenced a little or negligibly by pH, traditional salting-out anions (Cl- and SO42-), and the relatively polar aspirin guest. However, the traditional salting-in I- anion and the more hydrophobic 1-pyrenebutyric acid (PBA) guest could effectively quench their fluorescence. 2D NOESY 1H NMR spectra verified that GQD-PEI-IBAm accommodated the relatively polar aspirin guest using the PEI-IBAm shell, but adsorbed the relatively hydrophobic PBA guest through the nanographene core. The release rate of the guest encapsulated by the thermoresponsive GQD is different below and above Tcp.Oxidized graphene sheets (OGS) were treated with a hyperbranched polyethylenimine (PEI) under hydrothermal conditions to generate nanocomposites of graphene quantum dots (GQDs) functionalized with PEI (GQD-PEIs). The influence of the reaction temperature and the PEI/OGS feed ratio on the photoluminescence properties of the GQD-PEIs was studied. The obtained GQD-PEIs were characterized by TEM, dynamic light scattering, elemental analysis, FTIR, zeta potential measurements and 1H NMR spectroscopy, from which their structural information was inferred. Subsequently, isobutyric amide (IBAm) groups were attached to the GQD-PEIs through the amidation reaction of isobutyric anhydride with the PEI moieties, which resulted in GQD-PEI-IBAm nanocomposites. GQD-PEI-IBAm was not only thermoresponsive, but also responded to other stimuli, including inorganic salts, pH, and loaded organic guests. The cloud point temperature (Tcp) of aqueous solutions of GQD-PEI-IBAm could be modulated through changing the number of IBAm units in GQD-PEI-IBAm, by varying the type and concentration of the inorganic salts and loaded organic guests, or by varying the pH. All the obtained GQD-PEI-IBAm nanocomposites were photoluminescent, and their maximum emission wavelengths were not influenced by outside stimuli. Their emission intensities were influenced a little or negligibly by pH, traditional salting-out anions (Cl- and SO42-), and the relatively polar aspirin guest. However, the traditional salting-in I- anion and the more hydrophobic 1-pyrenebutyric acid (PBA) guest could effectively quench their fluorescence. 2D NOESY 1H NMR spectra verified that GQD-PEI-IBAm accommodated the relatively polar aspirin guest using the PEI-IBAm shell, but adsorbed the relatively hydrophobic PBA guest through the nanographene core. The release rate of the guest encapsulated by the thermoresponsive GQD is different below and above Tcp. Electronic supplementary information (ESI) available: Elemental analysis data; typical FTIR spectra; typical photographs of the GQD solution before and after phase transition; typical luminescence photographs, and typical photoluminescence spectra. See DOI: 10.1039/c4nr00739e

FT-IR and FT-Raman characterization of non-cellulosic polysaccharides fractions isolated from plant cell wall.

PubMed

Chylińska, Monika; Szymańska-Chargot, Monika; Zdunek, Artur

2016-12-10

The purpose of this work was to reveal the structural changes of cell wall polysaccharides' fractions during tomato fruit development by analysis of spectral data. Mature green and red ripe tomato fruit were taken into consideration. The FT-IR spectra of water soluble pectin (WSP), imidazole soluble pectin (ISP) and diluted alkali soluble pectin (DASP) contained bands typical for pectins. Whereas for KOH fraction spectra bands typical for hemicelluloses were present. The FT-IR spectra showed the drop down of esterification degree of WSP and ISP polysaccharides during maturation. The changes in polysaccharides structure revealed by spectra were the most visible in the case of pectic polysaccharides. The WSP and DASP fraction pectins molecules length were shortened during tomato maturation and ripening. Whereas the ISP fraction spectra analysis showed that this fraction contained rhamnogalacturonan I, but also for red ripe was rich in pectic galactan comparing with ISP fraction from mature green. Copyright © 2016 Elsevier Ltd. All rights reserved.

Analysis of bacteria on steel surfaces using reflectance micro-Fourier transform infrared spectroscopy.

PubMed

Ojeda, Jesús J; Romero-González, María E; Banwart, Steven A

2009-08-01

Reflectance micro-Fourier transform infrared (FT-IR) analysis has been applied to characterize biofilm formation of Aquabacterium commune, a common microorganism present on drinking water distribution systems, onto the increasingly popular pipe material stainless steel EN1.4307. The applicability of the reflectance micro-FT-IR technique for analyzing the bacterial functional groups is discussed, and the results are compared to spectra obtained using more conventional FT-IR techniques: transmission micro-FT-IR, attenuated transmitted reflectance (ATR), and KBr pellets. The differences between the infrared spectra of wet and dried bacteria, as well as free versus attached bacteria, are also discussed. The spectra obtained using reflectance micro-FT-IR spectroscopy were comparable to those obtained using other FT-IR techniques. The absence of sample preparation, the potential to analyze intact samples, and the ability to characterize opaque and thick samples without the need to transfer the bacterial samples to an infrared transparent medium or produce a pure culture were the main advantages of reflectance micro-FT-IR spectroscopy.

An empirical evaluation of three vibrational spectroscopic methods for detection of aflatoxins in maize.

PubMed

Lee, Kyung-Min; Davis, Jessica; Herrman, Timothy J; Murray, Seth C; Deng, Youjun

2015-04-15

Three commercially available vibrational spectroscopic techniques, including Raman, Fourier transform near infrared reflectance (FT-NIR), and Fourier transform infrared (FTIR) were evaluated to help users determine the spectroscopic method best suitable for aflatoxin analysis in maize (Zea mays L.) grain based on their relative efficiency and predictive ability. Spectral differences of Raman and FTIR spectra were more marked and pronounced among aflatoxin contamination groups than those of FT-NIR spectra. From the observations and findings in our current and previous studies, Raman and FTIR spectroscopic methods are superior to FT-NIR method in terms of predictive power and model performance for aflatoxin analysis and they are equally effective and accurate in predicting aflatoxin concentration in maize. The present study is considered as the first attempt to assess how spectroscopic techniques with different physical processes can influence and improve accuracy and reliability for rapid screening of aflatoxin contaminated maize samples. Copyright © 2014 Elsevier Ltd. All rights reserved.

Synthesis and characterization of cassava starch with maleic acid derivatives by etherification reaction.

PubMed

Clasen, Samuel H; Müller, Carmen M O; Parize, Alexandre L; Pires, Alfredo T N

2018-01-15

Cassava starch was grafted with three different esters by the etherification reaction and its modification was characterized by 1 H NMR, FTIR, DSC, SEM, XDR, contact angle and SLS. The samples grafted with diethyl maleate, dipropyl maleate, and dibutyl maleate showed DS values of 2.3, 1.0 and 2.0, respectively, determined from 1 H NMR analysis and confirmed by FTIR analysis, with the appearance of bands at 1721, 1550 and 1126cm -1 . The FTIR, XRD, SEM and DSC results indicated a change in the intra and intermolecular hydrogen interactions in the grafted starch when compared to native starch. Based on the contact angles, it was observed that the macromolecular starch chain acquired hydrophobic characteristics through the substitution of the hydrogens with di maleate esters. The characteristics acquired by grafted starch allow it to be used for the encapsulation of bioactive molecules for the production of bioactive packages and the production of biodegradable packages. Copyright © 2017 Elsevier Ltd. All rights reserved.

Quantitative determination and evaluation of Paris polyphylla var. yunnanensis with different harvesting times using UPLC-UV-MS and FT-IR spectroscopy in combination with partial least squares discriminant analysis.

PubMed

Yang, Yuan-Gui; Zhang, Ji; Zhao, Yan-Li; Zhang, Jin-Yu; Wang, Yuan-Zhong

2017-07-01

A rapid method was developed and validated by ultra-performance liquid chromatography-triple quadrupole mass spectroscopy with ultraviolet detection (UPLC-UV-MS) for simultaneous determination of paris saponin I, paris saponin II, paris saponin VI and paris saponin VII. Partial least squares discriminant analysis (PLS-DA) based on UPLC and Fourier transform infrared (FT-IR) spectroscopy was employed to evaluate Paris polyphylla var. yunnanensis (PPY) at different harvesting times. Quantitative determination implied that the various contents of bioactive compounds with different harvesting times may lead to different pharmacological effects; the average content of total saponins for PPY harvested at 8 years was higher than that from other samples. The PLS-DA of FT-IR spectra had a better performance than that of UPLC for discrimination of PPY from different harvesting times. Copyright © 2016 John Wiley & Sons, Ltd.

FT-IR spectroscopic, thermal analysis of human urinary stones and their characterization

NASA Astrophysics Data System (ADS)

Selvaraju, R.; Raja, A.; Thiruppathi, G.

2015-02-01

In the present study, FT-IR, XRD, TGA-DTA spectral methods have been used to investigate the chemical compositions of urinary calculi. Multi-components of urinary calculi such as calcium oxalate, hydroxyl apatite, struvite and uric acid have been studied. The chemical compounds are identified by FT-IR spectroscopic technique. The mineral identification was confirmed by powder X-ray diffraction patterns as compared with JCPDS reported values. Thermal analysis techniques are considered the best techniques for the characterization and detection of endothermic and exothermic behaviors of the urinary stones. The percentages of each hydrate (COM and COD) are present together, in the presences of MAPH or UA. Finally, the present study suggests that the Urolithiasis is significant health problem in children, and is very common in some parts of the world, especially in India. So that present study is so useful and helpful to the scientific community for identification of latest human health problems and their remedies using spectroscopic techniques.

FTIR, FT-Raman, FT-NMR and quantum chemical investigations of 3-acetylcoumarin.

PubMed

Arjunan, V; Sakiladevi, S; Marchewka, M K; Mohan, S

2013-05-15

3-Acetylcoumarin (3AC) was synthesised by a Knoevenagel reaction. Conformational analysis using the B3LYP method was also carried out to determine the most stable conformation of the compound. FTIR and FT-Raman spectra of 3AC have been recorded in the range 4000-400 and 4000-100 cm(-1), respectively. (1)H and (13)C NMR spectra have also been recorded. The complete vibrational assignment and analysis of the fundamental modes of the compound were carried out using the experimental FTIR and FT-Raman data and quantum mechanical studies. The experimental vibrational frequencies were compared with the wavenumbers obtained theoretically from the DFT-B3LYP/B3PW91 gradient calculations employing the standard 6-31G(**), high level 6-311++G(**) and cc-pVTZ basis sets for optimised geometry of the compound. The frontier molecular orbital energies of the compound are determined by DFT method. Copyright © 2013 Elsevier B.V. All rights reserved.