diffraction ft-ir spectroscopy: Topics by Science.gov

Sample records for diffraction ft-ir spectroscopy

Comparative investigation of Fourier transform infrared (FT-IR) spectroscopy and X-ray diffraction (XRD) in the determination of cotton fiber crystallinity.

PubMed

Liu, Yongliang; Thibodeaux, Devron; Gamble, Gary; Bauer, Philip; VanDerveer, Don

2012-08-01

Despite considerable efforts in developing curve-fitting protocols to evaluate the crystallinity index (CI) from X-ray diffraction (XRD) measurements, in its present state XRD can only provide a qualitative or semi-quantitative assessment of the amounts of crystalline or amorphous fraction in a sample. The greatest barrier to establishing quantitative XRD is the lack of appropriate cellulose standards, which are needed to calibrate the XRD measurements. In practice, samples with known CI are very difficult to prepare or determine. In a previous study, we reported the development of a simple algorithm for determining fiber crystallinity information from Fourier transform infrared (FT-IR) spectroscopy. Hence, in this study we not only compared the fiber crystallinity information between FT-IR and XRD measurements, by developing a simple XRD algorithm in place of a time-consuming and subjective curve-fitting process, but we also suggested a direct way of determining cotton cellulose CI by calibrating XRD with the use of CI(IR) as references.
Wood liquefaction and its application to Novolac resin

Treesearch

Hui Pan; Chung-Yun Hse; Todd F. Shupe

2009-01-01

Wood liquefaction was conducted using phenol as a reagent solvent with a weak acid catalyst in two different reactors: (Alma et al., 1995a.) an atmospheric glass reactor and (Alma et al., 1995b.) a sealed ParrÂ® reactor. Residues were characterized by wet chemical analyses, Fourier transform infrared (FT-IR) spectroscopy, and X-ray diffraction (XRD). The FT-IR...
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 and characterization of nano TiO2-SiO2: PVA composite - a novel route

NASA Astrophysics Data System (ADS)

Venckatesh, Rajendran; Balachandaran, Kartha; Sivaraj, Rajeshwari

2012-07-01

A novel, simple, less time consuming and cost-effective sol-gel method has been developed to synthesize nano titania-silica with polyvinyl alcohol (PVA) composite relatively at low temperature in acidic pH. Titania sol is prepared by hydrolysis of titanium tetrachloride and was mixed with silicic acid and tetrahydrofuran mixture. The reaction was carried out under vigorous stirring for 6 h and dried at room temperature with the addition of PVA solution. The resulting powders were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, Fourier transform infrared (FT-IR), UV-visible spectroscopy and thermal techniques. The grain size of the particles was calculated by X-ray diffraction; surface morphology and chemical composition were determined from scanning electron microscopy-energy dispersive spectroscopy; metal oxide stretching was confirmed from FT-IR spectroscopy; bandgap was calculated using UV-visible spectroscopy, and thermal stability of the prepared composite was determined by thermogravimetric/differential thermal analysis. Since TiO2 got agglomerated on the surface of SiO2, effective absorptive sites increase which in turn increase the photocatalytic efficiency of the resulting composite.
Curcumin-β-cyclodextrin inclusion complex: stability, solubility, characterisation by FT-IR, FT-Raman, X-ray diffraction and photoacoustic spectroscopy, and food application.

PubMed

Mangolim, Camila Sampaio; Moriwaki, Cristiane; Nogueira, Ana Claudia; Sato, Francielle; Baesso, Mauro Luciano; Neto, Antônio Medina; Matioli, Graciette

2014-06-15

Curcumin was complexed with β-CD using co-precipitation, freeze-drying and solvent evaporation methods. Co-precipitation enabled complex formation, as indicated by the FT-IR and FT-Raman techniques via the shifts in the peaks that were assigned to the aromatic rings of curcumin. In addition, photoacoustic spectroscopy and X-ray diffraction, with the disappearance of the band related to aromatic rings, by Gaussian fitting, and modifications in the spectral lines, respectively, also suggested complex formation. The possible complexation had an efficiency of 74% and increased the solubility of the pure colourant 31-fold. Curcumin-β-CD complex exhibited a sunlight stability 18% higher than the pure colourant. This material was stable to pH variations and storage at -15 and 4°C. With an isothermal heating at 100 and 150°C for 2h, the material exhibited a colour retention of approximately 99%. The application of curcumin-β-CD complex in vanilla ice creams intensified the colour of the products and produced a great sensorial acceptance. Copyright © 2013 Elsevier Ltd. All rights reserved.
Comparative investigation of Fourier Transform Infrared (FT-IR) spectroscopy and X-ray Diffraction (XRD) in the determination of cotton fiber crystallinity

USDA-ARS?s Scientific Manuscript database

Despite considerable efforts in developing the curve-fitting protocol to evaluate the crystallinity index (CI) from the X-ray diffraction (XRD) measurement, in its present state XRD procedure can only provide a qualitative or semi-quantitative assessment of the amounts of crystalline or amorphous po...
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.
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.
Evaluation of morphological and chemical aspects of different wood species by spectroscopy and thermal methods

NASA Astrophysics Data System (ADS)

Popescu, Maria-Cristina; Popescu, Carmen-Mihaela; Lisa, Gabriela; Sakata, Yusaku

2011-03-01

The aim of this study is to find the most convenient procedure to make an easy differentiation between various kinds of wood. The wood samples used were: fir (Acer alba), poplar (Populus tremula), lime (Tillia cordata), sycamore (Acer pseudoplatanus), sweet cherry (Prunus avium), hornbeam (Carpinus betulus), walnut (Juglans regia), beech (Fagus sylvatica), oak (Quercus robur). The methods of investigation used were FT-IR spectroscopy, X-ray diffraction and thermogravimetry. By FT-IR spectroscopy, was observed that the ratio values of lignin/carbohydrate IR bands for wood decreases with increasing the average wood density, showing a decrease in lignin content. Also, the calculated values of lignin percentage from the FT-IR spectra are in very good correlation with the values from literature. Following the deconvolution process of the X-ray diffraction patterns, it was found that the degree of crystallinity, the apparent lateral crystallite size, the proportion of crystallite interior chains and cellulose fraction tend to increase with increasing of the wood density. Thermal analysis is able to give information about degradation temperatures for the principal components of different wood samples. The shape of DTG curves depends on the wood species that cause the enlargement of the peaks or the maxima of the decomposition step varies at larger or smaller temperatures ranges. The temperatures and weight loss percentage are particular for each kind of wood. This study showed that analytical methods used have the potential to be important sources of information for a quick evaluation of the chemical composition of wood samples.
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
Experimental (13C NMR, 1H NMR, FT-IR, single-crystal X-ray diffraction) and DFT studies on 3,4-bis(isoproylamino)cyclobut-3-ene-1,2-dione.

PubMed

Süleymanoğlu, Nevin; Ustabaş, Reşat; Alpaslan, Yelda Bingöl; Eyduran, Fatih; Ozyürek, Cengiz; Iskeleli, Nazan Ocak

2011-12-01

In this work, 3,4-bis(isoproylamino)cyclobut-3-ene-1,2-dione C(10)H(16)N(2)O(2) (I), was synthesized and characterized by (13)C NMR, (1)H NMR, FT-IR, UV-vis spectroscopy and single-crystal X-ray diffraction. DFT method with 6-31G(d,p) basis set has been used to calculate the optimized geometrical parameters, atomic charges, vibrational frequencies and chemical shift values. The calculated vibrational frequencies and chemical shift values are compared with experimental FT-IR and NMR spectra. The results of the calculation shows good agreement between experimental and calculated values of the compound I. The existence of N-H⋯O type intermolecular ve C-H⋯O type intramolecular hydrogen bonds can be deduced from differences between experimental and calculated results of FT-IR and NMR. In addition, the molecular electrostatic potential map and frontier molecular orbitals and electronic absorption spectra were performed at B3LYP/6-31G(d,p) level of theory. HOMO-LUMO electronic transition of 4.90 eV are derived from the contribution of the bands π→π* and n→π* The spectral results obtained from FT-IR, NMR and X-ray of I revealed that the compound I is in predominantly enamine tautomeric form, which was supported by DFT calculations. Copyright © 2011 Elsevier B.V. All rights reserved.
Fourier Transform Infrared Spectroscopy: Part II. Advantages of FT-IR.

ERIC Educational Resources Information Center

Perkins, W. D.

1987-01-01

This is Part II in a series on Fourier transform infrared spectroscopy (FT-IR). Described are various advantages of FT-IR spectroscopy including energy advantages, wavenumber accuracy, constant resolution, polarization effects, and stepping at grating changes. (RH)
Evaluation of photostability of solid-state nicardipine hydrochloride polymorphs by using Fourier-transformed reflection-absorption infrared spectroscopy - effect of grinding on the photostability of crystal form.

PubMed

Teraoka, Reiko; Otsuka, Makoto; Matsuda, Yoshihisa

2004-11-22

Photostability and physicochemical properties of nicardipine hydrochloride polymorphs (alpha- and beta-form) were studied by using Fourier-transformed reflection-absorption infrared spectroscopy (FT-IR-RAS) of the tablets, X-ray powder diffraction analysis, differential scanning calorimetry (DSC), and color difference measurement. It was clear from the results of FT-IR-RAS spectra after irradiation that nicardipine hydrochloride in the solid state decomposed to its pyridine derivative when exposed to light. The photostability of the ground samples of two forms was also measured in the same manner. The two crystalline forms of the drug changed to nearly amorphous form after 150 min grinding in a mixer mill. X-ray powder diffraction patterns of those ground samples showed almost halo patterns. The nicardipine hydrochloride content on the surface of the tablet was determined based on the absorbance at 1700 cm(-1) attributable to the C=O stretch vibration in FT-IR-RAS spectra before and after irradiation by fluorescent lamp (3500 lx). The photodegradation followed apparently the first-order kinetics for any sample. The apparent photodegradation rate constant of beta-form was greater than that of alpha-form. The ground samples decomposed rapidly under the same light irradiation as compared with the intact crystalline forms. The photodegradation rate constant decreased with increase of the heat of fusion. copyright 2004 Elsevier B.V.
Facile green synthesis of fluorescent N-doped carbon dots from Actinidia deliciosa and their catalytic activity and cytotoxicity applications

NASA Astrophysics Data System (ADS)

Arul, Velusamy; Sethuraman, Mathur Gopalakrishnan

2018-04-01

Green synthesis of fluorescent nitrogen doped carbon dots (N-CDs) using Actinidia deliciosa (A. deliciosa) fruit extract as a carbon precursor and aqueous ammonia as a nitrogen dopant is reported here. The synthesized N-CDs were characterized by high resolution transmission electron microscopy (HR-TEM), energy dispersive spectroscopy (EDS), selected area electron diffraction (SAED), UV-Visible spectroscopy (UV-Vis), fluorescence spectroscopy, Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), Raman spectroscopy and X-ray photoelectron spectroscopy (XPS). The average size of the N-CDs was approximately 3.59 nm and the calculated inter layer distance was found to be 0.21 nm. Raman spectroscopy and SAED pattern revealed the graphitic nature of the synthesized N-CDs. The N-CDs were found to emit intense blue color at 405 nm under the excitation of 315 nm. The doping of nitrogen over the surface of the N-CDs was confirmed by EDS, FT-IR and XPS studies. The synthesized N-CDs were found to exhibit excellent catalytic activity in the reduction of Rhodamine-B using sodium borohydrate. The MTT assay was used to evaluate the cytotoxicity and biocompatibility of N-CDs towards L-929 and MCF-7 cells. From the results obtained, it was found that the N-CDs exhibit low cytotoxicity and superior biocompatibility on both L-929 and MCF-7 cells.
Synthesis and optical properties of polycrystalline Li2Al2B2O7 (LABO)

NASA Astrophysics Data System (ADS)

Dagdale, S. R.; Muley, G. G.

2016-05-01

A polycrystalline lithium aluminum borate (Li2Al2B2O7, LABO) has been synthesized by using simple solid-state technique. The obtained LABO polycrystalline was characterized by powder X-ray diffraction; Fourier transform infrared (FT-IR) spectroscopy and second harmonic generation (SHG) efficiency measurement. The functional groups were identified using the FT-IR spectroscopic data. The SHG efficiency of the polycrystalline material was obtained by the classic Kurtz powder technique using a fundamental wavelength 1064 nm of Nd:YAG laser and it is found to be 1.4 times that of potassium dihydrogen phosphate (KDP).
A validated Fourier transform infrared spectroscopy method for quantification of total lactones in Inula racemosa and Andrographis paniculata.

PubMed

Shivali, Garg; Praful, Lahorkar; Vijay, Gadgil

2012-01-01

Fourier transform infrared (FT-IR) spectroscopy is a technique widely used for detection and quantification of various chemical moieties. This paper describes the use of the FT-IR spectroscopy technique for the quantification of total lactones present in Inula racemosa and Andrographis paniculata. To validate the FT-IR spectroscopy method for quantification of total lactones in I. racemosa and A. paniculata. Dried and powdered I. racemosa roots and A. paniculata plant were extracted with ethanol and dried to remove ethanol completely. The ethanol extract was analysed in a KBr pellet by FT-IR spectroscopy. The FT-IR spectroscopy method was validated and compared with a known spectrophotometric method for quantification of lactones in A. paniculata. By FT-IR spectroscopy, the amount of total lactones was found to be 2.12 ± 0.47% (n = 3) in I. racemosa and 8.65 ± 0.51% (n = 3) in A. paniculata. The method showed comparable results with a known spectrophotometric method used for quantification of such lactones: 8.42 ± 0.36% (n = 3) in A. paniculata. Limits of detection and quantification for isoallantolactone were 1 µg and 10 µg respectively; for andrographolide they were 1.5 µg and 15 µg respectively. Recoveries were over 98%, with good intra- and interday repeatability: RSD ≤ 2%. The FT-IR spectroscopy method proved linear, accurate, precise and specific, with low limits of detection and quantification, for estimation of total lactones, and is less tedious than the UV spectrophotometric method for the compounds tested. This validated FT-IR spectroscopy method is readily applicable for the quality control of I. racemosa and A. paniculata. Copyright © 2011 John Wiley & Sons, Ltd.
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.
Preparation of hydroxyapatite from animal bones.

PubMed

Sobczak, Agnieszka; Kowalski, Zygmunt; Wzorek, Zbigniew

2009-01-01

This paper presents the method of obtaining hydroxyapatite from animal bones. Bone sludge and calcined products were characterized by X-ray diffraction (XRD), Fourier transformed infrared spectroscopy (FT-IR) and scanning electron microscopy (SEM). Calcium concentration was determined with titration, and phosphorus--spectrophotometrically. Making use of the AAS and ICP methods the content of microelements was determined. In all the products, hydroxyapatite was the only crystalline phase indicated. The FT-IR spectra confirmed that calcination removed the total of organic substances. Calcium and phosphorus contents were 38% and 18%, respectively, which corresponded to the Ca/P molar ratio of nonstoichiometric hydroxyapatite. The specific surfaces of products were measured by BET method. The volume of micro- and mesopores was determined.
Detection of metanil yellow contamination in turmeric using FT-Raman and FT-IR spectroscopy

NASA Astrophysics Data System (ADS)

Dhakal, Sagar; Chao, Kuanglin; Qin, Jianwei; Kim, Moon; Schmidt, Walter; Chan, Dian

2016-05-01

Turmeric is well known for its medicinal value and is often used in Asian cuisine. Economically motivated contamination of turmeric by chemicals such as metanil yellow has been repeatedly reported. Although traditional technologies can detect such contaminants in food, high operational costs and operational complexities have limited their use to the laboratory. This study used Fourier Transform Raman Spectroscopy (FT-Raman) and Fourier Transform - Infrared Spectroscopy (FT-IR) to identify metanil yellow contamination in turmeric powder. Mixtures of metanil yellow in turmeric were prepared at concentrations of 30%, 25%, 20%, 15%, 10%, 5%, 1% and 0.01% (w/w). The FT-Raman and FT-IR spectral signal of pure turmeric powder, pure metanil yellow powder and the 8 sample mixtures were obtained and analyzed independently to identify metanil yellow contamination in turmeric. The results show that FT-Raman spectroscopy and FT-IR spectroscopy can detect metanil yellow mixed with turmeric at concentrations as low as 1% and 5%, respectively, and may be useful for non-destructive detection of adulterated turmeric powder.
Green synthesis of gold nanoparticles using Stevia rebaudiana leaf extracts: Characterization and their stability.

PubMed

Sadeghi, Babak; Mohammadzadeh, M; Babakhani, B

2015-07-01

Various methods invented and developed for the synthesis of gold nanoparticles that increases daily consumed. According to this method, including potential environmental pollution problems and the complexity of the synthesis, in this study, the feasibility of using the leaves extract of Stevia rebaudiana (SR) for the reduction of gold ions to nanoparticles form have been studied. Stevia leaves were used to prepare the aqueous extract for this study. Gold nanoparticles were characterized with different techniques such as UV-vis spectroscopy, FT-IR spectroscopy, X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). Transmission electron microscopy experiments showed that these nanoparticles are spherical and uniformly distributed and its size is from 5 to 20 nm. FT-IR spectroscopy revealed that gold nanoparticles were functionalized with biomolecules that have primary amine group (NH2), carbonyl group, OH groups and other stabilizing functional groups. X-ray diffraction pattern showed high purity and face centered cubic structure of gold nanoparticles with size of 17 nm. The scanning electron microscopy (SEM) implies the right of forming gold nanoparticles. The results, confirm that gold nanoparticles have synthesized by the leaves extract of S. rebaudiana (SR). Copyright © 2015 Elsevier B.V. All rights reserved.

Topics in Chemical Instrumentation: Fourier Transform-Infrared Spectroscopy: Part I. Instrumentation.

ERIC Educational Resources Information Center

Perkins, W. D.

1986-01-01

Discusses: (1) the design of the Fourier Transform-Infrared Spectroscopy (FT-IR) spectrometer; (2) the computation of the spectrum from the interferogram; and (3) the use of apodization. (Part II will discuss advantages of FT-IR over dispersive techniques and show applications of FT-IR to difficult spectroscopic measurements.) (JN)
FT-IR and Zeta potential measurements on TiO nanoparticles

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

Singh, Jaiveer; Rathore, Ravi; Kaurav, Netram, E-mail: netramkaurav@yahoo.co.uk

2016-05-23

In the present investigation, ultrafine TiO particles have been synthesized successfully by thermal decomposition method. The sample was characterized by X-ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy. As-synthesized TiO nanoparticles have a cubic structure as characterized by power X-ray diffraction (XRD), which shows that TiO nanoparticles have narrow size distribution with particle size 11.5 nm. FTIR data shows a strong peak at 1300 cm{sup −1}, assignable to the Ti-O stretching vibrations mode.
A novel method for the elaboration of hydroxyapatite with high purity by sol-gel using the albumin and comparison with the classical methods

NASA Astrophysics Data System (ADS)

Mohammed, Eddya; Bouazza, Tbib; Khalil, El-Hami

2018-02-01

In this paper, we report the first synthesis of hydroxyapatite (Hap) by sol-gel using the albumin (egg white) compared with the four classical elaboration methods such as co-precipitation, solid state, and solid-liquid samples of hydroxyapatite. We use a reference sample of hydroxyapatite bought from Fluka Chemika company (Lot and Filling code 385330/1 14599). All samples are characterized by X-ray diffraction (XRD), Uv-visible spectroscopy (Uv-Vis), and Fourier transforms infrared spectroscopy (FT-IR). The XRD study showed the existence of a Hexagonal phase for all our samples prepared in our laboratory and an orthorhombic phase for the Fulka Chemika sample of Hap (Lot and Filling code 385330/1 14599). The study by Uv-visible spectroscopy was performed to determine and compare the optical gap and the disorder of each sample of Hap. The FT-IR spectroscopy demonstrated that all our Hap samples had a similar mode of vibration of the chemical bonds (OH-) and (PO4)3-.
Detection of starch adulteration in onion powder by FT-NIR and FT-IR spectroscopy

USDA-ARS?s Scientific Manuscript database

Adulteration of onion powder with cornstarch was identified by Fourier transform near-infrared (FT-NIR) and Fourier transform infrared (FT-IR) spectroscopy. The reflectance spectra of 180 pure and adulterated samples (1–35 wt% starch) were collected and preprocessed to generate calibration and predi...
Some critical aspects of FT-IR, TGA, powder XRD, EDAX and SEM studies of calcium oxalate urinary calculi.

PubMed

Joshi, Vimal S; Vasant, Sonal R; Bhatt, J G; Joshi, Mihir J

2014-06-01

Urinary calculi constitute one of the oldest afflictions of humans as well as animals, which are occurring globally. The calculi vary in shape, size and composition, which influence their clinical course. They are usually of the mixed-type with varying percentages of the ingredients. In medical management of urinary calculi, either the nature of calculi is to be known or the exact composition of calculi is required. In the present study, two selected calculi were recovered after surgery from two different patients for detailed examination and investigated by using Fourier-Transform infrared spectroscopy (FT-IR), thermo-gravimetric analysis (TGA), powder X-ray diffraction (XRD), scanning electron microscopy and energy dispersive analysis of X-rays (EDAX) techniques. The study demonstrated that the nature of urinary calculi and presence of major phase in mixed calculi could be identified by FT-IR, TGA and powder XRD, however, the exact content of various elements could be found by EDAX only.
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.
Green synthesis of nitrogen-doped graphitic carbon sheets with use of Prunus persica for supercapacitor applications

NASA Astrophysics Data System (ADS)

Atchudan, Raji; Edison, Thomas Nesakumar Jebakumar Immanuel; Perumal, Suguna; Lee, Yong Rok

2017-01-01

Nitrogen-doped graphitic carbon sheets (N-GCSs) were prepared from the extract of unripe Prunus persica fruit by a direct hydrothermal method. The synthesized N-GCSs were examined by high resolution transmission electron microscopy (HRTEM), nitrogen adsorption-desorption isotherms, X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), and Fourier transform infrared (FT-IR) spectroscopy. HRTEM showed that the synthesized carbon sheets were graphitic with lattice fringes and an inter-layer distance of 0.36 nm. Doping with the nitrogen moiety present over the synthesized GCSs was confirmed by XPS, FT-IR spectroscopy, and energy dispersive X-ray spectroscopy elemental mapping. The fruit extract associated with hydrothermal-carbonization method is economical and eco-friendly with a single step process. The resulting carbon sheets could be modified and are promising candidates for nano-electronic applications, including supercapacitors. The synthesized N-GCSs-2 provided a high specific capacitance of 176 F g-1 at a current density of 0.1 A g-1. This electrode material has excellent cyclic stability, even after 2000 cycles of charge-discharge at a current density of 0.5 A g-1.
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, 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.
Effect of microwave treatment on structure of binders based on sodium carboxymethyl starch: FT-IR, FT-Raman and XRD investigations

NASA Astrophysics Data System (ADS)

Kaczmarska, Karolina; Grabowska, Beata; Spychaj, Tadeusz; Zdanowicz, Magdalena; Sitarz, Maciej; Bobrowski, Artur; Cukrowicz, Sylwia

2018-06-01

The paper deals with the influence of the microwave treatment on sodium carboxymethyl starch (CMS-Na) applied as a binder for moulding sands. The Fourier transformation infrared spectrometry (FT-IR), Raman spectroscopy (FT-Raman) and XRD analysis data of native potato starch and three different carboxymethyl starches (CMS-Na) with various degree of substitution (DS) before and after exposition to microwave radiation have been compared. FT-IR studies showed that polar groups present in CMS-Na structure take part in the formation of new hydrogen bonds network after water evaporation. However, these changes depend on DS value of the modified starch. The FT-Raman study confirmed that due to the impact on the samples by microwave, the changes of intensity in the characteristic bands associated with the crystalline regions in the sample were noticed. The X-ray diffraction data for microwave treated CMS-Na samples have been compared with the diffractograms of initial materials and analysis of XRD patterns confirmed that microwave-treated samples exhibit completely amorphous structure. Analysis of structural changes allows to state that the binding of sand grains in moulding sand with CMS-Na polymeric binder consists in the formation of hydrogen bonds networks (physical cross-linking).
Effect of microwave treatment on structure of binders based on sodium carboxymethyl starch: FT-IR, FT-Raman and XRD investigations.

PubMed

Kaczmarska, Karolina; Grabowska, Beata; Spychaj, Tadeusz; Zdanowicz, Magdalena; Sitarz, Maciej; Bobrowski, Artur; Cukrowicz, Sylwia

2018-06-15

The paper deals with the influence of the microwave treatment on sodium carboxymethyl starch (CMS-Na) applied as a binder for moulding sands. The Fourier transformation infrared spectrometry (FT-IR), Raman spectroscopy (FT-Raman) and XRD analysis data of native potato starch and three different carboxymethyl starches (CMS-Na) with various degree of substitution (DS) before and after exposition to microwave radiation have been compared. FT-IR studies showed that polar groups present in CMS-Na structure take part in the formation of new hydrogen bonds network after water evaporation. However, these changes depend on DS value of the modified starch. The FT-Raman study confirmed that due to the impact on the samples by microwave, the changes of intensity in the characteristic bands associated with the crystalline regions in the sample were noticed. The X-ray diffraction data for microwave treated CMS-Na samples have been compared with the diffractograms of initial materials and analysis of XRD patterns confirmed that microwave-treated samples exhibit completely amorphous structure. Analysis of structural changes allows to state that the binding of sand grains in moulding sand with CMS-Na polymeric binder consists in the formation of hydrogen bonds networks (physical cross-linking). Copyright © 2018 Elsevier B.V. All rights reserved.
Broadband near-field infrared spectromicroscopy using photothermal probes and synchrotron radiation.

PubMed

Donaldson, Paul M; Kelley, Chris S; Frogley, Mark D; Filik, Jacob; Wehbe, Katia; Cinque, Gianfelice

2016-02-08

In this paper, we experimentally demonstrate the use of infrared synchrotron radiation (IR-SR) as a broadband source for photothermal near-field infrared spectroscopy. We assess two methods of signal transduction; cantilever resonant thermal expansion and scanning thermal microscopy. By means of rapid mechanical chopping (50-150 kHz), we modulate the IR-SR at rates matching the contact resonance frequencies of atomic force microscope (AFM) cantilevers, allowing us to record interferograms yielding Fourier transform infrared (FT-IR) photothermal absorption spectra of polystyrene and cyanoacrylate films. Complementary offline measurements using a mechanically chopped CW IR laser confirmed that the resonant thermal expansion IR-SR measurements were below the diffraction limit, with a spatial resolution better than 500 nm achieved at a wavelength of 6 μm, i.e. λ/12 for the samples studied. Despite achieving the highest signal to noise so far for a scanning thermal microscopy measurement under conditions approaching near-field (dictated by thermal diffusion), the IR-SR resonant photothermal expansion FT-IR spectra measured were significantly higher in signal to noise in comparison with the scanning thermal data.
Green Synthesis of Magnetite (Fe3O4) Nanoparticles Using Seaweed ( Kappaphycus alvarezii) Extract

NASA Astrophysics Data System (ADS)

Yew, Yen Pin; Shameli, Kamyar; Miyake, Mikio; Kuwano, Noriyuki; Bt Ahmad Khairudin, Nurul Bahiyah; Bt Mohamad, Shaza Eva; Lee, Kar Xin

2016-06-01

In this study, a simple, rapid, and eco-friendly green method was introduced to synthesize magnetite nanoparticles (Fe3O4-NPs) successfully. Seaweed Kappaphycus alvarezii ( K. alvarezii) was employed as a green reducing and stabilizing agents. The synthesized Fe3O4-NPs were characterized with X-ray diffraction (XRD), ultraviolet-visible spectroscopy (UV-Vis), Fourier transform infrared (FT-IR), and transmission electron microscopy (TEM) techniques. The X-ray diffraction planes at (220), (311), (400), (422), (511), (440), and (533) were corresponding to the standard Fe3O4 patterns, which showed the high purity and crystallinity of Fe3O4-NPs had been synthesized. Based on FT-IR analysis, two characteristic absorption peaks were observed at 556 and 423 cm-1, which proved the existence of Fe3O4 in the prepared nanoparticles. TEM image displayed the synthesized Fe3O4-NPs were mostly in spherical shape with an average size of 14.7 nm.
Green Synthesis of Magnetite (Fe3O4) Nanoparticles Using Seaweed (Kappaphycus alvarezii) Extract.

PubMed

Yew, Yen Pin; Shameli, Kamyar; Miyake, Mikio; Kuwano, Noriyuki; Bt Ahmad Khairudin, Nurul Bahiyah; Bt Mohamad, Shaza Eva; Lee, Kar Xin

2016-12-01

In this study, a simple, rapid, and eco-friendly green method was introduced to synthesize magnetite nanoparticles (Fe3O4-NPs) successfully. Seaweed Kappaphycus alvarezii (K. alvarezii) was employed as a green reducing and stabilizing agents. The synthesized Fe3O4-NPs were characterized with X-ray diffraction (XRD), ultraviolet-visible spectroscopy (UV-Vis), Fourier transform infrared (FT-IR), and transmission electron microscopy (TEM) techniques. The X-ray diffraction planes at (220), (311), (400), (422), (511), (440), and (533) were corresponding to the standard Fe3O4 patterns, which showed the high purity and crystallinity of Fe3O4-NPs had been synthesized. Based on FT-IR analysis, two characteristic absorption peaks were observed at 556 and 423 cm(-1), which proved the existence of Fe3O4 in the prepared nanoparticles. TEM image displayed the synthesized Fe3O4-NPs were mostly in spherical shape with an average size of 14.7 nm.
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).
Collaborative Student Laboratory Exercise Using FT-IR Spectroscopy for the Kinetics Study of a Biotin Analogue

ERIC Educational Resources Information Center

Leong, Jhaque; Ackroyd, Nathan C.; Ho, Karen

2014-01-01

The synthesis of N-methoxycarbonyl-2-imidazolidone, an analogue of biotin, was conducted by organic chemistry students and confirmed using FT-IR and H NMR. Spectroscopy students used FT-IR to measure the rate of hydrolysis of the product and determined the rate constant for the reaction using the integrated rate law. From the magnitude of the rate…
Rapid and automatic chemical identification of the medicinal flower buds of Lonicera plants by the benchtop and hand-held Fourier transform infrared spectroscopy

NASA Astrophysics Data System (ADS)

Chen, Jianbo; Guo, Baolin; Yan, Rui; Sun, Suqin; Zhou, Qun

2017-07-01

With the utilization of the hand-held equipment, Fourier transform infrared (FT-IR) spectroscopy is a promising analytical technique to minimize the time cost for the chemical identification of herbal materials. This research examines the feasibility of the hand-held FT-IR spectrometer for the on-site testing of herbal materials, using Lonicerae Japonicae Flos (LJF) and Lonicerae Flos (LF) as examples. Correlation-based linear discriminant models for LJF and LF are established based on the benchtop and hand-held FT-IR instruments. The benchtop FT-IR models can exactly recognize all articles of LJF and LF. Although a few LF articles are misjudged at the sub-class level, the hand-held FT-IR models are able to exactly discriminate LJF and LF. As a direct and label-free analytical technique, FT-IR spectroscopy has great potential in the rapid and automatic chemical identification of herbal materials either in laboratories or in fields. This is helpful to prevent the spread and use of adulterated herbal materials in time.
TiO2 nanoparticles versus TiO2-SiO2 nanocomposites: A comparative study of photo catalysis on acid red 88

NASA Astrophysics Data System (ADS)

Balachandran, K.; Venckatesh, Rajendran; Sivaraj, Rajeshwari; Rajiv, P.

2014-07-01

A novel, simple, less time-consuming and cost-effective wet chemical technique was used to synthesis TiO2 nanoparticles and TiO2-SiO2 nanocomposites using Titanium tetra isopropoxide (TTIP) as a precursor relatively at low temperature in acidic pH. Titania sol was prepared by hydrolysis of TTIP and was mixed with silicic acid and tetrahydrofuran mixture. The reaction was carried out under vigorous stirring for 6 h and dried at room temperature. The resulting powders were characterized by UV-Visible spectroscopy, Fourier transform infrared (FT-IR), X-ray diffraction, scanning electron microscope (SEM) and transmission electron microscope (TEM). The grain size of the particles was calculated by X-ray diffraction, surface morphology and chemical composition was determined from scanning electron microscopy-energy dispersive spectroscopy, metal oxide stretching was confirmed from FT-IR spectroscopy, band gap was calculated using UV-Visible spectroscopy. Surface area of the composite as calculated by BET analyzer and it was found to be 65 and 75 m2/g for TiO2 and TiO2-SiO2 respectively. The photocatalytic experiments were performed with aqueous solution of acid red 88 with TiO2 and TiO2-SiO2 batch studies for 4 h irradiation, direct photolysis of TiO2 and TiO2-SiO2 contributed 94.2% and 96.5% decomposition in solar radiation for the optimized concentration of acid red 88.
Effects on structural, optical, and magnetic properties of pure and Sr-substituted MgFe2O4 nanoparticles at different calcination temperatures

NASA Astrophysics Data System (ADS)

Loganathan, A.; Kumar, K.

2016-06-01

In the present work, pure and Sr2+ ions substituted Mg ferrite nanoparticles (NPs) had been prepared by co-precipitation method and their structural, optical, and magnetic properties at different calcination temperatures were studied. On this purpose, thermo gravimetric and differential thermal analysis (TG-DTA), Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), scanning electron microscopy, UV-Visible diffused reflectance spectroscopy, impedance spectroscopy, and vibrating sample magnetometer were carried out. The exo- and endothermic processes of synthesized precursors were investigated by TG-DTA measurements. The structural properties of the obtained products were examined by XRD analysis and show that the synthesized NPs are in the cubic spinel structure. The existence of two bands around 578-583 and 430-436 cm-1 in FT-IR spectrum also confirmed the formation of spinel-structured ferrite NPs. The lattice constants and particle size are estimated using XRD data and found to be strongly dependent on calcination temperatures. The optical, electrical, and magnetic properties of ferrite compositions also investigated and found to be strongly dependant on calcination temperatures.
Synthesis and characterization of fluorapatite-titania (FAp-TiO 2) nanocomposite via mechanochemical process

NASA Astrophysics Data System (ADS)

Ebrahimi-Kahrizsangi, Reza; Nasiri-Tabrizi, Bahman; Chami, Akbar

2010-09-01

In this paper, synthesis of bionanocomposite of fluorapatite-titania (FAp-TiO 2) was studied by using one step mechanochemical process. Characterization of the products was accomplished by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, energy dispersive X-ray spectroscopy (EDX), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) techniques. Based on XRD patterns and FT-IR spectroscopy, correlation between the structural features of the nanostructured FAp-TiO 2 and the process conditions was discussed. Variations in crystallite size, lattice strain, and volume fraction of grain boundary were investigated during milling and the following heat treatment. Crystallization of the nanocomposite occurred after thermal treatment at 650 °C. Morphological features of powders were influenced by the milling time. The resulting FAp-20 wt.%TiO 2 nanocomposite powder exhibited an average particle size of 15 nm after 20 h of milling. The results show that the one step mechanosynthesis technique is an effective route to prepare FAp-based nanocomposites with excellent morphological and structural features.

Mulberry leaf extract mediated synthesis of gold nanoparticles and its anti-bacterial activity against human pathogens

NASA Astrophysics Data System (ADS)

Adavallan, K.; Krishnakumar, N.

2014-06-01

Gold nanoparticles (Au-NPs) were synthesized at room temperature using Morus alba (mulberry) leaf extract as reducing and stabilizing agent. The development of plant mediated synthesis of nanoparticles is gaining importance due to its simplicity, low cost, non-toxicity, eco-friendliness, long term stability and reproducible aqueous synthesis method to obtain a self-assembly of nearly monodispersed Au-NPs. The formation and morphology of biosynthesized nanoparticles are investigated with the help of UV-Vis spectroscopy, dynamic light scattering (DLS), transmission electron microscopy (TEM), atomic force microscopy (AFM), x-ray diffraction (XRD), and Fourier transform infrared spectroscopy (FT-IR) techniques. Au-NPs formation was screened by UV-Vis spectroscopy through color conversion due to surface plasmon resonance band at 538 nm for Au-NPs. DLS studies revealed that the average size of Au-NPs was 50 nm. TEM studies showed the particles to be nearly spherical with few irregular shapes and particle size ranges 15-53 nm. The AFM image clearly shows the surface morphology of the well-dispersed Au-NPs with less than 50 nm. The high crystallinity of nanoparticles is evident from bright circular spots in the selected area electron diffraction (SAED) pattern. X-ray diffraction pattern showed high purity and face-centered cubic structure of Au-NPs. The FT-IR results indicate the presence of different functional groups present in the biomolecule capping the nanoparticles. Further, biosynthesized Au-NPs show strong zone of inhibition against Vibrio cholera (gram-negative) and Staphylococcus aureus (gram-positive) whereas, chemically synthesized Au-NPs and mulberry leaf extract exhibit a fair zone of inhibition.
Super-resolved FT-IR spectroscopy: Strategies, challenges, and opportunities for membrane biophysics.

PubMed

Li, Jessica J; Yip, Christopher M

2013-10-01

Direct correlation of molecular conformation with local structure is critical to studies of protein- and peptide-membrane interactions, particularly in the context of membrane-facilitated aggregation, and disruption or disordering. Infrared spectroscopy has long been a mainstay for determining molecular conformation, following folding dynamics, and characterizing reactions. While tremendous advances have been made in improving the spectral and temporal resolution of infrared spectroscopy, it has only been with the introduction of scanned-probe techniques that exploit the raster-scanning tip as either a source, scattering tool, or measurement probe that researchers have been able to obtain sub-diffraction limit IR spectra. This review will examine the history of correlated scanned-probe IR spectroscopies, from their inception to their use in studies of molecular aggregates, membrane domains, and cellular structures. The challenges and opportunities that these platforms present for examining dynamic phenomena will be discussed. This article is part of a Special Issue entitled: FTIR in membrane proteins and peptide studies. Copyright © 2013 Elsevier B.V. All rights reserved.
Efficient synthesis of highly fluorescent nitrogen-doped carbon dots for cell imaging using unripe fruit extract of Prunus mume

NASA Astrophysics Data System (ADS)

Atchudan, Raji; Edison, Thomas Nesakumar Jebakumar Immanuel; Sethuraman, Mathur Gopalakrishnan; Lee, Yong Rok

2016-10-01

Highly fluorescent nitrogen-doped carbon dots (N-CDs) were synthesized using the extract of unripe Prunus mume (P. mume) fruit by a simple one step hydrothermal-carbonization method. The N-CDs were synthesized at different pH ranges, 2.3, 5, 7, and 9. The pH of the P. mume extract was adjusted using an aqueous ammonia solution (25%). The optical properties of N-CDs were examined by UV-vis and fluorescence spectroscopy. The N-CDs synthesized at pH 9 emitted high fluorescence intensity compared to other obtained N-CDs. The N-CDs synthesized at pH 9 was further characterized by high resolution transmission electron microscopy (HR-TEM), X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), and Fourier transform-infra red (FT-IR) spectroscopy. HR-TEM showed that the average size of the synthesized N-CDs was approximately 9 nm and the interlayer distance was 0.21 nm, which was validated by XRD. The graphitic nature of the synthesized N-CDs were confirmed by Raman spectroscopy. XPS and FT-IR spectroscopy confirmed the doping of the nitrogen moiety over the synthesized CDs. The synthesized nitrogen doped CDs (N-CDs) were low toxicity and were used as a staining probe for fluorescence cell imaging.
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.
Eco-friendly and green synthesis of BiVO4 nanoparticle using microwave irradiation as photocatalayst for the degradation of Alizarin Red S

NASA Astrophysics Data System (ADS)

Abraham, S. Daniel; David, S. Theodore; Bennie, R. Biju; Joel, C.; Kumar, D. Sanjay

2016-06-01

Bismuth vanadate (BiVO4) nanocrystals have been successfully synthesised using microwave-assisted combustion synthesis (MCS), and characterised using Fourier transform infrared (FT-IR) and Raman spectra, surface area analysis (BET), X-ray diffraction (XRD), scanning electron microscopy (SEM), Energy Dispersive X-ray analysis (EDX), diffused reflectance spectroscopy (DRS) and Photoluminescence (PL) spectroscopy. The XRD results confirmed the formation of monoclinic bismuth vanadate. The formations of BiO & VO43-vibrations were ascertained from FT-IR data. The morphology of hallow internal structural micro entities were confirmed by SEM. The optical properties were determined by DRS and PL spectra. Hence, the influence of the preparation methods on the structure, morphology and optical activities of bismuth vanadate was investigated systematically. Photocatalytic degradation (PCD) of Alizarin Red S (ARS), an effective disrupting chemical in aqueous medium was investigated using BiVO4 nanoparticles. The kinetics of PCD was found to follow pseudo first-order.
Micro-Raman and FT-IR spectroscopic studies of ceramic shards excavated from ancient Stratonikeia city at Eskihisar village in West-South Turkey

NASA Astrophysics Data System (ADS)

Bahçeli, Semiha; Güleç, Gamze; Erdoğan, Hasan; Söğüt, Bilal

2016-02-01

In this study, micro-Raman and Fourier transformed infrared (FT-IR) spectroscopies, X-ray diffraction (XRD) and scanning electron microscope with energy dispersive X-ray (SEM-EDX) were used to characterize the mineralogical structures of pigments of four ceramic fragments in which one of them belongs to Hellenistic period (1st - IVth century BC) and other three ceramic shards belong to Early Rome (IVth century BC- 1st century AD) excavated from Stratonikeia ancient city. In the results of investigations on these four ceramic fragments, the various phases were identified: quartz, kaolinite, albit (or Na-feldspar), calcite, anastase, hematite and magnetite. Furthermore, the obtained findings indicate that firing temperature is about 800-850 °C for all the shards.
A study on the stability and green synthesis of silver nanoparticles using Ziziphora tenuior (Zt) extract at room temperature.

PubMed

Sadeghi, Babak; Gholamhoseinpoor, F

2015-01-05

Biomolecules present in plant extracts can be used to reduce metal ions to nanoparticles in a single-step green synthesis process. This biogenic reduction of metal ion to base metal is quite rapid, readily conducted at room temperature and pressure, and easily scaled up. Mediated Synthesis by plant extracts is environmentally benign. The involved reducing agents include the various water soluble plant metabolites (e.g. alkaloids, phenolic compounds, terpenoids) and co-enzymes. Silver (Ag) nanoparticles have the particular focus of plant-based syntheses. Extracts of a diverse range of Ziziphora tenuior (Zt) have been successfully used in making nanoparticles. The aim of this study was to investigate the antioxidant properties of this plant and its ability to synthesize silver nanoparticles. Z.tenuior leaves were used to prepare the aqueous extract for this study. Silver nanoparticles were characterized with different techniques such as UV-vis spectroscopy, Fourier transform infrared (FT-IR) spectroscopy, X-ray diffraction (XRD), Scanning electron microscopy (SEM), and transmission electron microscopy (TEM). Transmission electron microscopy experiments showed that these nanoparticles are spherical and uniformly distributed and its size is from 8 to 40 nm. FT-IR spectroscopy revealed that silver nanoparticles were functionalized with biomolecules that have primary amine group (NH₂), carbonyl group, -OH groups and other stabilizing functional groups. X-ray diffraction pattern showed high purity and face centered cubic structure of silver nanoparticles with size of 38 nm. In addition to plant extracts, live plants can be used for the synthesis. Here were view the methods of making nanoparticles using plant extracts. The scanning electron microscopy (SEM) implies the right of forming silver nanoparticles. The results of TEM, SEM, FT-IR, UV-VIS and XRD confirm that the leaves extract of Zt can synthesis silver nanoparticles. Copyright © 2014 Elsevier B.V. All rights reserved.
A simple method to synthesize polyhedral hexagonal boron nitride nanofibers

NASA Astrophysics Data System (ADS)

Lin, Liang-xu; Zheng, Ying; Li, Zhao-hui; shen, Xiao-nv; Wei, Ke-mei

2007-12-01

Hexagonal boron nitride (h-BN) fibers with polyhedral morphology were synthesized with a simple-operational, large-scale and low-cost method. The sample obtained was studied by X-ray photoelectron spectrometer (XPS), electron energy lose spectroscopy (EELS), X-ray powder diffraction (XRD), Fourier transformation infrared spectroscopy (FT-IR), etc., which matched with h-BN. Environment scanning electron microscopy (ESEM) and transmission electron microscope (TEM) indicated that the BN fibers possess polyhedral morphology. The diameter of the BN fibers is mainly in the range of 100-500 nm.
Structure and thermal decomposition of sulfated β-cyclodextrin intercalated in a layered double hydroxide

NASA Astrophysics Data System (ADS)

Wang, Ji; Wei, Min; Rao, Guoying; Evans, David G.; Duan, Xue

2004-01-01

The sodium salt of hexasulfated β-cyclodextrin has been synthesized and intercalated into a magnesium-aluminum layered double hydroxide by ion exchange. The structure, composition and thermal decomposition behavior of the intercalated material have been studied by variable temperature X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), inductively coupled plasma emission spectroscopy (ICP), and thermal analysis (TG-DTA) and a model for the structure has been proposed. The thermal stability of the intercalated sulfated β-cyclodextrin is significantly enhanced compared with the pure form before intercalation.
Coriandrum sativum mediated synthesis of silver nanoparticles and evaluation of their biological characteristics

NASA Astrophysics Data System (ADS)

Senthilkumar, N.; Aravindhan, V.; Ruckmani, K.; Vetha Potheher, I.

2018-05-01

Silver (Ag) nanoparticles (NPs) were prepared by percolated green synthesis method using Coriandrum sativum leaf, root, seed and stem extracts and reported its antibacterial activity. The synthesized Ag NPs were confirmed by UV–visible Spectroscopy, Powder x-ray Diffraction (PXRD), Fourier Transform Infra Red (FT-IR) Spectroscopy analyzes. The Maximum absorbance observed around 400–450 nm reveal the characteristic absorbance of Ag NPs. The Dynamic Light Scattering (DLS) analysis shows the stability of synthesized NPs with average size varying from 35 to 53 nm and also zeta potential stability varying from ‑20 to ‑30 mV. The cubic structure, crystalline nature and purity of the material was confirmed by powder x-ray diffraction studies. FT-IR spectrum shows the presence of various functional groups in the resultant material. The Field Emission Scanning Electron Microscopy (FESEM) image shows the surface morphology of the synthesized NPs and the Energy Dispersive x-ray Analysis (EDAX) confirms the presence of silver metal ions. The Coriandrum sativum aqueous extract exhibited excellent antimicrobial activity against Klebsiella pneumoniae (Gram -ve) bacteria. Numerous studies have been made previously in our field of study but optimization has not been carried out by both extract (different parts like leaf, root, seed and stem) and without addition of any external source such as chemicals, heat etc.
Application of Fourier transform infrared (FT-IR) spectroscopy in determination of microalgal compositions.

PubMed

Meng, Yingying; Yao, Changhong; Xue, Song; Yang, Haibo

2014-01-01

Fourier transform infrared spectroscopy (FT-IR) was applied in algal strain screening and monitoring cell composition dynamics in a marine microalga Isochrysis zhangjiangensis during algal cultivation. The content of lipid, carbohydrate and protein of samples determined by traditional methods had validated the accuracy of FT-IR method. For algal screening, the band absorption ratios of lipid/amide I and carbo/amide I from FT-IR measurements allowed for the selection of Isochrysis sp. and Tetraselmis subcordiformis as the most potential lipid and carbohydrate producers, respectively. The cell composition dynamics of I. zhangjiangensis measured by FT-IR revealed the diversion of carbon allocation from protein to carbohydrate and neutral lipid when nitrogen-replete cells were subjected to nitrogen limitation. The carbo/amide I band absorption ratio had also been demonstrated to depict physiological status under nutrient stress in T. subcordiformis. FT-IR serves as a tool for the simultaneous measurement of lipid, carbohydrate, and protein content in cell. Copyright © 2013 Elsevier Ltd. All rights reserved.
TiO2 nanoparticles versus TiO2-SiO2 nanocomposites: a comparative study of photo catalysis on acid red 88.

PubMed

Balachandran, K; Venckatesh, Rajendran; Sivaraj, Rajeshwari; Rajiv, P

2014-07-15

A novel, simple, less time-consuming and cost-effective wet chemical technique was used to synthesis TiO2 nanoparticles and TiO2-SiO2 nanocomposites using Titanium tetra isopropoxide (TTIP) as a precursor relatively at low temperature in acidic pH. Titania sol was prepared by hydrolysis of TTIP and was mixed with silicic acid and tetrahydrofuran mixture. The reaction was carried out under vigorous stirring for 6h and dried at room temperature. The resulting powders were characterized by UV-Visible spectroscopy, Fourier transform infrared (FT-IR), X-ray diffraction, scanning electron microscope (SEM) and transmission electron microscope (TEM). The grain size of the particles was calculated by X-ray diffraction, surface morphology and chemical composition was determined from scanning electron microscopy-energy dispersive spectroscopy, metal oxide stretching was confirmed from FT-IR spectroscopy, band gap was calculated using UV-Visible spectroscopy. Surface area of the composite as calculated by BET analyzer and it was found to be 65 and 75 m(2)/g for TiO2 and TiO2-SiO2 respectively. The photocatalytic experiments were performed with aqueous solution of acid red 88 with TiO2 and TiO2-SiO2 batch studies for 4h irradiation, direct photolysis of TiO2 and TiO2-SiO2 contributed 94.2% and 96.5% decomposition in solar radiation for the optimized concentration of acid red 88. Copyright © 2014 Elsevier B.V. All rights reserved.
A novel method for the functionalization of aminoacids L-glycine, L-glutamic acid and L-arginine on maghemite/magnetite nanoparticles

NASA Astrophysics Data System (ADS)

Bruno, A. J.; Correa, J. R.; Peláez-Abellán, E.; Urones-Garrote, E.

2018-06-01

Nanoparticles of maghemite/magnetite functionalized with L-glycine, L-glutamic acid and L-arginine were synthesized by a novel method. The novel procedure consists in an alternative of that reported by Massart for the precipitation of magnetite in which the aminoacid is added in the carboxylate form. The amounts of aminoacid in the initial molar concentrations were 35%, 45% and 65% with respect to the ferrophase. The obtained nanoparticles were characterized by several techniques: X-ray diffraction (XRD), Fourier transform IR spectroscopy (FT-IR), transmission electron microscopy (TEM), Electron energy-loss spectroscopy (EELS) and magnetometry. The IR spectroscopy confirmed that the selected aminoacids were functionalized on the surface of iron oxide. XRD and EELS confirm that iron oxide consists of a maghemite-magnetite intermediate phase with an average particle size about 6 nm, which was measured by transmission electron microscopy. The superparamagnetic character of the nanoparticles was evaluated by magnetometry.
Green synthesis of silver nanoparticles using marine algae Caulerpa racemosa and their antibacterial activity against some human pathogens

NASA Astrophysics Data System (ADS)

Kathiraven, T.; Sundaramanickam, A.; Shanmugam, N.; Balasubramanian, T.

2015-04-01

We present the synthesis and antibacterial activity of silver nanoparticles using Caulerpa racemosa, a marine algae. Fresh C. racemosa was collected from the Gulf of Mannar, Southeast coast of India. The seaweed extract was used for the synthesis of AgNO3 at room temperature. UV-visible spectrometry study revealed surface plasmon resonance at 413 nm. The characterization of silver nanoparticle was carried out using Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD) and transmission electron microscope (TEM). FT-IR measurements revealed the possible functional groups responsible for reduction and stabilization of the nanoparticles. X-ray diffraction analysis showed that the particles were crystalline in nature with face-centered cubic geometry.TEM micrograph has shown the formation of silver nanoparticles with the size in the range of 5-25 nm. The synthesized AgNPs have shown the best antibacterial activity against human pathogens such as Staphylococcus aureus and Proteus mirabilis. The above eco-friendly synthesis procedure of AgNPs could be easily scaled up in future for the industrial and therapeutic needs.
Synthesis and optical properties of Mg-Al layered double hydroxides precursor powders

NASA Astrophysics Data System (ADS)

Lin, Chia-Hsuan; Chu, Hsueh-Liang; Hwang, Weng-Sing; Wang, Moo-Chin; Ko, Horng-Huey

2017-12-01

The synthesis and optical properties of Mg-Al layered double hydroxide (LDH) precursor powders were investigated using X-ray diffraction (XRD), Fourier transform-infrared (FT-IR) spectroscopy, transmission electron microscopy (TEM), selected area electron diffraction (SAED), high-resolution TEM (HRTEM), UV-transmission spectrometer, and fluorescence spectrophotometer. The FT-IR results show that the intense absorption at around 1363-1377 cm-1 can be assigned to the antisymmetric ν3 mode of interlayer carbonate anions because the LDH phase contains some CO32-. The XRD results show that all of the Mg-Al LDH precursor powders contain only a single phase of [Mg0.833Al0.167(OH)2](CO3)0.083.(H2O)0.75 but have broad and weak intensities of peaks. All of Mg-Al LDHs precursor powders before calcination have the same photoluminescence (PL) spectra. Moreover, these spectra were excited at λex = 235 nm, and the broad emission band was in the range 325-650 nm. In the range, there were relatively strong intensity at around 360, 407 and 510 nm, respectively.
IDENTIFICATION OF BIS(2-CHLOROETHYL) ETHER HYDROLYSIS PRODUCTS BY DIRECT AQUEOUS INJECTION GC/FT-IR

EPA Science Inventory

Gas chromatography coupled to Fourier-transform infrared spectroscopy (GC/FT-IR) is rapidly becoming an accepted analytical technique complementary to GC/mass spectroscopy for identifying organic compounds in mixtures at low to moderate concentrations. irect aqueous injection (DA...
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.
Molecular orientation in aligned electrospun polyimide nanofibers by polarized FT-IR spectroscopy.

PubMed

Yang, Haoqi; Jiang, Shaohua; Fang, Hong; Hu, Xiaowu; Duan, Gaigai; Hou, Haoqing

2018-07-05

Quantitative explanation on the improved mechanical properties of aligned electrospun polyimide (PI) nanofibers as the increased imidization temperatures is highly required. In this work, polarized FT-IR spectroscopy is applied to solve this problem. Based on the polarized FT-IR spectroscopy and the molecular model in the fibers, the length of the repeat unit of PI molecule, the angle between the fiber axis and the symmetric stretching direction of carbonyl group on the imide ring, and the angle between the PI molecular axis and fiber axis are all investigated. The Mark-Howink equation is used to calculate the number-average molar mass of PI molecules. The orientation states of PI molecules in the electrospun nanofibers are studied from the number-average molar mass of PI molecules and the average fiber diameter. Quantitative analysis of the orientation factor of PI molecules in the electrospun nanofibers is performed by polarized FT-IR spectroscopy. Copyright © 2018 Elsevier B.V. All rights reserved.
Identification of different forms of cocaine and substances used in adulteration using near-infrared Raman spectroscopy and infrared absorption spectroscopy.

PubMed

Penido, Ciro A F O; Pacheco, Marcos Tadeu T; Zângaro, Renato A; Silveira, Landulfo

2015-01-01

Identification of cocaine and subsequent quantification immediately after seizure are problems for the police in developing countries such as Brazil. This work proposes a comparison between the Raman and FT-IR techniques as methods to identify cocaine, the adulterants used to increase volume, and possible degradation products in samples seized by the police. Near-infrared Raman spectra (785 nm excitation, 10 sec exposure time) and FT-IR-ATR spectra were obtained from different samples of street cocaine and some substances commonly used as adulterants. Freebase powder, hydrochloride powder, and crack rock can be distinguished by both Raman and FT-IR spectroscopies, revealing differences in their chemical structure. Most of the samples showed characteristic peaks of degradation products such as benzoylecgonine and benzoic acid, and some presented evidence of adulteration with aluminum sulfate and sodium carbonate. Raman spectroscopy is better than FT-IR for identifying benzoic acid and inorganic adulterants in cocaine. © 2014 American Academy of Forensic Sciences.
Preparation and Characterization of Polyurethanes with Cross-Linked Siloxane in the Side Chain by Sol-Gel Reactions

PubMed Central

Zhao, Hui; Hao, Tong-Hui; Hu, Guo-Hua; Shi, Dean; Huang, Da; Jiang, Tao; Zhang, Qun-Chao

2017-01-01

A series of novel polyurethanes containing cross-linked siloxane in the side chain (SPU) were successfully synthesized through a sol-gel process. The SPU was composed of 0%–20% N-(n-butyl)-3-aminopropyltriethoxysilane (HDI-T) modified hexamethylene diisocynate homopolymer. The effects of HDI-T content on both the structure and properties of SPU were investigated by Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), mechanical properties tests, gel content test, water contact angle measurement and water absorption test. FT-IR, XPS and XRD results confirmed the successful incorporation of HDI-T onto polyurethanes and the formation of Si–O–Si. The surface roughness and the Si content of SPU enhanced with the increase of HDI-T content. Both crystallization and melting temperature shifted to a lower point after the incorporation of HDI-T. The hydrophobicity, tensile strength, Young’s modulus and pencil hardness overall increased with the increasing of HDI-T content, whereas the thermal stability and the elongation at break of SPU slightly decreased. PMID:28772607

Synthesis and characterization of silver nanoparticles using crystal compound of sodium para-hydroxybenzoate tetrahydrate isolated from Vitex negundo. L leaves and its apoptotic effect on human colon cancer cell lines.

PubMed

Durai, Prabhu; Chinnasamy, Arulvasu; Gajendran, Babu; Ramar, Manikandan; Pappu, Srinivasan; Kasivelu, Govindaraju; Thirunavukkarasu, Ashokkumar

2014-09-12

Metallic nanoparticles are major concern, particularly silver nanoparticles (AgNPs) are used in various applications. In the present investigation, we report a novel strategy with biological approach for synthesis of AgNPs using sodium para-hydroxybenzoate tetrahydrate (SPHT) isolated from Vitex negundo leaves. The synthesized SPHT-AgNPs were characterized by UV-vis spectroscopy, high resolution transmission electron microscopy (HRTEM) with selected area electron diffraction (SAED) pattern, field emission scanning electron microscopy (FESEM) with energy-dispersive X-ray spectroscopy (EDX), zeta potential and Fourier transform infrared spectroscopy (FT-IR) analysis. The various pH and temperature were evaluated to find their stability effects on SPHT-AgNPs synthesis peak at 430 nm. The size of SPHT-AgNPs were ranging from 26 to 39 nm and were spherical in shape. The hydroxyl and carboxylic functional groups from bio-reducing mediators of SPHT have a stronger ability towards synthesis of AgNPs, which was confirmed using FT-IR spectrum. In addition, anticancer activity were determined by MTT assay, Annexin V-FITC/PI and cell cycle analysis. Copyright © 2014 Elsevier Masson SAS. All rights reserved.
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.
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.
Detection and classification of salmonella serotypes using spectral signatures collected by fourier transform infrared (FT-IR) spectroscopy

USDA-ARS?s Scientific Manuscript database

Spectral signatures of Salmonella serotypes namely Salmonella Typhimurium, Salmonella Enteritidis, Salmonella Infantis, Salmonella Heidelberg and Salmonella Kentucky were collected using Fourier transform infrared spectroscopy (FT-IR). About 5-10 µL of Salmonella suspensions with concentrations of 1...
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...
XPS Spectra Analysis of Ti2+, Ti3+ Ions and Dye Photodegradation Evaluation of Titania-Silica Mixed Oxide Nanoparticles

NASA Astrophysics Data System (ADS)

Chinh, Vu Duc; Broggi, Alessandra; Di Palma, Luca; Scarsella, Marco; Speranza, Giorgio; Vilardi, Giorgio; Thang, Pham Nam

2018-04-01

TiO2-SiO2 mixed oxides have been prepared by the sol-gel technique from tetrabutyl orthotitanate and tetraethyl orthosilicate. The prepared materials were characterized by x-ray diffraction, scanning electron microscopy, energy dispersive x-ray spectroscopy, nitrogen physisorption, Fourier-transform infrared spectroscopy (FT-IR) and x-ray photoelectron spectroscopy (XPS). The results indicate that the TiO2-SiO2 mixed oxides have a large surface area and a nanoscale size. FT-IR spectra show that Ti atoms are bonded to silica by oxygen bridging atoms in Ti-O-Si bonds. The titanium valence states in TiO2-SiO2 mixed oxides were investigated by XPS, and their spectra report the presence of Ti2+ and Ti3+ cations for high silica concentration, suggesting the formation of oxygen vacancies. The photocatalytic activity of the prepared materials has been evaluated for the photodegradation of methylene blue (MB). The mixed oxides were activated by means of a UV light source, and the concentration of MB was monitored by UV-Vis spectroscopy. The synthesized TiO2-SiO2 shows significantly higher MB removal efficiency in comparison with that of the commercial TiO2 Degussa, P25.
Comparison of FTIR-ATR and Raman spectroscopy in determination of VLDL triglycerides in blood serum with PLS regression

NASA Astrophysics Data System (ADS)

Oleszko, Adam; Hartwich, Jadwiga; Wójtowicz, Anna; Gąsior-Głogowska, Marlena; Huras, Hubert; Komorowska, Małgorzata

2017-08-01

Hypertriglyceridemia, related with triglyceride (TG) in plasma above 1.7 mmol/L is one of the cardiovascular risk factors. Very low density lipoproteins (VLDL) are the main TG carriers. Despite being time consuming, demanding well-qualified staff and expensive instrumentation, ultracentrifugation technique still remains the gold standard for the VLDL isolation. Therefore faster and simpler method of VLDL-TG determination is needed. Vibrational spectroscopy, including FT-IR and Raman, is widely used technique in lipid and protein research. The aim of this study was assessment of Raman and FT-IR spectroscopy in determination of VLDL-TG directly in serum with the isolation step omitted. TG concentration in serum and in ultracentrifugated VLDL fractions from 32 patients were measured with reference colorimetric method. FT-IR and Raman spectra of VLDL and serum samples were acquired. Partial least square (PLS) regression was used for calibration and leave-one-out cross validation. Our results confirmed possibility of reagent-free determination of VLDL-TG directly in serum with both Raman and FT-IR spectroscopy. Quantitative VLDL testing by FT-IR and/or Raman spectroscopy applied directly to maternal serum seems to be promising screening test to identify women with increased risk of adverse pregnancy outcomes and patient friendly method of choice based on ease of performance, accuracy and efficiency.
Preparation of thermally stable nanocrystalline hydroxyapatite by hydrothermal method.

PubMed

Prakash Parthiban, S; Elayaraja, K; Girija, E K; Yokogawa, Y; Kesavamoorthy, R; Palanichamy, M; Asokan, K; Narayana Kalkura, S

2009-12-01

Thermally stable hydroxyapatite (HAp) was synthesized by hydrothermal method in the presence of malic acid. X-ray diffraction (XRD), Fourier transform infra-red spectroscopy (FT-IR), Raman spectroscopy, scanning electron microscopy (SEM), differential thermal analysis (DTA), thermogravimetric analysis (TGA) was done on the synthesized powders. These analyses confirmed the sample to be free from impurities and other phases of calcium phosphates, and were of rhombus morphology along with nanosized particles. IR and Raman analyses indicated the adsorption of malic acid on HAp. Thermal stability of the synthesized HAp was confirmed by DTA and TGA. The synthesized powders were thermally stable upto 1,400 degrees C and showed no phase change. The proposed method might be useful for producing thermally stable HAp which is a necessity for high temperature coating applications.
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 ...
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.
Electrosynthesis and characterization of zinc tungstate nanoparticles

NASA Astrophysics Data System (ADS)

Rahimi-Nasrabadi, Mehdi; Pourmortazavi, Seied Mahdi; Ganjali, Mohammad Reza; Hajimirsadeghi, Seiedeh Somayyeh; Zahedi, Mir Mahdi

2013-09-01

Zinc tungstate nanoparticles with different sizes are produced through an electrolysis process including a zinc plate anode in sodium tungstate solution. The shape and size of the product was found to be controlled by varying reaction parameters such as electrolysis voltage, stirring rate of electrolyte solution and temperature. The morphological (SEM) characterization analysis was performed on the product and UV-Vis spectrophotometry and FT-IR spectroscopy was utilized to characterize the electrodeposited nanoparticles. Study of the particle size of the product versus the electrolysis voltage showed that, increasing the voltage from 4 to 8 V, led to the particle size of zinc tungstate to decrease, but further increasing the voltage from 8 to 12 V, the particle size of the produced particles increased. The size and shape of the product was also found to be dependent on the stirring rate and temperature of the electrolyte solution. X-ray diffraction (XRD), scanning electron microscopy (SEM), FT-IR spectroscopy, and photoluminescence, were used to study the structure as well as composition of the nano-material prepared under optimum conditions.
An efficient and heterogeneous recyclable silicotungstic acid with modified acid sites as a catalyst for conversion of fructose and sucrose into 5-hydroxymethylfurfural in superheated water.

PubMed

Jadhav, Arvind H; Kim, Hern; Hwang, In Taek

2013-03-01

Acidity modified silver exchanged silicotungstic acid (AgSTA) catalyst was prepared and characterized by X-ray diffraction, FT-IR spectroscopy, Raman spectroscopy, FT-IR pyridine adsorption, SEM imaging, EDX mapping, and antimicrobial activity was also tested. The catalytic activity was evaluated for the dehydration of fructose and sucrose in superheated water. As a result, 98% conversion of fructose with 85.7% HMF yield and 87.4% HMF selectivity in 120 min reaction time at 120 °C reaction temperature using 10 wt.% of AgSTA catalyst was achieved. While, 92% sucrose conversion with 62.5% of HMF yield was obtained from sucrose at uniform condition in 160 min. The effect of reaction parameters, such as reaction temperature, time, catalyst dosage, and effect acidity on HMF yield was also investigated. The AgSTA catalyst was separated from the reaction mixture by filtration process at end of the reaction and reused eight times without loss of catalytic activity. Copyright © 2013 Elsevier Ltd. All rights reserved.
Nanofibers of cellulose bagasse from Agave tequilana Weber var. azul by electrospinning: preparation and characterization.

PubMed

Robles-García, Miguel Ángel; Del-Toro-Sánchez, Carmen Lizette; Márquez-Ríos, Enrique; Barrera-Rodríguez, Arturo; Aguilar, Jacobo; Aguilar, José A; Reynoso-Marín, Francisco Javier; Ceja, I; Dórame-Miranda, R; Rodríguez-Félix, Francisco

2018-07-15

In this study, cellulose of bagasse from Agave tequilana Weber var. azul was extracted to elaborate nanofibers by the electrospinning technique. Fiber characterization was performed using Transmission Electron Microscopy (TEM), x-ray, Fournier Transform-InfraRed (FT-IR) spectroscopy, and thermal analysis by Differential Scanning Calorimetry-Thermogravimetric Analysis (DSC-TGA). Different diameters (ranging from 54.57 ± 0.02 to 171 ± 0.01 nm) of nanofibers were obtained. Cellulose nanofibers were analyzed by means of x-ray diffraction, where we observed a total loss of crystallinity in comparison with the cellulose, while FT-IR spectroscopy revealed that the hemicellulose and lignin present in the agave bagasse were removed. Thermal analysis showed that nanofibers exhibit enhanced thermal properties, and the zeta potential value (-32.5 mV) demonstrated moderate stability in the sample. In conclusion, the nanofibers obtained provide other alternatives-of-use for this agro-industrial residue and could have potential in various industrial applications, among these encapsulation of bioactive compounds and reinforcing material, to mention a few. Copyright © 2018 Elsevier Ltd. All rights reserved.
Discrimination of different genuine Danshen and their extracts by Fourier transform infrared spectroscopy combined with two-dimensional correlation infrared spectroscopy

NASA Astrophysics Data System (ADS)

Liu, Xin-hu; Xu, Chang-hua; Sun, Su-qin; Huang, Jian; Zhang, Ke; Li, Guo-yu; Zhu, Yun; Zhou, Qun; Zhang, Zhi-cheng; Wang, Jin-hui

2012-11-01

In this study, six varieties of Danshen from different populations and genuine ("Daodi" in Chinese transliteration) regions were discriminated and identified by a three-step infrared spectroscopy method (Fourier transform-infrared spectroscopy (FT-IR) coupled with second derivative infrared spectroscopy (SD-IR) and two dimensional correlation infrared spectroscopy (2D-IR)). Though only small differences were found among the FT-IR spectra of the six Danshen samples, the positions and intensities of peaks at 3393, 3371, 1613, 1050, and 1036 cm-1 could be considered as the key factors to discriminate them. More significant differences were exhibited in their SD-IR, particularly for the peaks around 1080, 1144, 695, 665, 800, 1610, 1510, 1450, 1117 and 1077 cm-1. The visual 2D-IR spectra provided dynamic chemical structure information of the six Danshen samples with presenting different particular auto-peak clusters, respectively. Moreover, the contents of salvianolic acid B in all samples were measured quantitatively by a validated ultra performance liquid chromatography (UPLC), which was consistent with the FT-IR findings. This study provides a promising method for characteristics and quality control of the complicated and extremely similar herbal medicine like Danshen, which is more cost effective and time saving.
Morphological and phase evolution of TiO 2 nanocrystals prepared from peroxotitanate complex aqueous solution: Influence of acetic acid

NASA Astrophysics Data System (ADS)

Chang, Jeong Ah; Vithal, Muga; Baek, In Chan; Seok, Sang Il

2009-04-01

Nanosized anatase and rutile TiO 2 having different shape, phase and size have been prepared from aqueous solutions of peroxo titanium complex starting from titanium(IV) isopropoxide (TTIP), acetic acid and hydrogen peroxide (H 2O 2) in water/isopropanol media by a facile sol-gel process. The TiO 2 nanocrystals are characterized by powder X-ray diffraction (XRD), Raman spectroscopy, FT-IR spectroscopy, TEM, high resolution transmission electron microscopy (HRTEM) and selected area electron diffraction (SAED) techniques. The influence of pH and the sequence of addition of reaction contents on the phase and morphology of TiO 2 are studied. The reasons for the observation of only anatase and/or mixture of anatase and rutile are given.
Crystallization of a non-steroidal anti-inflammatory drug from ethanol-water solution in presence of polymers: physicochemical characterization and release behaviour from suppositories.

PubMed

Mallick, Subrata; Dey, Pintu K; Sannigrahi, Santanu; Mitra, Avishek

2004-01-01

Altered crystallization condition has been designed and adopted to a model non-steroidal anti-inflammatory drug, while crystallizing from ethanol-water solution in absence and presence of polymers such as Eudragit RS and ethylcellulose. To minimize the gastro-intestinal side effects nimesulide was considered as a model drug candidate for the development of suppository formulation. Physicochemical characteristics of the crystals were evaluated by Scanning Electron Microscopy (SEM). X-ray diffraction (XRD) and Fourier Transformed Infrared Spectroscopy (FT-IR). Smoothness and sharpness of the crystal have been decreased with increased concentration of a polymer. A little change in crystal habit and geometry has also been observed. Crystals are discrete in nature and more than 90% were in the range of 20-90 micron. The X-ray diffractions of nimesulide crystallized in absence of polymer and physical mixture of drug-polymer revealed fewer high intensity reflections when compared with the drug crystallized in presence of Eudragit RS, which testified a slight decreased ordering of crystal lattice in the latter. In presence of ethylcellulose, slightly increased ordering of crystal lattice was observed. No strong interactions were noticed as revealed by FT-IR spectroscopy. Drug dissolution rate from suppository formulations containing nimesulide crystallized in presence of polymer was found to delay as compared with the suppository prepared by nimesulide crystallized in absence of polymer.
Adsorption of malachite green dye from aqueous solution on the bamboo leaf ash

NASA Astrophysics Data System (ADS)

Kuntari, Priwidyanjati, Dessyntha Anggiani

2017-12-01

Bamboo leaf ash has been developed as an adsorbent material for removal malachite green from aqueous solution. Adsorption parameters have studied are contact time and initial pH. The effect of contact time and pH were examined in the batch adsorption processes. The physicochemical characters of bamboo leaf ash were investigated by using X-Ray Diffraction (XRD) and FT-IR spectroscopy. Malachite green concentration was determined by UV-Vis spectrophotometer. FT-IR spectrogram of bamboo leaf ash shows that typical fingerprint of adsorbent material with Si-O-Si or Al-O-Al group. The X-ray diffractograms of bamboo leaf ash show that adsorbent material has a highly amorphous nature. The percentage of adsorption was showed raised with increasing contact time. The optimum removal of malachite green when the initial dye concentration, initial pH, weight of adsorbent and contact time was 20 mg/L, 7, 0.25 g and 75 minutes respectively.
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.
Evaluation of Turmeric Powder Adulterated with Metanil Yellow Using FT-Raman and FT-IR Spectroscopy

PubMed Central

Dhakal, Sagar; Chao, Kuanglin; Schmidt, Walter; Qin, Jianwei; Kim, Moon; Chan, Diane

2016-01-01

Turmeric powder (Curcuma longa L.) is valued both for its medicinal properties and for its popular culinary use, such as being a component in curry powder. Due to its high demand in international trade, turmeric powder has been subject to economically driven, hazardous chemical adulteration. This study utilized Fourier Transform-Raman (FT-Raman) and Fourier Transform-Infra Red (FT-IR) spectroscopy as separate but complementary methods for detecting metanil yellow adulteration of turmeric powder. Sample mixtures of turmeric powder and metanil yellow were prepared at concentrations of 30%, 25%, 20%, 15%, 10%, 5%, 1%, and 0.01% (w/w). FT-Raman and FT-IR spectra were acquired for these mixture samples as well as for pure samples of turmeric powder and metanil yellow. Spectral analysis showed that the FT-IR method in this study could detect the metanil yellow at the 5% concentration, while the FT-Raman method appeared to be more sensitive and could detect the metanil yellow at the 1% concentration. Relationships between metanil yellow spectral peak intensities and metanil yellow concentration were established using representative peaks at FT-Raman 1406 cm−1 and FT-IR 1140 cm−1 with correlation coefficients of 0.93 and 0.95, respectively. PMID:28231130
Chemical profiling and adulteration screening of Aquilariae Lignum Resinatum by Fourier transform infrared (FT-IR) spectroscopy and two-dimensional correlation infrared (2D-IR) spectroscopy.

PubMed

Qu, Lei; Chen, Jian-Bo; Zhang, Gui-Jun; Sun, Su-Qin; Zheng, Jing

2017-03-05

As a kind of expensive perfume and valuable herb, Aquilariae Lignum Resinatum (ALR) is often adulterated for economic motivations. In this research, Fourier transform infrared (FT-IR) spectroscopy is employed to establish a simple and quick method for the adulteration screening of ALR. First, the principal chemical constituents of ALR are characterized by FT-IR spectroscopy at room temperature and two-dimensional correlation infrared (2D-IR) spectroscopy with thermal perturbation. Besides the common cellulose and lignin compounds, a certain amount of resin is the characteristic constituent of ALR. Synchronous and asynchronous 2D-IR spectra indicate that the resin (an unstable secondary metabolite) is more sensitive than cellulose and lignin (stable structural constituents) to the thermal perturbation. Using a certified ALR sample as the reference, the infrared spectral correlation threshold is determined by 30 authentic samples and 6 adulterated samples. The spectral correlation coefficient of an authentic ALR sample to the standard reference should be not less than 0.9886 (p=0.01). Three commercial adulterated ALR samples are identified by the correlation threshold. Further interpretation of the infrared spectra of the adulterated samples indicates the common adulterating methods - counterfeiting with other kind of wood, adding ingredient such as sand to increase the weight, and adding the cheap resin such as rosin to increase the content of resin compounds. Results of this research prove that FT-IR spectroscopy can be used as a simple and accurate quality control method of ALR. Copyright © 2016 Elsevier B.V. All rights reserved.

Chemical profiling and adulteration screening of Aquilariae Lignum Resinatum by Fourier transform infrared (FT-IR) spectroscopy and two-dimensional correlation infrared (2D-IR) spectroscopy

NASA Astrophysics Data System (ADS)

Qu, Lei; Chen, Jian-bo; Zhang, Gui-Jun; Sun, Su-qin; Zheng, Jing

2017-03-01

As a kind of expensive perfume and valuable herb, Aquilariae Lignum Resinatum (ALR) is often adulterated for economic motivations. In this research, Fourier transform infrared (FT-IR) spectroscopy is employed to establish a simple and quick method for the adulteration screening of ALR. First, the principal chemical constituents of ALR are characterized by FT-IR spectroscopy at room temperature and two-dimensional correlation infrared (2D-IR) spectroscopy with thermal perturbation. Besides the common cellulose and lignin compounds, a certain amount of resin is the characteristic constituent of ALR. Synchronous and asynchronous 2D-IR spectra indicate that the resin (an unstable secondary metabolite) is more sensitive than cellulose and lignin (stable structural constituents) to the thermal perturbation. Using a certified ALR sample as the reference, the infrared spectral correlation threshold is determined by 30 authentic samples and 6 adulterated samples. The spectral correlation coefficient of an authentic ALR sample to the standard reference should be not less than 0.9886 (p = 0.01). Three commercial adulterated ALR samples are identified by the correlation threshold. Further interpretation of the infrared spectra of the adulterated samples indicates the common adulterating methods - counterfeiting with other kind of wood, adding ingredient such as sand to increase the weight, and adding the cheap resin such as rosin to increase the content of resin compounds. Results of this research prove that FT-IR spectroscopy can be used as a simple and accurate quality control method of ALR.
Study on antibacterial alginate-stabilized copper nanoparticles by FT-IR and 2D-IR correlation spectroscopy

PubMed Central

Díaz-Visurraga, Judith; Daza, Carla; Pozo, Claudio; Becerra, Abraham; von Plessing, Carlos; García, Apolinaria

2012-01-01

Background The objective of this study was to clarify the intermolecular interaction between antibacterial copper nanoparticles (Cu NPs) and sodium alginate (NaAlg) by Fourier transform infrared spectroscopy (FT-IR) and to process the spectra applying two-dimensional infrared (2D-IR) correlation analysis. To our knowledge, the addition of NaAlg as a stabilizer of copper nanoparticles has not been previously reported. It is expected that the obtained results will provide valuable additional information on: (1) the influence of reducing agent ratio on the formation of copper nanoparticles in order to design functional nanomaterials with increased antibacterial activity, and (2) structural changes related to the incorporation of Cu NPs into the polymer matrix. Methods Cu NPs were prepared by microwave heating using ascorbic acid as reducing agent and NaAlg as stabilizing agent. The characterization of synthesized Cu NPs by ultraviolet visible spectroscopy, transmission electron microscopy (TEM), electron diffraction analysis, X-ray diffraction (XRD), and semiquantitative analysis of the weight percentage composition indicated that the average particle sizes of Cu NPs are about 3–10 nm, they are spherical in shape, and consist of zerovalent Cu and Cu2O. Also, crystallite size and relative particle size of stabilized Cu NPs were calculated by XRD using Scherrer’s formula and FT from the X-ray diffraction data. Thermogravimetric analysis, differential thermal analysis, differential scanning calorimetry (DSC), FT-IR, second-derivative spectra, and 2D-IR correlation analysis were applied to studying the stabilization mechanism of Cu NPs by NaAlg molecules. The minimum inhibitory concentration (MIC) and minimum bactericidal concentration (MBC) of stabilized Cu NPs against five bacterial strains (Staphylococccus aureus ATCC 6538P, Escherichia coli ATCC 25922 and O157: H7, and Salmonella enterica serovar Typhimurium ATCC 13311 and 14028) were evaluated with macrodilution, agar dilution plate count, and well-diffusion methods. Results On the basis of the semiquantitative analysis, there was a direct correlation between the reducing agent ratio and the percentage of zerovalent Cu. This was confirmed with the statistical analysis of population of Cu NPs from TEM micrographs. At lower reducing agent ratios, two phases coexist (Cu2O and zerovalent Cu) due to incomplete reduction of copper ions by the reducing agent; however, at higher reducing agent ratios, the Cu NPs consist mainly of zerovalent Cu. Crystallite size and relative particle size of stabilized Cu NPs showed considerable differences in results and tendencies in respect to TEM analysis. However, the relative particle size values obtained from FT of XRD data agreed well with the histograms from the TEM observations. From FT results, the relative particle size and reducing agent ratio of stabilized Cu NPs showed an inverse correlation. The incomplete reduction of copper ions at lower reducing agent ratios was also confirmed by DSC studies. FT-IR and 2D-IR correlation spectra analysis suggested the first event involved in the stabilization of Cu NPs is their electrostatic interaction with –C=O of carboxylate groups of NaAlg, followed by the interaction with the available O–C–O−, and finally with the –OH groups. Bacterial susceptibility to stabilized nanoparticles was found to vary depending on the bacterial strains. The lowest MIC and MBC of stabilized Cu NPs ranged between 2 mg/L and 8 mg/L for all studied strains. Disk-diffusion studies with both E. coli strains revealed greater effectiveness of the stabilized Cu NPs compared to the positive controls (cloxacillin, amoxicillin, and nitrofurantoin). S. aureus showed the highest sensitivity to stabilized Cu NPs compared to the other studied strains. Conclusion Cu NPs were successfully synthesized via chemical reduction assisted with microwave heating. Average particle size, polydispersity, and phase composition of Cu NPs depended mainly on the reducing agent ratio. Likewise, thermal stability and antibacterial activity of stabilized Cu NPs were affected by their phase composition. Because of the carboxylate groups in polymer chains, the structural changes of stabilized Cu NPs are different from those of NaAlg. NaAlg acted as a size controller and stabilizing agent of Cu NPs, due to their ability to bind strongly to the metal surface. Our study on the stabilizing agent–dependent structural changes of stabilized NPs is helpful for wide application of NaAlg as an important biopolymer. PMID:22848180
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-).
Mechanochemical synthesis and structural characterization of three novel cocrystals of dimethylglyoxime with N-heterocyclic aromatic compounds and acetamide

NASA Astrophysics Data System (ADS)

Abidi, Syed Sibte Asghar; Azim, Yasser; Gupta, Abhishek Kumar; Pradeep, Chullikkattil P.

2017-12-01

With an aim to explore the interactions of (RR'Cdbnd Nsbnd OH) oxime moiety of dimethylglyoxime (DMG) with pyridyl ring of N-heterocyclic aromatic compounds and acetamide, three novel cocrystals of dimethylglyoxime with acridine (ACR), 1,10-phenanthroline monohydrate (PT) and acetamide (ACT) are reported. These three cocrystals were obtained with a mechanochemical synthesis approach and were characterized by single crystal X-ray diffraction (SCXRD), powder X-ray diffraction (PXRD), fourier transform-infrared spectroscopy (FT-IR), differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). Additionally, Hirshfeld surface analysis is used to investigate the intermolecular interaction and the crystal packing of cocrystals.
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.
Characterisation of 1,3-diammonium propylselenate monohydrate by XRD, FT-IR, FT-Raman, DSC and DFT studies

NASA Astrophysics Data System (ADS)

Thirunarayanan, S.; Arjunan, V.; Marchewka, M. K.; Mohan, S.; Atalay, Yusuf

2016-03-01

The crystals of 1,3-diammonium propylselenate monohydrate (DAPS) were prepared and characterised X-ray diffraction (XRD), FT-IR, FT-Raman spectroscopy, and DFT/B3LYP methods. It comprises protonated propyl ammonium moieties (diammonium propyl cations), selenate anions and water molecule which are held together by a number of hydrogen bonds and form infinite chains. The XRD data confirm the transfer of two protons from selenic acid to 1,3-diaminopropane molecule. The DAPS complex is stabilised by the presence of O-H···O and N-H···O hydrogen bonds and the electrostatic interactions as well. The N···O and O···O bond distances are 2.82-2.91 and 2.77 Å, respectively. The FT-IR and FT-Raman spectra of 1,3-diammonium propyl selenate monohydrate are recorded and the complete vibrational assignments have been discussed. The geometry is optimised by B3LYP method using 6-311G, 6-311+G and 6-311+G* basis sets and the energy, structural parameters, vibrational frequencies, IR and Raman intensities are determined. Differential scanning colorimetry (DSC) data were also presented to analyse the possibility of the phase transition. Complete natural bonding orbital (NBO) analysis is carried out to analyse the intramolecular electronic interactions and their stabilisation energies. The electrostatic potential of the complex lies in the range +1.902e × 10-2 to -1.902e × 10-2. The limits of total electron density of the complex is +8.43e × 10-2 to -8.43e × 10-2.
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
Biological and catalytic applications of green synthesized fluorescent N-doped carbon dots using Hylocereus undatus.

PubMed

Arul, Velusamy; Edison, Thomas Nesakumar Jebakumar Immanuel; Lee, Yong Rok; Sethuraman, Mathur Gopalakrishnan

2017-03-01

In this work, a simple hydrothermal route for the synthesis of fluorescent nitrogen doped carbon dots (N-CDs) is reported. The Hylocereus undatus (H. undatus) extract and aqueous ammonia are used as carbon and nitrogen source, respectively. The optical properties of synthesized N-CDs are analyzed using UV-Visible (UV-Vis) and fluorescence spectroscopy. The surface morphology, elemental composition, crystallinity and functional groups present in the N-CDs are examined using high resolution transmission electron microscopy (HR-TEM) with energy dispersive spectroscopy (EDS), selected area electron diffraction (SAED), X-ray diffraction (XRD) and Fourier transform infrared (FT-IR) spectroscopy, respectively. The synthesized N-CDs emit strong blue fluorescence at 400nm under the excitation of 320nm. Further, the excitation dependent emission properties are also observed from the fluorescence of synthesized N-CDs. The HR-TEM results reveal that synthesized N-CDs are in spherical shape with average diameter of 2.5nm. The XRD pattern exhibits, the graphitic nature of synthesized N-CDs. The doping of nitrogen is confirmed from the EDS and FT-IR studies. The cytotoxicity and biocompatibility of N-CDs are evaluated through MTT assay on L-929 (Lymphoblastoid-929) and MCF-7 (Michigan Cancer Foundation-7) cells. The results indicate that the fluorescent N-CDs show less cytotoxicity and good biocompatibility on both L-929 and MCF-7 cells. Moreover, the N-CDs show excellent catalytic activity towards the reduction of methylene blue by sodium borohydride. Copyright © 2017 Elsevier B.V. All rights reserved.
Structural and microstructural aspects of asbestos-cement waste vitrification

NASA Astrophysics Data System (ADS)

Iwaszko, Józef; Zawada, Anna; Przerada, Iwona; Lubas, Małgorzata

2018-04-01

The main goal of the work was to evaluate the vitrification process of asbestos-cement waste (ACW). A mixture of 50 wt% ACW and 50 wt% glass cullet was melted in an electric furnace at 1400 °C for 90 min and then cast into a steel mold. The vitrified product was subjected to annealing. Optical microscopy, scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR) and X-ray diffraction (XRD) were used to evaluate the effects of the vitrification. The chemical constitution of the material before and after the vitrification process was also analyzed. It was found that the vitrified product has an amorphous structure in which the components of asbestos-cement waste are incorporated. MIR spectroscopy showed that the absorption bands of chrysotile completely disappeared after the vitrification process. The results of the spectroscopic studies were confirmed by X-ray studies - no diffraction reflections from the chrysotile crystallographic planes were observed. As a result of the treatment, the fibrous asbestos construction, the main cause of its pathogenic properties, completely disappeared. The vitrified material was characterized by higher resistance to ion leaching in an aquatic environment than ACW and a smaller volume of nearly 72% in relation to the apparent volume of the substrates. The research has confirmed the high effectiveness of vitrification in neutralizing hazardous waste containing asbestos and the FT-IR spectroscopy was found to be useful to identify asbestos varieties and visualizing changes caused by the vitrification process. The work also presents the current situation regarding the utilization of asbestos-containing products.
Analysis and identification of two similar traditional Chinese medicines by using a three-stage infrared spectroscopy: Ligusticum chuanxiong, Angelica sinensis and their different extracts

NASA Astrophysics Data System (ADS)

Xiang, Li; Wang, Jingjuan; Zhang, Guijun; Rong, Lixin; Wu, Haozhong; Sun, Suqin; Guo, Yizhen; Yang, Yanfang; Lu, Lina; Qu, Lei

2016-11-01

Rhizoma Chuanxiong (CX) and Radix Angelica sinensis (DG) are very important Traditional Chinese Medicine (TCM) and usually used in clinic. They both are from the Umbelliferae family, and have almost similar chemical constituents with each other. It is complicated, time-consuming and laborious to discriminate them by using the chromatographic methods such as high performance liquid chromatography (HPLC) and gas chromatography (GC). Therefore, to find a fast, applicable and effective identification method for two herbs is urged in quality research of TCM. In this paper, by using a three-stage infrared spectroscopy (Fourier transform infrared spectroscopy (FT-IR), the second derivative infrared spectroscopy (SD-IR) and two-dimensional correlation infrared spectroscopy (2D-IR)), we analyzed and discriminated CX, DG and their different extracts (aqueous extract, alcoholic extract and petroleum ether extract). In FT-IR, all the CX and DG samples' spectra seemed similar, but they had their own unique macroscopic fingerprints to identify. Through comparing with the spectra of sucrose and the similarity calculation, we found the content of sucrose in DG raw materials was higher than in CX raw materials. The significant differences in alcoholic extract appeared that in CX alcoholic extract, the peaks at 1743 cm-1 was obviously stronger than the peak at same position in DG alcoholic extract. Besides in petroleum ether extract, we concluded CX contained much more ligustilide than DG by the similarity calculation. With the function of SD-IR, some tiny differences were amplified and overlapped peaks were also unfolded in FT-IR. In the range of 1100-1175 cm-1, there were six peaks in the SD-IR spectra of DG and the intensity, shape and location of those six peaks were similar to that of sucrose, while only two peaks could be observed in that of CX and those two peaks were totally different from sucrose in shape and relative intensity. This result was consistent with that of the FT-IR. Several undetected characteristic fingerprints in FT-IR and SD-IR spectra were further disclosed by 2D-IR spectra. In the range of 1120-1500 cm-1, the FT-IR spectra and the SD-IR spectra of aqueous extract of CX and DG were almost similar and hard to be discriminated, but the 2D-IR spectra were markedly different. These findings indicated that the three-stage infrared spectroscopy can identify not only the main compositions in these two medicinal materials and their different extracts, but also can compare the differences of categories and quantities of chemical constituents between the similar samples. In conclusion, the three-stage infrared spectroscopy could identify the two similar TCM (CX and DG) quickly and effectively.
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.
Synthesis and characterization of some metal oxide nanocrystals by microwave irradiation

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

Rashad, M.; Gaber, A.; Abdelrahim, M. A.

2013-12-16

Copper oxide and cobalt oxide (CuO, Co3O4) nanocrystals (NCs) have been successfully prepared in a short time using microwave irradiation. The resulted powders of nanocrystals (NCs) were characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). Thermogravimetric analysis (TGA) measurements are also studied. Fourier-transform infrared (FT-IR) and UV–visible absorption spectroscopy of both kind of nanoparticels are illustrated. Optical absorption analysis indicated the direct band gap for both kinds of nanocrystals.
Cu sbnd Al sbnd Fe layered double hydroxides with CO32- and anionic surfactants with different alkyl chains in the interlayer

NASA Astrophysics Data System (ADS)

Trujillano, Raquel; Holgado, María Jesús; González, José Luis; Rives, Vicente

2005-08-01

Layered double hydroxides (LDHs), with the hydrotalcite-like structure containing Cu(II), Al(III) and Fe(III) in the layers, and different alkyl sulfonates in the interlayer, have been prepared and characterized by powder X-ray diffraction, FT-IR spectroscopy, differential thermal analysis and thermogravimetric analysis. Pure crystalline phases have been obtained in all cases. Upon heating, combustion of the organic chain takes place at lower temperature than the corresponding sodium salts.
The effect of chemical modification on the physico-chemical characteristics of halloysite: FTIR, XRF, and XRD studies

NASA Astrophysics Data System (ADS)

Szczepanik, Beata; Słomkiewicz, Piotr; Garnuszek, Magdalena; Czech, Kamil; Banaś, Dariusz; Kubala-Kukuś, Aldona; Stabrawa, Ilona

2015-03-01

The effect of chemical modification of halloysite from a Polish strip mine "Dunino" on the chemical composition and structure of this clay mineral was studied using infrared spectroscopy (ATR FT-IR), wavelength dispersive X-ray fluorescence (WDXRF), and X-ray powder diffraction (XRPD) methods. The results obtained by the WDXRF technique confirm that the content of silica and alumina was the highest for bleached halloysite samples and the lowest for acid-treated halloysite. A higher content of Fe2O3 in comparison to halloysite samples coming from other countries was observed for raw halloysite samples. XRPD diffraction pattern obtained for raw halloysite confirmed the presence of halloysite, kaolinite, hematite, and calcite minerals in the sample. Bleaching the halloysite removes (or significantly reduces) the content of other minerals present in the raw halloysite. The FT-IR spectra of the studied halloysite samples show in the 3700-3600 cm-1 region well-defined hydroxyl stretching bands characteristic for the kaolin-group minerals and bands associated with the vibrations of the aluminium-silicon skeleton in the 1400-1000 cm-1 region. Modifying halloysite with 4-chloro-aniline causes successive incorporation of amine into the BH sample.
Chamomile flower extract-directed CuO nanoparticle formation for its antioxidant and DNA cleavage properties.

PubMed

Duman, Fatih; Ocsoy, Ismail; Kup, Fatma Ozturk

2016-03-01

In this study, we report the synthesis of copper oxide nanoparticles (CuO NPs) using a medicinal plant (Matricaria chamomilla) flower extract as both reducing and capping agent and investigate their antioxidant activity and interaction with plasmid DNA (pBR322).The CuO NPs were characterized using Uv-Vis spectroscopy, FT-IR (Fourier transform infrared spectroscopy), DLS (dynamic light scattering), XRD (X-ray diffraction), EDX (energy-dispersive X-ray) spectroscopy and SEM (scanning electron microscopy). The CuO NPs exhibited nearly mono-distributed and spherical shapes with diameters of 140 nm size. UV-Vis absorption spectrum of CuO NPs gave a broad peak around 285 and 320 nm. The existence of functional groups on the surface of CuO NPs was characterized with FT-IR analysis. XRD pattern showed that the NPs are in the form of a face-centered cubic crystal. Zeta potential value was measured as -20 mV due to the presence of negatively charged functional groups in plant extract. Additionally, we demonstrated concentration-dependent antioxidant activity of CuO NPs and their interaction with plasmid DNA. We assumed that the CuO NPs both cleave and break DNA double helix structure. Copyright © 2015 Elsevier B.V. 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.
Effect of reaction atmosphere on structural and optical properties of hexagonal molybdenum oxide (h-MoO{sub 3})

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

Doss, V. Arumai; Chithambararaj, A.; Bose, A. Chandra, E-mail: acbose@nitt.edu

2016-05-23

The present work aims to synthesize single phase h-MoO{sub 3} nanocrytals by chemical precipitation method exposed under different reaction atmospheres. The reaction atmosphere have been successfully tuned as air, nitrogen and argon and studied its effects on structural, functional, morphology and optical properties by using X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared (FT-IR) spectroscopy and diffuse reflectance spectroscopy (DRS) measurements. The XRD result indicates that the sample exhibits characteristic hexagonal phase of MoO{sub 3}. The crystallite size is estimated by well known Scherrer’s method. The crystallite size is relative small in the case of sample prepared atmore » argon atmosphere. The functional groups such as Mo-O, N-H and O-H are identified from FT-IR spectroscopy. The particle exhibits rod like morphology with perfect hexagonal cross-section. The optical absorption observed at 420-450 nm corresponds to fundamental optical absorption by h-MoO{sub 3}. The band gap values are estimated using Kublka-Munk (K-M) function and found to be 2. 87 eV, 2.93 eV and 2.97 eV for samples synthesized under air, nitrogen and argon, respectively.« less
Electrical conductivity studies of graphene wrapped nanocrystalline LiMnPO{sub 4} composite

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

Cheruku, Rajesh; D, Surya Bhaskaram; Govindaraj, G., E-mail: ggraj-7@yahoo.com

Nanocrystalline LiMnPO{sub 4} material was synthesized by template free sucrose assisted hydrothermal method. The material possesses the orthorhombic crystal structure with Pnma, space group having four formula units. The GO was prepared by the hummer’s method and it was reduced graphene oxide (rGO) with hydrazine hydrate in the presence of nitrogen atmosphere. LiMnPO{sub 4} material was wrapped by the rGO to increase its conductivity. The structural characterization was accomplished through X-ray diffraction, FT-IR and Raman spectroscopy. Morphology was identified by the SEM, Electrical characterization was done through impedance spectroscopy and the results were reported.
Discrimination of wild-growing and cultivated Lentinus edodes by tri-step infrared spectroscopy

NASA Astrophysics Data System (ADS)

Lin, Haojian; Liu, Gang; Yang, Weimei; An, Ran; Ou, Quanhong

2018-01-01

It's not easy to discriminate dried wild-growing Lentinus edodes (WL) and cultivated Lentinus edodes (CL) by conventional method based on the morphological inspection of fruiting bodies. In this paper, fruiting body samples of WL and CL are discriminated by a tri-step IR spectroscopy method, including Fourier transform infrared (FT-IR) spectroscopy, second derivatives infrared (SD-IR) spectroscopy and two-dimensional correlation infrared (2D-IR) spectroscopy under thermal perturbation. The results show that the FT-IR spectra of WL and CL are similar in holistic spectral profile. More significant differences are exhibited in their SD-IR spectra in the range of 1700 - 900 cm-1. Furthermore, more evident differences have been observed in their synchronous 2D-IR spectra in the range of 2970 - 2900, 1678 - 1390, 1250 -1104 and 1090 - 1030 cm-1. The CL has thirteen auto-peaks at 2958, 2921, 1649, 1563, 1450, 1218, 1192, 1161, 1140, 1110, 1082, 1065 and 1047 cm-1, in which the four strongest auto-peaks are at 2921, 1563, 1192 and 1082 cm-1. The WL shows fifteen auto-peaks at 2960, 2937, 2921, 1650, 1615, 1555, 1458, 1219, 1190, 1138, 1111, 1084, 1068, 1048 and 1033 cm-1, in which the four strongest auto-peaks are at 2921, 1650, 1190 and 1068 cm-1. This study shows the potential of FT-IR spectroscopy and 2D correlation analysis in a simple and quick distinction of wild-growing and cultivated mushrooms.
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,...

Differentiation of the root of Cultivated Ginseng, Mountain Cultivated Ginseng and Mountain Wild Ginseng using FT-IR and two-dimensional correlation IR spectroscopy

NASA Astrophysics Data System (ADS)

Liu, Dan; Li, Yong-Guo; Xu, Hong; Sun, Su-Qin; Wang, Zheng-Tao

2008-07-01

Ginseng is one of the most widely used herbal medicines. Based on the grown environments and the cultivate method, three kinds of ginseng, Cultivated Ginseng (CG), Mountain Cultivated Ginseng (MCG) and Mountain Wild Ginseng (MWG) are classified. A novel and scientific-oriented method was developed and established to discriminate and identify three kinds of ginseng using Fourier transform infrared spectroscopy (FT-IR), secondary derivative IR spectra and two-dimensional correlation infrared spectroscopy (2D-IR). The findings indicated that the relative contents of starch in the CG were more than that in MCG and MWG, while the relative contents of calcium oxalate and lipids in MWG were more than that in CG and MCG, and the relative contents of fatty acid in MCG were more than that in CG and MWG. The hierarchical cluster analysis was applied to data analysis of MWG, CG and MWG, which could be classified successfully. The results demonstrated the macroscopic IR fingerprint method, including FT-IR, secondary derivative IR and 2D-IR, can be applied to discriminate different ginsengs rapidly, effectively and non-destructively.
Rapid detection of talcum powder in tea using FT-IR spectroscopy coupled with chemometrics

PubMed Central

Li, Xiaoli; Zhang, Yuying; He, Yong

2016-01-01

This paper investigated the feasibility of Fourier transform infrared transmission (FT-IR) spectroscopy to detect talcum powder illegally added in tea based on chemometric methods. Firstly, 210 samples of tea powder with 13 dose levels of talcum powder were prepared for FT-IR spectra acquirement. In order to highlight the slight variations in FT-IR spectra, smoothing, normalize and standard normal variate (SNV) were employed to preprocess the raw spectra. Among them, SNV preprocessing had the best performance with high correlation of prediction (RP = 0.948) and low root mean square error of prediction (RMSEP = 0.108) of partial least squares (PLS) model. Then 18 characteristic wavenumbers were selected based on a hybrid of backward interval partial least squares (biPLS) regression, competitive adaptive reweighted sampling (CARS) algorithm and successive projections algorithm (SPA). These characteristic wavenumbers only accounted for 0.64% of the full wavenumbers. Following that, 18 characteristic wavenumbers were used to build linear and nonlinear determination models by PLS regression and extreme learning machine (ELM), respectively. The optimal model with RP = 0.963 and RMSEP = 0.137 was achieved by ELM algorithm. These results demonstrated that FT-IR spectroscopy with chemometrics could be used successfully to detect talcum powder in tea. PMID:27468701
Identification of the traditional Tibetan medicine "Shaji" and their different extracts through tri-step infrared spectroscopy

NASA Astrophysics Data System (ADS)

Liu, Yue; Li, Jingyi; Fan, Gang; Sun, Suqin; Zhang, Yuxin; Zhang, Yi; Tu, Ya

2016-11-01

Hippophae rhamnoides subsp. sinensis Rousi, Hippophae gyantsensis (Rousi) Y. S. Lian, Hippophae neurocarpa S. W. Liu & T. N. He and Hippophae tibetana Schlechtendal are typically used under one name "Shaji", to treat cardiovascular diseases and lung disorders in Tibetan medicine (TM). A complete set of infrared (IR) macro-fingerprints of these four Hippophae species should be characterized and compared simply, accurately, and in detail for identification. In the present study, tri-step IR spectroscopy, which included Fourier transform IR (FT-IR) spectroscopy, second derivative IR (SD-IR) spectroscopy and two-dimensional correlation IR (2D-IR) spectroscopy, was employed to discriminate the four Hippophae species and their corresponding extracts using different solvents. The relevant spectra exhibited the holistic chemical compositions and variations. Flavonoids, fatty acids and sugars were found to be the main chemical components. Characteristic peak positions, intensities and shapes derived from FT-IR, SD-IR and 2D-IR spectra provided valuable information for sample discrimination. Principal component analysis (PCA) of spectral differences was performed to illustrate the objective identification. Results showed that the species and their extracts can be clearly distinguished. Thus, a quick, precise and effective tri-step IR spectroscopy combined with PCA can be applied to identify and discriminate medicinal materials and their extracts in TM research.
Univariate and multivariate analysis of tannin-impregnated wood species using vibrational spectroscopy.

PubMed

Schnabel, Thomas; Musso, Maurizio; Tondi, Gianluca

2014-01-01

Vibrational spectroscopy is one of the most powerful tools in polymer science. Three main techniques--Fourier transform infrared spectroscopy (FT-IR), FT-Raman spectroscopy, and FT near-infrared (NIR) spectroscopy--can also be applied to wood science. Here, these three techniques were used to investigate the chemical modification occurring in wood after impregnation with tannin-hexamine preservatives. These spectroscopic techniques have the capacity to detect the externally added tannin. FT-IR has very strong sensitivity to the aromatic peak at around 1610 cm(-1) in the tannin-treated samples, whereas FT-Raman reflects the peak at around 1600 cm(-1) for the externally added tannin. This high efficacy in distinguishing chemical features was demonstrated in univariate analysis and confirmed via cluster analysis. Conversely, the results of the NIR measurements show noticeable sensitivity for small differences. For this technique, multivariate analysis is required and with this chemometric tool, it is also possible to predict the concentration of tannin on the surface.
Solution combustion method for synthesis of nanostructured hydroxyapatite, fluorapatite and chlorapatite

NASA Astrophysics Data System (ADS)

Zhao, Junjie; Dong, Xiaochen; Bian, Mengmeng; Zhao, Junfeng; Zhang, Yao; Sun, Yue; Chen, JianHua; Wang, XuHong

2014-09-01

Hydroxyapatite (HAP), fluorapatite (Fap) and chlorapatite (Clap) were prepared by solution combustion method with further annealing at 800 °C. The characterization and structural features of the synthesized powders were evaluated by the powder X-ray diffraction (XRD, Fourier transform infrared spectroscopy (FT-IR), scanning electron microscope (SEM) and transmission electron microscopy (TEM) techniques. Characterization results from XRD and Rietveld analysis revealed that OH- in the HAP lattice were gradually substituted with the increase of F- and Cl- content and totally substituted at the molar concentration of 0.28 and 0.6, respectively. The results from FI-IR have also confirmed the incorporation of substituted anions in the apatite structure.
Crystal structure determination of new antimitotic agent bis(p-fluorobenzyl)trisulfide.

PubMed

An, Haoyun; Hu, Xiurong; Gu, Jianming; Chen, Linshen; Xu, Weiming; Mo, Xiaopeng; Xu, Wanhong; Wang, Xiaobo; Xu, Xiao

2008-01-01

The purpose of this research was to investigate the physical characteristics and crystalline structure of bis(p-fluorobenzyl)trisulfide, a new anti-tumor agent. Methods used included X-ray single crystal diffraction, X-ray powder diffraction (XRPD), Fourier-transform infrared (FT-IR) spectroscopy, differential scanning calorimetric (DSC) and thermogravimetric (TG) analyses. The findings obtained with X-ray single crystal diffraction showed that a monoclinic unit cell was a = 12.266(1) A, b = 4.7757(4) A, c = 25.510(1) A, beta = 104.25(1) degrees ; cell volume = 1,448.4(2) A(3), Z = 4, and space group C2/c. The XRPD studies of the four crystalline samples, obtained by recrystallization from four different solvents, indicated that they had the same diffraction patterns. The diffraction pattern stimulated from the crystal structure data is in excellent agreement with the experimental results. In addition, the identical FT-IR spectra of the four crystalline samples revealed absorption bands corresponding to S-S and C-S stretching as well as the characteristic aromatic substitution. Five percent weight loss at 163.3 degrees C was observed when TG was used to study the decomposition process in the temperature range of 20-200 degrees C. DSC also allowed for the determination of onset temperatures at 60.4(1)-60.7(3) degrees C and peak temperatures at 62.1(3)-62.4(3) degrees C for the four crystalline samples studied. The results verified that the single crystal structure shared the same crystal form with the four crystalline samples investigated.
Infrared spectroscopy and microscopy in cancer research and diagnosis

PubMed Central

Bellisola, Giuseppe; Sorio, Claudio

2012-01-01

Since the middle of 20th century infrared (IR) spectroscopy coupled to microscopy (IR microspectroscopy) has been recognized as a non destructive, label free, highly sensitive and specific analytical method with many potential useful applications in different fields of biomedical research and in particular cancer research and diagnosis. Although many technological improvements have been made to facilitate biomedical applications of this powerful analytical technique, it has not yet properly come into the scientific background of many potential end users. Therefore, to achieve those fundamental objectives an interdisciplinary approach is needed with basic scientists, spectroscopists, biologists and clinicians who must effectively communicate and understand each other's requirements and challenges. In this review we aim at illustrating some principles of Fourier transform (FT) Infrared (IR) vibrational spectroscopy and microscopy (microFT-IR) as a useful method to interrogate molecules in specimen by mid-IR radiation. Penetrating into basics of molecular vibrations might help us to understand whether, when and how complementary information obtained by microFT-IR could become useful in our research and/or diagnostic activities. MicroFT-IR techniques allowing to acquire information about the molecular composition and structure of a sample within a micrometric scale in a matter of seconds will be illustrated as well as some limitations will be discussed. How biochemical, structural, and dynamical information about the systems can be obtained by bench top microFT-IR instrumentation will be also presented together with some methods to treat and interpret IR spectral data and applicative examples. The mid-IR absorbance spectrum is one of the most information-rich and concise way to represent the whole “… omics” of a cell and, as such, fits all the characteristics for the development of a clinically useful biomarker. PMID:22206042
Dislocation, crystallite size distribution and lattice strain of magnesium oxide nanoparticles

NASA Astrophysics Data System (ADS)

Sutapa, I. W.; Wahid Wahab, Abdul; Taba, P.; Nafie, N. L.

2018-03-01

The oxide of magnesium nanoparticles synthesized using sol-gel method and analysis of the structural properties was conducted. The functional groups of nanoparticles has been analysed by Fourier Transform Infrared Spectroscopy (FT-IR). Dislocations, average size of crystal, strain, stress, the energy density of crystal, crystallite size distribution and morphologies of the crystals were determined based on X-ray diffraction profile analysis. The morphological of the crystal was analysed based on the image resulted from SEM analysis. The crystallite size distribution was calculated with the contention that the particle size has a normal logarithmic form. The most orientations of crystal were determined based on the textural crystal from diffraction data of X-ray diffraction profile analysis. FT-IR results showed the stretching vibration mode of the Mg-O-Mg in the range of 400.11-525 cm-1 as a broad band. The average size crystal of nanoparticles resulted is 9.21 mm with dislocation value of crystal is 0.012 nm-2. The strains, stress, the energy density of crystal are 1.5 x 10-4 37.31 MPa; 0.72 MPa respectively. The highest texture coefficient value of the crystal is 0.98. This result is supported by morphological analysis using SEM which shows most of the regular cubic-shaped crystals. The synthesis method is suitable for simple and cost-effective synthesis model of MgO nanoparticles.
Development of functionalized hydroxyapatite/poly(vinyl alcohol) composites

NASA Astrophysics Data System (ADS)

Stipniece, Liga; Salma-Ancane, Kristine; Rjabovs, Vitalijs; Juhnevica, Inna; Turks, Maris; Narkevica, Inga; Berzina-Cimdina, Liga

2016-06-01

Based on the well-known pharmaceutical excipient potential of poly(vinyl alcohol) (PVA) and clinical success of hydroxyapatite (HAp), the objective of this work was to fabricate functionalized composite microgranules. PVA was modified with succinic anhydride to introduce carboxyl groups (-COOH), respectively, by reaction between the -OH groups of PVA and succinic anhydride, for attachment of drug molecules. For the first time, the functionalized composite microgranules containing HAp/PVA in the ratio of 1:1 were prepared through in situ precipitation of HAp in modified PVA aqueous solutions followed by spray drying of obtained suspensions. The microgranules were characterized by Fourier-transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), and differential scanning calorimetry (DSC). The presence of -COOH groups was verified by FT-IR, and the amount of functional groups added to PVA molecules (averaging 15 mol%) was determined by nuclear magnetic resonance spectroscopy (NMR). DSC results showed that modification with -COOH groups slightly decreased the thermal stability of PVA. FT-IR and XRD analysis confirmed that the resulting composites contain mainly nanocrystalline HAp and PVA. Moreover, the images taken by FE-SEM revealed that the microgranules consisted of nanosized HAp crystallites homogenously embedded in the PVA matrix. DSC measurements indicated that decomposition mechanism of the HAp/PVA differs from that of pure PVA and occurs at lower temperatures. However, the presence of HAp had minor influence on the thermal decomposition of the PVA modified with succinic anhydride. The investigation of composite microgranules confirmed interaction and integration between the HAp and PVA.
Preparation and characterization of NiW-nHA composite catalyst for hydrocracking

NASA Astrophysics Data System (ADS)

Zhou, Gang; Hou, Yongzhao; Liu, Lei; Liu, Hongru; Liu, Can; Liu, Jing; Qiao, Huiting; Liu, Wenyong; Fan, Yubo; Shen, Shituan; Rong, Long

2012-11-01

The synthesis, characterization and catalytic capability of the NiW-nano-hydroxyapatite (NiW-nHA) composite were investigated in this paper. The NiW-nHA catalyst was prepared by a co-precipitation method. Then Fourier transform infrared (FT-IR) spectroscopy, transmission electron microscopy (TEM), X-ray diffraction (XRD) and energy dispersive spectroscopy (EDX) were used to analyze this material. In addition, the catalytic capacity of the NiW-nHA composite was also examined by FT-IR and gas chromatography (GC). The results of FT-IR analysis indicated that Ni, W and nHA combined closely. TEM observation revealed that this catalyst was needle shaped and the crystal retained a nanometer size. XRD data also suggested that a new phase of CaWO4 appeared and the lattice parameters of nHA changed in this system. nHA was the carrier of metals. The rates of Ni/W-loading were 73.24% and 65.99% according to the EDX data, respectively. Furthermore, the conversion of 91.88% Jatropha oil was achieved at 360 °C and 3 MPa h-1 over NiW-nHA catalyst. The straight chain alkanes ranging from C15 to C18 were the main components in the production. The yield of C15-C18 alkanes was up to 83.56 wt%. The reaction pathway involved hydrocracking of the C&z.dbd;C bonds of these triglycerides from Jatropha oil. This paper developed a novel non-sulfided catalyst to obtain a ``green biofuel'' from vegetable oil.
Preparation and characterization of cross-linked poly (vinyl alcohol)-graphene oxide nanocomposites as an interlayer for Schottky barrier diodes

NASA Astrophysics Data System (ADS)

Badrinezhad, Lida; Bilkan, Çigdem; Azizian-Kalandaragh, Yashar; Nematollahzadeh, Ali; Orak, Ikram; Altindal, Şemsettin

2018-01-01

Cross-linked polyvinyl alcohol (PVA) graphene oxide (GO) nanocomposites were prepared by simple solution-mixing route and characterized by Raman, UV-visible and fourier transform infrared (FT-IR) spectroscopy analysis, X-ray diffraction (XRD) and scanning electron microscopy (SEM) techniques. The XRD pattern and SEM analysis showed significant changes in the nanocomposite structures, and the FT-IR spectroscopy results confirmed the chemical interaction between the GO filler and the PVA matrix. After these morphological characterizations, PVA-GO-based diodes were fabricated and their electrical properties were characterized using current-voltage (I-V) and impedance-voltage-frequency (Z-V-f) measurements at room temperature. Semilogarithmic I-V characteristics of diode showed a good rectifier behavior. The values of C and G/ω increased with decreasing frequency due to the surface/interface states (Nss) which depend on the relaxation time and the frequency of the signal. The voltage, dependent profiles of Nss and series resistance (Rs) were obtained from the methods of high-low frequency capacitance and Nicollian and Brews, respectively. The obtained values of Nss and Rs were attributed to the use of cross-linked PVA-GO interlayer at the Au/n-Si interface.
Size-dependent photocatalytic activity of La0.8Sr0.2MnO3 nanoparticles prepared by hydrothermal synthesis

NASA Astrophysics Data System (ADS)

Rahmani Afje, F.; Ehsani, M. H.

2018-04-01

Synthesize of La0.8Sr0.2MnO3 (LSMO) manganite were carried out in different particle sizes by hydrothermal method. Structural and optical properties of the prepared specimens were studied by x-ray diffraction (XRD), Fourier transform infra-red (FT-IR) spectroscopy, field emission scanning electron microscopy (FESEM), and UV–vis spectroscopy. The XRD study, coupled with the Rietveld refinement, exhibited rhombohedral structure with R-3C space group. Using the FT-IR and FESEM analyses, the perovskite structure of the samples with Nano-rod-like morphologies were inferred. Furthermore, the average sizes of 48.11, 70.99 and 111.45 nm were obtained for the ones sintered at 800, 900, and 1000 °C temperatures, respectively. The optical research showed that band gap energy is about 2.13 eV, being suitable in visible-light photocatalytic activity for water purification from dyes and toxic organic materials. The photo-degradation efficiency for decolorizing methyl orange solution (10 ppm) for various samples (100 ppm) were systematically probed and a strong relation is concluded between particle size and photocatalytic activity.
Improving the dissolution and bioavailability of 6-mercaptopurine via co-crystallization with isonicotinamide.

PubMed

Wang, Jian-Rong; Yu, Xueping; Zhou, Chun; Lin, Yunfei; Chen, Chen; Pan, Guoyu; Mei, Xuefeng

2015-03-01

6-Mercaptopurine (6-MP) is a clinically important antitumor drug. The commercially available form was provided as monohydrate and belongs to BCS class II category. Co-crystallization screening by reaction crystallization method (RCM) and monitored by powder X-ray diffraction led to the discovery of a new co-crystal formed between 6-MP and isonicotinamide (co-crystal 1). Co-crystal 1 was thoroughly characterized by X-ray diffraction, FT-IR and Raman spectroscopy, and thermal analysis. Noticeably, the in vitro and in vivo studies revealed that co-crystal 1 possesses improved dissolution rate and superior bioavailability on animal model. Copyright © 2015 Elsevier Ltd. All rights reserved.
FT-IR spectroscopy: A powerful tool for studying the inter- and intraspecific biodiversity of cultivable non-Saccharomyces yeasts isolated from grape must.

PubMed

Grangeteau, Cédric; Gerhards, Daniel; Terrat, Sebastien; Dequiedt, Samuel; Alexandre, Hervé; Guilloux-Benatier, Michèle; von Wallbrunn, Christian; Rousseaux, Sandrine

2016-02-01

The efficiency of the FT-IR technique for studying the inter- and intra biodiversity of cultivable non-Saccharomyces yeasts (NS) present in different must samples was examined. In first, the capacity of the technique FT-IR to study the global diversity of a given sample was compared to the pyrosequencing method, used as a reference technique. Seven different genera (Aureobasidium, Candida, Cryptococcus, Hanseniaspora, Issatchenkia, Metschnikowia and Pichia) were identified by FT-IR and also by pyrosequencing. Thirty-eight other genera were identified by pyrosequencing, but together they represented less than 6% of the average total population of 6 musts. Among the species identified, some of them present organoleptic potentials in winemaking, particularly Starmerella bacillaris (synonym Candidazemplinina). So in a second time, we evaluated the capacity of the FT-IR technique to discriminate the isolates of this species because few techniques were able to study intraspecific NS yeast biodiversity. The results obtained were validated by using a classic method as ITS sequencing. Biodiversity at strain level was high: 19 different strains were identified from 58 isolates. So, FT-IR spectroscopy seems to be an accurate and reliable method for identifying major genera present in the musts. The two biggest advantages of the FT-IR are the capacity to characterize intraspecific biodiversity of non-Saccharomyces yeasts and the possibility to discriminate a lot of strains. Copyright © 2015 Elsevier B.V. All rights reserved.
Detection of E. coli O157:H7 from ground beef using Fourier transform infrared (FT-IR) spectroscopy and chemometrics.

PubMed

Davis, Reeta; Irudayaraj, Joseph; Reuhs, Bradley L; Mauer, Lisa J

2010-08-01

FT-IR spectroscopy methods for detection, differentiation, and quantification of E. coli O157:H7 strains separated from ground beef were developed. Filtration and immunomagnetic separation (IMS) were used to extract live and dead E. coli O157:H7 cells from contaminated ground beef prior to spectral acquisition. Spectra were analyzed using chemometric techniques in OPUS, TQ Analyst, and WinDAS software programs. Standard plate counts were used for development and validation of spectral analyses. The detection limit based on a selectivity value using the OPUS ident test was 10(5) CFU/g for both Filtration-FT-IR and IMS-FT-IR methods. Experiments using ground beef inoculated with fewer cells (10(1) to 10(2) CFU/g) reached the detection limit at 6 h incubation. Partial least squares (PLS) models with cross validation were used to establish relationships between plate counts and FT-IR spectra. Better PLS predictions were obtained for quantifying live E. coli O157:H7 strains (R(2)> or = 0.9955, RMSEE < or = 0.17, RPD > or = 14) and different ratios of live and dead E. coli O157:H7 cells (R(2)= 0.9945, RMSEE = 2.75, RPD = 13.43) from ground beef using Filtration-FT-IR than IMS-FT-IR methods. Discriminant analysis and canonical variate analysis (CVA) of the spectra differentiated various strains of E. coli O157:H7 from an apathogenic control strain. CVA also separated spectra of 100% dead cells separated from ground beef from spectra of 0.5% live cells in the presence of 99.5% dead cells of E. coli O157:H7. These combined separation and FT-IR methods could be useful for rapid detection and differentiation of pathogens in complex foods.
Fourier transform infrared spectroscopy imaging of live epithelial cancer cells under non-aqueous media.

PubMed

Soh, JunYi; Chueng, Adeline; Adio, Aminat; Cooper, Alan J; Birch, Brian R; Lwaleed, Bashir A

2013-04-01

Fourier transform infrared (FT-IR) imaging is increasingly being applied to biomedical specimens, but strong IR absorption by water complicates live cell imaging. This study investigates the viability of adherent epithelial cells maintained for short periods under mineral oils in order to facilitate live cell spectroscopy using FT-IR with subsequent imaging. The MGH-U1 urothelial or CaCo2 colorectal cancer cell lines were grown on plastic surfaces or mid-range infrared transparent windows. Medium in established cultures was replaced with paraffin mineral oil, or Fluorolube, for up to 2 h, and viability assessed by supravital staining. Drug handling characteristics were also assessed. Imaging of preparations was attempted by reflectance and transmission using a Varian FT-IR microscope. Cells covered by mineral oil remained viable for 2 h, with recovery into normal medium possible. MTT ((3-(4,5-dimethylthlazol-2-yl)-2,5-diphenyl tetrazolium) conversion to crystalline formazan and differential patterns of drug uptake were maintained. The combination of a calcium fluoride substrate, Fluorolube oil, and transmission optics proved best for spectroscopy. Spectral features were used to obtain images of live cells. The viability of cells overlaid with IR transparent oils was assessed as part of a technique to optimise conditions for FT-IR imaging. Images of untreated cells were obtained using both reflectance and transmission. This represents an effective means of imaging live cells by IR spectroscopy, and also means that imaging is not necessarily a terminal event. It also increases options for producing images based on real-time biochemistry in a range of in vitro experimental and 'optical biopsy' contexts.
Visible-light-assisted SLCs template synthesis of sea anemone-like Pd/PANI nanocomposites with high electrocatalytic activity for methane oxidation in acidic medium

NASA Astrophysics Data System (ADS)

Tan, De-Xin; Wang, Yan-Li

2018-03-01

Sea anemone-like palladium (Pd)/polyaniline (PANI) nanocomposites were synthesized via visible-light-assisted swollen liquid crystals (SLCs) template method. The resulting samples were characterized by transmission electron microscopy (TEM), selected area electron diffraction (SAED), energy dispersive spectrometer (EDS), x-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), ultraviolet-visible (UV–vis) absorption spectroscopy and Fourier transform infrared (FT-IR) spectroscopy, respectively. The electrocatalytic properties of Pd/PANI nanocomposites modified glass carbon electrode (GCE) for methane oxidation were investigated by cycle voltammetry (CV) and chronoamperometry. Those dispersed sea anemone-like Pd/PANI nanocomposites had an average diameter of 320 nm. The obtained Pd nanoparticles with an average diameter of about 45 nm were uniformly distributed in PANI matrix. Sea anemone-like Pd/PANI nanocomposites exhibited excellent electrocatalytic activity and stability for oxidation of methane (CH4).
Potential Second-Harmonic Ghost Bands in Fourier Transform Infrared (FT-IR) Difference Spectroscopy of Proteins.

PubMed

Ito, Shota; Kandori, Hideki; Lorenz-Fonfria, Victor A

2018-06-01

Fourier transform infrared (FT-IR) difference absorption spectroscopy is a common method for studying the structural and dynamical aspects behind protein function. In particular, the 2800-1800 cm -1 spectral range has been used to obtain information about internal (deuterated) water molecules, as well as site-specific details about cysteine residues and chemically modified and artificial amino acids. Here, we report on the presence of ghost bands in cryogenic light-induced FT-IR difference spectra of the protein bacteriorhodopsin. The presence of these ghost bands can be particularly problematic in the 2800-1900 cm -1 region, showing intensities similar to O-D vibrations from water molecules. We demonstrate that they arise from second harmonics from genuine chromophore bands located in the 1400-850 cm -1 region, generated by double-modulation artifacts caused from reflections of the IR beam at the sample and at the cryostat windows back to the interferometer (inter-reflections). The second-harmonic ghost bands can be physically removed by placing an optical filter of suitable cutoff in the beam path, but at the cost of losing part of the multiplexing advantage of FT-IR spectroscopy. We explored alternatives to the use of optical filters. Tilting the cryostat windows was effective in reducing the intensity of the second harmonic artifacts but tilting the sample windows was not, presumably by their close proximity to the focal point of the IR beam. We also introduce a simple numerical post-processing approach that can partially, but not fully, correct for second-harmonic ghost bands in FT-IR difference spectra.
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.
Analysis of Chuanxiong Rhizoma and its active components by Fourier transform infrared spectroscopy combined with two-dimensional correlation infrared spectroscopy.

PubMed

Guo, Yizhen; Lv, Beiran; Wang, Jingjuan; Liu, Yang; Sun, Suqin; Xiao, Yao; Lu, Lina; Xiang, Li; Yang, Yanfang; Qu, Lei; Meng, Qinghong

2016-01-15

As complicated mixture systems, active components of Chuanxiong Rhizoma are very difficult to identify and discriminate. In this paper, the macroscopic IR fingerprint method including Fourier transform infrared spectroscopy (FT-IR), the second derivative infrared spectroscopy (SD-IR) and two-dimensional correlation infrared spectroscopy (2DCOS-IR), was applied to study and identify Chuanxiong raw materials and its different segmented production of HPD-100 macroporous resin. Chuanxiong Rhizoma is rich in sucrose. In the FT-IR spectra, water eluate is more similar to sucrose than the powder and the decoction. Their second derivative spectra amplified the differences and revealed the potentially characteristic IR absorption bands and combined with the correlation coefficient, concluding that 50% ethanol eluate had more ligustilide than other eluates. Finally, it can be found from 2DCOS-IR spectra that proteins were extracted by ethanol from Chuanxiong decoction by HPD-100 macroporous resin. It was demonstrated that the above three-step infrared spectroscopy could be applicable for quick, non-destructive and effective analysis and identification of very complicated and similar mixture systems of traditional Chinese medicines. Copyright © 2015 Elsevier B.V. All rights reserved.

Cocrystals of Kemp’s triacid. Part III: Structure of hydrogen-bonded complex of Kemp’s triacid with 1,1,3,3-tetramethylguanidine studied by X-ray and FT-IR methods

NASA Astrophysics Data System (ADS)

Huczyński, Adam; Ratajczak-Sitarz, Małgorzata; Katrusiak, Andrzej; Brzezinski, Bogumil

2008-12-01

The 2:2 hydrogen-bonded complex between Kemp's triacid (KTA) and 1,1,3,3-tetramethylguanidine (TMG) has been synthesised and studied by X-ray diffraction and by FT-IR spectroscopy. Cocrystals of KTA-TMG belong to the monoclinic system and crystallize in the space group is P21 with a = 10.5017(3) Å, b = 7.9504(3) Å, c = 11.8910(4) Å, β = 104.004(4)° and Z = 2. The ring of the KTA monoanion molecule exhibits a chair conformation with all three carboxylic groups in the axial positions and all three methyl groups in the equatorial positions. In the crystal of the complex, cooperative systems involving inter- and intra-molecular hydrogen bonds are formed. In the solid state two protonated TMG molecules and two deprotonated KTA molecules form a dimer in which three-dimensional hydrogen-bonded networks are found.
Synthesis and characterization of CdO nano particles by the sol-gel method

NASA Astrophysics Data System (ADS)

Vadgama, V. S.; Vyas, R. P.; Jogiya, B. V.; Joshi, M. J.

2017-05-01

Cadmium Oxide (CdO) is an inorganic compound and one of the main precursors to other cadmium compounds. It finds applications in cadmium plating, storage batteries, in transparent conducting film, etc. Here, an attempt is made to synthesize CdO nano particles by sol-gel technique. The gel was prepared using cadmium nitrate tetra hydrate (Cd(NO3)2.4H2O) and aqueous ammonium hydroxide (NH4OH) as a precursor. The synthesized powder is further characterized by techniques like Powder X-ray diffraction (XRD), Transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR) and Thermal gravimetric analysis (TGA). Powder XRD analysis suggested the nano-crystalline nature of the sample with the cubic crystal system. Nano scaled particles of spherical morphology with the size ranging from 50-100 nm are observed from TEM images. While, FT-IR study is used to confirm the presence of different functional groups. Thermo-gravimetric analysis suggests the highly thermally stable nature of the samples. The results are discussed.
Immobilized copper(II) macrocyclic complex on MWCNTs with antibacterial activity

NASA Astrophysics Data System (ADS)

Tarlani, Aliakbar; Narimani, Khashayar; Mohammadipanah, Fatemeh; Hamedi, Javad; Tahermansouri, Hasan; Amini, Mostafa M.

2015-06-01

In a new approach, a copper(II) tetraaza macrocyclic complex (CuTAM) was covalently bonded on modified multi-walled carbon nanotubes (MWCNTs). To achieve this purpose, MWCNTs were converted to MWCNT-COCl and then reacted to NH groups of TAM ligand. The prepared material was characterized by Fourier Transform Infrared (FT-IR), X-ray diffraction (XRD), Raman spectroscopy, thermal gravimetric analysis (TGA), and FESEM (field emission scanning electron microscopy). FT-IR and TGA demonstrated the presence of the organic moieties, and XRD proved that the structure of MWCNTs remained intact during the three modification steps. An increase in the ID/IG ratio in Raman spectra confirmed the surface modifications. Finally, the samples were subjected to an antibacterial assessment to compare their biological activity. The antibacterial test showed that the grafted complex on the surface of the nanotube (MWCNT-CO-CuTAM) has higher antibacterial activity against Bacillus subtilis ATCC 6633 than the MWCNT-COOH and CuTAM with 1000 and 2000 μg/mL.
Solvothermal synthesis of fusiform hexagonal prism SrCO{sub 3} microrods via ethylene glycol solution

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

Shi Liange; Du Fanglin

2007-08-07

Fusiform hexagonal prism SrCO{sub 3} microrods were prepared by a simple solvothermal route at 120 deg. C, and characterized by X-ray powder diffraction (XRD), field-emission scanning electron microscopy (FE-SEM) and Fourier transform infrared (FT-IR) spectroscopy. By controlling the content of ethylene glycol (EG), it was found that ethylene glycol (EG) played an important role in the formation of such SrCO{sub 3} microrods. Finally, effects of other solvents on the products, including 1,2-propanediol and glycerin, were also investigated.
Synthesis, characterization and luminescent properties of mixed phase bismuth molybdate-doped with Eu3+ ions

NASA Astrophysics Data System (ADS)

Wang, Liyong; Guo, Xiaoqing; Cai, Xiaomeng; Song, Qingwei; Han, Yuanyuan; Jia, Guang

2018-02-01

Red phosphors of Eu3+-doped bismuth molybdate (BMO) are prepared by a low temperature hydrothermal method assisting with Phenol Formaldehyde resin (PFr), and characterized by X-ray diffraction (XRD) patterns, Fourier transform infrared-spectroscopy (FT-IR), thermogravimetric analyzer (TGA), differential thermal analyzer (DTA), and photoluminescence (PL) spectroscopy. PL properties influence factors including molar ratio of Bi3+ and Mo3+ ions, PFr dosage and dopants concentration are discussed in detail. The results show that BMO can act as a useful host for Eu3+ ions doping, and energy transferring from Bi3+ to Eu3+ achieved efficiently, the BMO phosphors displayed intense red color emission under ultraviolet light excitation.
The detection and discrimination of human body fluids using ATR FT-IR spectroscopy.

PubMed

Orphanou, Charlotte-Maria; Walton-Williams, Laura; Mountain, Harry; Cassella, John

2015-07-01

Blood, saliva, semen and vaginal secretions are the main human body fluids encountered at crime scenes. Currently presumptive tests are routinely utilised to indicate the presence of body fluids, although these are often subject to false positives and limited to particular body fluids. Over the last decade more sensitive and specific body fluid identification methods have been explored, such as mRNA analysis and proteomics, although these are not yet appropriate for routine application. This research investigated the application of ATR FT-IR spectroscopy for the detection and discrimination of human blood, saliva, semen and vaginal secretions. The results demonstrated that ATR FT-IR spectroscopy can detect and distinguish between these body fluids based on the unique spectral pattern, combination of peaks and peak frequencies corresponding to the macromolecule groups common within biological material. Comparisons with known abundant proteins relevant to each body fluid were also analysed to enable specific peaks to be attributed to the relevant protein components, which further reinforced the discrimination and identification of each body fluid. Overall, this preliminary research has demonstrated the potential for ATR FT-IR spectroscopy to be utilised in the routine confirmatory screening of biological evidence due to its quick and robust application within forensic science. Copyright © 2015 Elsevier Ireland Ltd. 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.
Sonochemical fabrication of fluorinated mesoporous titanium dioxide microspheres

NASA Astrophysics Data System (ADS)

Yu, Changlin; Yu, Jimmy C.; Chan, Mui

2009-05-01

A sonochemical-hydrothermal method for preparing fluorinated mesoporous TiO 2 microspheres was developed. Formation of mesoporous TiO 2 and doping of fluorine was achieved by sonication and then hydrothermal treatment of a solution containing titanium isopropoxide, template, and sodium fluoride. The as-synthesized TiO 2 microspheres were characterized by X-ray diffraction (XRD), Fourier translation infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy-dispersive X-ray (EDX) spectroscopy, photoluminescence spectroscopy (PL), and BET surface areas. The P123 template was removed completely during the hydrothermal and washing steps, which was different from the conventional calcination treatment. The as- synthesized TiO 2 microspheres had good crystallinity and high stability. Results from the photocatalytic degradation of methylene blue (MB) showed that fluorination could remarkably improve the photocatalytic activity of titanium dioxide.
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.
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.
Synthesis and photocatalytic degradation study of methylene blue dye under visible light irradiation by Fe1-xBixVO4 solid solutions (0 ≤ x ≤ 1.0)

NASA Astrophysics Data System (ADS)

Bera, Ganesh; Reddy, V. R.; Mal, Priyanath; Das, Pradip; Turpu, G. R.

2018-05-01

The novel hetero-structures Fe1-xBixVO4 solid solutions (0 ≤ x ≤ 1.0) with the two dissimilar end member of FeVO4 - BiVO4, were successfully synthesized by the standard solid state reaction method. The structural and chemical properties of as prepared photo-catalyst samples were characterized by X-ray diffraction (XRD), Raman spectroscopy, Fourier transform infrared spectroscopy (FT-IR) and UV-visible absorption spectroscopy techniques. It is confirmed from the results of XRD, Raman and FT-IR that FeVO4 and BiVO4 are in triclinic (space group P-1 (2)) and monoclinic (space group I2/b (15)) phases respectively. The Bi incorporation into Fe site of FeVO4 emerges as hetero-structures of both the end members of the solid solutions. In addition, the photocatalytic activity in the degradation of methylene blue (MB) dye under visible light irradiation was carried out through UV-visible spectroscopy measurement of photo-catalysts FeVO4, BiVO4 and mixed phases of both photo-catalyst. The results indicate that under visible light irradiation the photocatalytic activity of mixed phases were very effective and higher than the both single phases of the solid solutions. The composition x= 0.25 exhibits an excellent photocatalytic property for the degradation of MB solution under visible light irradiation rather than other.
Preparation of a novel breviscapine-loaded halloysite nanotubes complex for controlled release of breviscapine

NASA Astrophysics Data System (ADS)

Gao, Min; Lu, Liqian; Wang, Xiaoyue; Lin, Houke; Zhou, Qingsong

2017-11-01

For sustain the release rate and prolong half-life of breviscapine in vivo, the breviscapine-loaded halloysite nanotubes complex was prepared. The breviscapine was encapsulated into halloysite nanotubes (HNTs) using a vacuum process. The complex were investigated by scanning electron microscopy (SEM), differential scanning calorimetry (DSC), transmission electron microscope (TEM), X-ray diffraction (XRD) and fourier transform infrared spectroscopy(FT-IR). The formation of breviscapine-loaded HNTs complex was proved by the test results of SEM, DSC, TEM and IR analysise. The results confirmed that breviscapine was successfully loaded in the halloysite nanotubes. Additionally, the in vitro drug release of breviscapine from breviscapine-loaded HNTs complex was investigated, the result indicated this complex has apparent sustained-release effect.
Effect of aging temperature on formation of sol-gel derived fluor-hydroxyapatite nanoparticles.

PubMed

Joughehdoust, S; Behnamghader, A; Jahandideh, R; Manafi, S

2010-04-01

Synthetic hydroxyapatite (HA) has been recognized as one of the most important bone substitute materials in orthopaedics and dentistry over past few decades because of its chemical and biological similarity to the mineral phase of human bone. One solution for reduction the solubility of HA in biological environments is replacing F- by OH in HA structure and forming fluor-hydroxyapatite (FHA) solid solution. In this paper, FHA nanoparticles were successfully synthesized by a sol-gel method. Also, the influence of aging temperature on formation of FHA powder was studied. Equimolar solutions of calcium nitrate tetrahydrate, triethyl phosphite and ammonium fluoride in ethanol were used as Ca, P and F precursors. After aging at different temperatures, the synthesized powders were heat treated at 550 degrees C. The powders were investigated with X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), selected area electron diffraction pattern (SAED), energy dispersive analysis of X-ray (EDAX) and zetasizer measurement. The results of XRD proved the presence of fluorapatite (FA) and HA in all samples. In addition, the formation of FHA was confirmed by FT-IR results. XRD studies also showed that the crystallites were in nanometric scale. At the same time, this result was in good agreement with the result of zetasizer analysis.
Chemical fingerprinting of Arabidopsis using Fourier transform infrared (FT-IR) spectroscopic approaches.

PubMed

Gorzsás, András; Sundberg, Björn

2014-01-01

Fourier transform infrared (FT-IR) spectroscopy is a fast, sensitive, inexpensive, and nondestructive technique for chemical profiling of plant materials. In this chapter we discuss the instrumental setup, the basic principles of analysis, and the possibilities for and limitations of obtaining qualitative and semiquantitative information by FT-IR spectroscopy. We provide detailed protocols for four fully customizable techniques: (1) Diffuse Reflectance Infrared Fourier Transform Spectroscopy (DRIFTS): a sensitive and high-throughput technique for powders; (2) attenuated total reflectance (ATR) spectroscopy: a technique that requires no sample preparation and can be used for solid samples as well as for cell cultures; (3) microspectroscopy using a single element (SE) detector: a technique used for analyzing sections at low spatial resolution; and (4) microspectroscopy using a focal plane array (FPA) detector: a technique for rapid chemical profiling of plant sections at cellular resolution. Sample preparation, measurement, and data analysis steps are listed for each of the techniques to help the user collect the best quality spectra and prepare them for subsequent multivariate analysis.
Characterization of Meldrum's acid derivative 5-(5-Ethyl-1,3,4-thiadiazol-2-ylamino)methylene-2,2-dimethyl-1,3-dioxane-4,6-dione by Raman and FT-IR spectroscopy and DFT calculations

NASA Astrophysics Data System (ADS)

de Toledo, T. A.; da Silva, L. E.; Teixeira, A. M. R.; Freire, P. T. C.; Pizani, P. S.

2015-07-01

In this study, the structural and vibrational properties of Meldrum's acid derivative 5-(5-Ethyl-1,3,4-thiadiazol-2-ylamino)methylene-2,2-dimethyl-1,3-dioxane-4,6-dione, C11H13N3O4S were studied combining experimental techniques such as Raman and FT-IR spectroscopy and density functional theory (DFT) calculations. The Raman and FT-IR spectra were recorded at room conditions in the regions from 80 to 3400 cm-1 and 400 to 4000 cm-1, respectively. Vibrational wavenumbers were predicted using DFT calculations with the hybrid functional B3LYP and basis set 6-31G(d,p). A comparison between experimental and theoretical data is provided for the Raman and FT-IR spectra. The descriptions of the normal modes were carried by means of potential energy distribution (PED).
Honey bee odorant-binding protein 14: effects on thermal stability upon odorant binding revealed by FT-IR spectroscopy and CD measurements.

PubMed

Schwaighofer, Andreas; Kotlowski, Caroline; Araman, Can; Chu, Nam; Mastrogiacomo, Rosa; Becker, Christian; Pelosi, Paolo; Knoll, Wolfgang; Larisika, Melanie; Nowak, Christoph

2014-03-01

In the present work, we study the effect of odorant binding on the thermal stability of honey bee (Apis mellifera L.) odorant-binding protein 14. Thermal denaturation of the protein in the absence and presence of different odorant molecules was monitored by Fourier transform infrared spectroscopy (FT-IR) and circular dichroism (CD). FT-IR spectra show characteristic bands for intermolecular aggregation through the formation of intermolecular β-sheets during the heating process. Transition temperatures in the FT-IR spectra were evaluated using moving-window 2D correlation maps and confirmed by CD measurements. The obtained results reveal an increase of the denaturation temperature of the protein when bound to an odorant molecule. We could also discriminate between high- and low-affinity odorants by determining transition temperatures, as demonstrated independently by the two applied methodologies. The increased thermal stability in the presence of ligands is attributed to a stabilizing effect of non-covalent interactions between odorant-binding protein 14 and the odorant molecule.
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.
Chemometric analysis of attenuated total reflectance infrared spectra of Proteus mirabilis strains with defined structures of LPS.

PubMed

Zarnowiec, Paulina; Mizera, Andrzej; Chrapek, Magdalena; Urbaniak, Mariusz; Kaca, Wieslaw

2016-07-01

Proteus spp. strains are some of the most important pathogens associated with complicated urinary tract infections and bacteremia affecting patients with immunodeficiency and long-term urinary catheterization. For epidemiological purposes, various molecular typing methods have been developed for this pathogen. However, these methods are labor intensive and time consuming. We evaluated a new method of differentiation between strains. A collection of Proteus spp. strains was analyzed by attenuated total reflectance Fourier transform infrared (ATR FT-IR) spectroscopy in the mid-infrared region. ATR FT-IR spectroscopy used in conjunction with a diamond ATR accessory directly produced the biochemical profile of the surface chemistry of bacteria. We conclude that a combination of ATR FT-IR spectroscopy and mathematical modeling provides a fast and reliable alternative for discrimination between Proteus isolates, contributing to epidemiological research. © The Author(s) 2016.
Distribution of Hydroxyl Groups in Kukersite Shale Oil: Quantitative Determination Using Fourier Transform Infrared (FT-IR) Spectroscopy.

PubMed

Baird, Zachariah Steven; Oja, Vahur; Järvik, Oliver

2015-05-01

This article describes the use of Fourier transform infrared (FT-IR) spectroscopy to quantitatively measure the hydroxyl concentrations among narrow boiling shale oil cuts. Shale oil samples were from an industrial solid heat carrier retort. Reference values were measured by titration and were used to create a partial least squares regression model from FT-IR data. The model had a root mean squared error (RMSE) of 0.44 wt% OH. This method was then used to study the distribution of hydroxyl groups among more than 100 shale oil cuts, which showed that hydroxyl content increased with the average boiling point of the cut up to about 350 °C and then leveled off and decreased.
Vibrational spectroscopic study, structural analysis, photophysical properties and theoretical calculations of cis-(±)-2,4,5-tris(pyridin-2-yl)imidazoline

NASA Astrophysics Data System (ADS)

Baldenebro-López, Jesús; Báez-Castro, Alberto; Glossman-Mitnik, Daniel; Höpfl, Herbert; Cruz-Enríquez, Adriana; Miranda-Soto, Valentín; Parra-Hake, Miguel; Campos-Gaxiola, José J.

2017-02-01

cis-(±)-2,4,5-tris(pyridin-2-yl)imidazoline has been fully characterized by FT-IR, FT-Raman, UV-Vis and fluorescence spectroscopy, one- and two-dimensional NMR spectroscopy (1H, 1H-1H gCOSY, 1H-1H gNOESY,13C{1H} ATP, 1H-13C and 1H-15N gHSQC and 1H-13C gHMBC), high-resolution mass spectrometry (HR-FAB+), TG-DSC analysis and low-temperature single-crystal X-ray diffraction analysis. Additionally, the molecular geometry and the vibrational infrared and Raman frequencies were calculated by density functional theory using the M06/6-31G(d) level of theory, showing good agreement with the experimental results. The title compound showed interesting photophysical properties, which were studied experimentally in solution and in the solid state by UV-Vis and fluorescence spectroscopy and compared to the theoretically obtained parameters using TD-DFT calculations. Natural and Mulliken atomic charges and the molecular electrostatic potential (MEP) have been mapped.

Preparation and characterization of biomimetic silk fibroin/chitosan composite nanofibers by electrospinning for osteoblasts culture.

PubMed

Chen, Jyh-Ping; Chen, Shih-Hsien; Lai, Guo-Jyun

2012-03-06

In this study, we have successfully fabricated electrospun bead-free silk fibroin [SF]/chitosan [CS] composite nanofibers [NFs] covering the whole range of CS content (0%, 25%, 50%, 75%, and 100%). SF/CS spinning solutions were prepared in a mixed solvent system of trifluoroacetic acid [TFA] and dichloromethane. The morphology of the NFs was observed by scanning electron microscope, and the average fiber diameter ranges from 215 to 478 nm. Confocal laser scanning microscopy confirms the uniform distribution of SF and CS within the composite NFs. To increase biocompatibility and preserve nanostructure when seeded with cells in culture medium, NFs were treated with an ethanol/ammonia aqueous solution to remove residual TFA and to change SF protein conformation. After the chemical treatment, SF/CS NFs could maintain the original structure for up to 54 days in culture medium. Properties of pristine and chemically treated SF/CS NFs were investigated by Fourier transform infrared spectroscopy [FT-IR], X-ray diffraction [XRD], and thermogravimetry/differential scanning calorimetry [TG/DSC]. Shift of absorption peaks in FT-IR spectra confirms the conformation change of SF from random coil to β-sheet by the action of ethanol, which is also consistent with the SF crystalline diffraction patterns measured by XRD. From TG/DSC analysis, the decomposition temperature peaks due to salt formation from TFA and protonated amines disappeared after chemical treatment, indicating complete removal of TFA by binding with ammonium ions during the treatment. This was also confirmed with the disappearance of F1s peak in X-ray photoelectron spectroscopy spectra and disappearance of TFA salt peaks in FT-IR spectra. The composite NFs could support the growth and osteogenic differentiation of human fetal osteoblastic [hFOB] cells, but each component in the composite NF shows distinct effect on cell behavior. SF promotes hFOB proliferation while CS enhances hFOB differentiation. The composite SF/CS NFs will be suitable for bone tissue engineering applications by choosing a suitable blend composition.PACS: 87.85.jf; 87.85.Rs; 68.37.Hk.
Facile and low temperature route to synthesis of CuS nanostructure in mesoporous material by solvothermal method.

PubMed

Sohrabnezhad, Sh; Zanjanchi, M A; Hosseingholizadeh, S; Rahnama, R

2014-04-05

The synthesis of CuS nanomaterial in MCM-41 matrix has been realized by chemical synthesis between MCM-41, copper sulfate pentahydrate and thiourea via a solvothermal method in ethylene glycol and water, separately. X-ray diffraction analysis (XRD), diffuse reflectance spectroscopy (DRS), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and fourier transform infrared (FT-IR) were used to characterize the products. At synthesized CuS/MCM-41 sample in ethylene glycol, X-ray diffraction and diffuse reflectance spectroscopy showed pure covellite phase of copper sulfide with high crystality. But prepared CuS/MCM-41 sample in water shows the covellite, chalcocite and the djurleite phase of copper sulfide nanostructures. The formation of CuS nanostructures was confirmed by FT-IR. Photocatalytic activity of CuS/MCM-41 nanocomposites was studied for degradation of Methylene Blue (MB) under visible light. The CuS/MCM-41 nanocomposite is more effective nanocatalyst than synthesized CuS/MCM-41 sample in water for degradation of methylene blue. Several parameters were examined, catalyst amount (0.1-1gL(-1)), pH (1-13) and initial concentration of MB (0.96-10ppm). The extent of degradation was estimated from the residual concentration by spectrophotometrically. The support size was obtained in the range 60-145nm by TEM. In the same way, the average size of copper sulfide in CuSMCM-41E and CuS/MCM-41W nanostructures were obtained about 10nm and 16nm, respectively. Copyright © 2013 Elsevier B.V. All rights reserved.
Structure and magnetic properties of SiO{sub 2}/PCL novel sol–gel organic–inorganic hybrid materials

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

Catauro, Michelina, E-mail: michelina.catauro@unina2.it; Bollino, Flavia; Cristina Mozzati, Maria

2013-07-15

Organic–inorganic nanocomposite materials have been synthesized via sol–gel. They consist of an inorganic SiO{sub 2} matrix, in which different percentages of poly(ε-caprolactone) (PCL) have been incorporated. The formation of H-bonds among the carbonyl groups of the polymer chains and Si–OH group of the inorganic matrix has been proved by means of Fourier transform infrared spectroscopy (FT-IR) analysis and has been confirmed by solid-state nuclear magnetic resonance (NMR). X-Ray diffraction (XRD) analysis highlighted the amorphous nature of the synthesized materials. Scanning electron microscope (SEM) micrograph and atomic force microscope (AFM) topography showed their homogeneous morphology and nanostructure nature. Considering the opportunitymore » to synthesize these hybrid materials under microgravity conditions by means of magnetic levitation, superconducting quantum interference device (SQUID) magnetometry has been used to quantify their magnetic susceptibility. This measure has shown that the SiO{sub 2}/PCL hybrid materials are diamagnetic and that their diamagnetic susceptibility is independent of temperature and increases with the PCL amount. - Graphical abstract: Characterization and magnetic properties of SiO{sub 2}/PCL organic–inorganic hybrid materials synthesized via sol–gel. FT-IR, Fourier transform infrared spectroscopy; solid-state NMR: solid-state nuclear magnetic resonance; SQUID: superconducting quantum interference device. - Highlights: • Sol–gel synthesis of SiO{sub 2}/PCL amorphous class I organic–inorganic hybrid materials. • FT-IR and NMR analyses show the hydrogen bonds formation between SiO{sub 2} and PCL. • AFM and SEM analyses confirm that the SiO{sub 2}/PCL are homogenous hybrid materials. • The SQUID measures show that the simples are diamagnetic. • Diamagnetic susceptibility of SiO{sub 2}/PCL materials increases with the PCL amount.« less
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®
Application of Fourier transform infrared (FT-IR) spectroscopy to the study of the modification of epoxidized sunflower oil by acrylation.

PubMed

Irinislimane, Ratiba; Belhaneche-Bensemra, Naima

2012-12-01

Commercial sunflower oil was epoxidized at the laboratory-scale. The epoxidized sunflower oil (ESFO) was modified following the acrylation reaction. Modification was carried out simultaneously using acrylic acid (AA) and triethylamine (TEA). To optimize the reaction conditions, the effects of four temperatures (40, 60, 80, and 100 °C), the ESFO:AA (100:100) ratio, and 0.2% TEA were investigated. The rate of conversion was analyzed with both FT-IR and titration of the oxirane ring. After that, the temperature with the highest conversion was selected and used throughout for all modification reactions. Then, four ratios (100:100, 100:90, 100:80, and 100:75) of ESFO:AA were analyzed at four different concentrations of TEA (0.2, 0.3, 0.4, and 0.5%) to determine the best estimate for both the ESFO:AA ratio and the catalyst concentration. Conversion rate was analyzed using FT-IR spectroscopy by measuring the concentrations of ester, carbonyl, and alcohol groups. Moreover, oxirane-ring concentration was estimated using the titration method (with gentian violet as indicator) and FT-IR spectroscopy (epoxy ring absorptions at 1270 cm(-1) and 877 cm(-1)). Based on conversion yield, the optimum ESFO:AA ratio corresponds to 100:80; the best temperature reaction was at 60 °C, and the best TEA concentration was 0.2%. The critical amounts of reactants needed to reach maximum conversion were established. The final acid value of the acrylated ESFO after washing (pH = 7) was 2.1 mg potassium hydroxide (KOH)·g(-1). All results show that FT-IR spectroscopy is a simple, low-cost, rapid method for investigating the kinetics of a reaction.
DOE Office of Scientific and Technical Information (OSTI.GOV)

Deus, R.C.; Cortés, J.A., E-mail: leandrosrr89@gmail.com; Ramirez, M.A.

Highlights: • CeO{sub 2} nanoparticles were obtained by microwave-hydrothermal method. • Rietveld refinement reveals a cubic structure. • KOH mineralizer agent exhibit weak agglomeration at low temperature and shorter time. - Abstract: The structural and photoluminescent properties at room temperature of CeO{sub 2} and La-doped CeO{sub 2} particles were undertaken. The obtained particles were synthesized by a microwave-assisted hydrothermal method (MAH) under different lanthanum contents. X-ray diffraction (XRD), Fourier transform infrared (FT-IR), Fourier transform Raman (FT-Raman), Ultra-violet spectroscopy (UV–vis) and photoluminescence (PL) measurements were carried out. XRD revealed that the powders are free of secondary phases and crystallize in themore » cubic structure. Raman data show that increasing La doping content increase oxygen vacancies due to lattice expansion. The UV/vis absorption spectroscopy suggested the presence of intermediate energy levels in the band gap of structurally ordered powders. Lanthanum addition creates oxygen vacancies and shifts the photoluminescence in the low energy range leading to intense PL emission.« less
Application of Diffuse Reflectance FT-IR Spectroscopy for the Surface Study of Kevlar Fibers

NASA Astrophysics Data System (ADS)

Chatzi, E. G.; Ishida, H.; Koenig, J. L.

1985-12-01

The surfaces of Kevlar-49 aramid fibers, being used in high-performance composite materials, have been characterized by diffuse reflectance Fourier transform infrared (FT-IR) spectroscopy. Enhancement of the surface selectivity of the technique has been achieved using KBr overlayers. The water absorbed by both the skin and the core of the fibers has been characterized by using this technique and the accessibility of the fiber functional groups has been evaluated.
Vibrational spectra (FT-IR, Raman and MI-IR) of α- and β-alanine

NASA Astrophysics Data System (ADS)

Rosado, Mário Túlio S.; Duarte, Maria Leonor R. S.; Fausto, Rui

1997-06-01

The vibrational spectra of α- and β-alaine molecules in both their zwitterionic and neutral forms are studied by FT-IR, Raman and MI-IR spectroscopy. Together with results from theoretical SCF-MO ab initio calculations, the spectroscopic data obtained under the various experimental conditions used in this study (crystalline phase; low temperature matrix isolated molecules) enable to undertake a detailed assignment of the vibrational spectra of the studied compounds.
Low temperature-fired Ni-Cu-Zn ferrite nanoparticles through auto-combustion method for multilayer chip inductor applications

PubMed Central

2012-01-01

Ferrite nanoparticles of basic composition Ni0.7-xZnxCu0.3Fe2O4 (0.0 ≤ x ≤ 0.2, x = 0.05) were synthesized through auto-combustion method and were characterized for structural properties using X-ray diffraction [XRD], scanning electron microscopy, transmission electron microscopy, and Fourier transform infrared spectroscopy [FT-IR]. XRD analysis of the powder samples sintered at 600°C for 4 h showed the cubic spinel structure for ferrites with a narrow size distribution from 28 to 32 nm. FT-IR showed two absorption bands (v1 and v2) that are attributed to the stretching vibration of tetrahedral and octahedral sites. The effect of Zn doping on the electrical properties was studied using dielectric and impedance spectroscopy at room temperature. The dielectric parameters (ε', ε″, tanδ, and σac) show their maximum value for 10% Zn doping. The dielectric constant and loss tangent decrease with increasing frequency of the applied field. The results are explained in the light of dielectric polarization which is similar to the conduction phenomenon. The complex impedance shows that the conduction process in grown nanoparticles takes place predominantly through grain boundary volume. PACS: 75.50.Gg; 78.20; 77.22.Gm. PMID:22316055
Spectroscopic characterization, antioxidant and antitumour studies of novel bromo substituted thiosemicarbazone and its copper(II), nickel(II) and palladium(II) complexes

NASA Astrophysics Data System (ADS)

Jagadeesh, M.; Lavanya, M.; Kalangi, Suresh K.; Sarala, Y.; Ramachandraiah, C.; Varada Reddy, A.

2015-01-01

A new, slightly distorted octahedral complex of copper(II), square planar complexes of nickel(II) and palladium(II) with 2,4‧-dibromoacetophenone thiosemicarbazone (DBAPTSC) are synthesized. The ligand and the complexes are characterized by FT-IR, FT-Raman, powder X-ray diffraction studies. The IR and Raman data are correlated for the presence of the functional groups which specifically helped in the confirmation of the compounds. In addition, the free ligand is unambiguously characterized by 1H and 13C NMR spectroscopy while the copper(II) complex is characterized by electron paramagnetic resonance spectroscopy (EPR). The g values for the same are found to be 2.246 (g1), 2.012 (g2) and 2.005 (g3) which suggested rhombic distortions. The HOMO-LUMO band gap calculations for these compounds are found to be in between 0.5 and 4.0 eV and these compounds are identified as semiconducting materials. The synthesized ligand and its copper(II), nickel(II) and palladium(II) complexes are subjected to antitumour activity against the HepG2 human hepatoblastoma cell lines. Among all the compounds, nickel(II) complex is found to exert better antitumour activity with 57.6% of cytotoxicity.
FT-IR examination of the development of secondary cell wall in cotton fibers

USDA-ARS?s Scientific Manuscript database

The secondary cell wall development of cotton fibers harvested at 18, 20, 24, 28, 32, 36 and 40 days after flowering was examined using attenuated total reflection Fourier transform-infrared (ATR FT-IR) spectroscopy. Generally, a progressive intensity increase for bands assigned to cellulose Iß was ...
Rapid and quantitative detection of the microbial spoilage in milk using Fourier transform infrared spectroscopy and chemometrics.

PubMed

Nicolaou, Nicoletta; Goodacre, Royston

2008-10-01

Microbiological safety plays a very significant part in the quality control of milk and dairy products worldwide. Current methods used in the detection and enumeration of spoilage bacteria in pasteurized milk in the dairy industry, although accurate and sensitive, are time-consuming. FT-IR spectroscopy is a metabolic fingerprinting technique that can potentially be used to deliver results with the same accuracy and sensitivity, within minutes after minimal sample preparation. We tested this hypothesis using attenuated total reflectance (ATR), and high throughput (HT) FT-IR techniques. Three main types of pasteurized milk - whole, semi-skimmed and skimmed - were used and milk was allowed to spoil naturally by incubation at 15 degrees C. Samples for FT-IR were obtained at frequent, fixed time intervals and pH and total viable counts were also recorded. Multivariate statistical methods, including principal components-discriminant function analysis and partial least squares regression (PLSR), were then used to investigate the relationship between metabolic fingerprints and the total viable counts. FT-IR ATR data for all milks showed reasonable results for bacterial loads above 10(5) cfu ml(-1). By contrast, FT-IR HT provided more accurate results for lower viable bacterial counts down to 10(3) cfu ml(-1) for whole milk and, 4 x 10(2) cfu ml(-1) for semi-skimmed and skimmed milk. Using FT-IR with PLSR we were able to acquire a metabolic fingerprint rapidly and quantify the microbial load of milk samples accurately, with very little sample preparation. We believe that metabolic fingerprinting using FT-IR has very good potential for future use in the dairy industry as a rapid method of detection and enumeration.
Fourier transform infrared spectroscopy of DNA from Borrelia burgdorferi sensu lato and Ixodes ricinus ticks

NASA Astrophysics Data System (ADS)

Muntean, Cristina M.; Stefan, Razvan; Bindea, Maria; Cozma, Vasile

2013-06-01

In this work we present a method for detection of motile and immotile Borrelia burgdorferi genomic DNA, in relation with infectious and noninfectious spirochetes. An FT-IR study of DNA isolated from B. burgdorferi sensu lato strains and from positive and negative Ixodes ricinus ticks, respectively, is reported. Motile bacterial cells from the species B. burgdorferi sensu stricto, Borrelia garinii and Borrelia afzelii were of interest. Also, FT-IR absorbance spectra of DNA from immotile spirochetes of B. burgdorferi sensu stricto, in the absence and presence of different antibiotics (doxycycline, erythromycin, gentamicin, penicillin V or phenoxymethylpenicillin, tetracycline, respectively) were investigated. FT-IR spectra, providing a high molecular structural information, have been analyzed in the wavenumber range 400-1800 cm-1. FT-IR signatures, spectroscopic band assignments and structural interpretations of these DNAs are reported. Spectral differences between FT-IR absorbances of DNAs from motile bacterial cells and immotile spirochetes, respectively, have been found. Particularly, alterations of the sugar-phosphate B-form chain in the case of DNA from Borrelia immotile cells, as compared with DNA from B. burgdorferi sensu lato motile cells have been observed. Based on this work, specific B. burgdorferi sensu lato and I. ricinus DNA-ligand interactions, respectively, might be further investigated using Fourier transform infrared spectroscopy.
Thermal stability of chemically bonded phases on silica gel by photoacoustic FT-IR spectroscopy

NASA Astrophysics Data System (ADS)

Kierys, A.; Pasieczna, S.; Ryczkowski, J.; Goworek, J.

2006-11-01

The temperature resistance of chemically bonded phases on commercial silica gel, LiChrosorb RP 2, RP 8, RP 18 and unmodified Si 60 were tested at different temperatures by photoacoustic FT-IR spectroscopy. The surface characteristics and possible degradation of hydrocarbon phase at higher temperatures were investigated by means of FT-IR/PAS technique. For a series of investigated samples heated up to 423 K, the FT-IR/PAS spectra are similar to those for initial silica samples. The most characteristic band for alkyl modified silica gel, i.e., RP 2, RP 8, and RP 18 was observed between 3200 cm-1 to 2800 cm-1 corresponding to various hydrocarbon species. The bands at 3745 cm-1, 3650 cm-1, and 3430 cm-1 observed in the photoacoustic FT-IR spectra may be ascribed to isolated silanol groups (Si-OH), geminal groups (Si-(OH)2) and hydrogen-bonded Si-OH groups, respectively. For all samples the intensity of the broad band in the region 3800 cm-1 to 3200 cm-1 decreases with the increasing temperature. The additional peak at 3745 cm-1 for chemically bonded long hydrocarbon chain, i.e., C18 and C8 after thermal treatment at 573 K is observed.
Synthesis and Characterization of a New Co-Crystal Explosive with High Energy and Good Sensitivity

NASA Astrophysics Data System (ADS)

Gao, Han; Jiang, Wei; Liu, Jie; Hao, Gazi; Xiao, Lei; Ke, Xiang; Chen, Teng

2017-10-01

A new energetic co-crystal consisting of one of the most powerful explosive molecules 2,4,6,8,10,12-hexanitro-2,4,6,8,10,12-hexaazaisowurtzitane (CL-20) and the military explosive cyclotrimethylenetrinitramine (RDX) was prepared with a simple solvent evaporation method. Scanning electron microscopy (SEM) revealed the morphology of the bar-shaped product, which differed greatly from the morphology of the individual components. Fourier transform infrared spectroscopy (FT-IR), Raman spectroscopy, X-ray diffraction spectrum (XRD), and differential scanning calorimetry (DSC) proved the formation of the co-crystal at the molecular level. The result of mechanical sensitivity test indicated the sensitivity was effectively reduced compared to raw CL-20. Finally, a possible crystallization mechanism was discussed.
Ethylene polymerization on a SiH4-modified Phillips catalyst: detection of in situ produced α-olefins by operando FT-IR spectroscopy.

PubMed

Barzan, Caterina; Groppo, Elena; Quadrelli, Elsje Alessandra; Monteil, Vincent; Bordiga, Silvia

2012-02-21

Ethylene polymerization on a model Cr(II)/SiO(2) Phillips catalyst modified with gas phase SiH(4) leads to a waxy product containing a bimodal MW distribution of α-olefins (M(w) < 3000 g mol(-1)) and a highly branched polyethylene, LLDPE (M(w) ≈ 10(5) g mol(-1), T(m) = 123 °C), contrary to the unmodified catalyst which gives a linear and more dense PE, HDPE (M(w) = 86,000 g mol(-1) (PDI = 7), T(m) = 134 °C). Pressure and temperature resolved FT-IR spectroscopy under operando conditions (T = 130-230 K) allows us to detect α-olefins, and in particular 1-hexene and 1-butene (characteristic IR absorption bands at 3581-3574, 1638 and 1598 cm(-1)) as intermediate species before their incorporation in the polymer chains. The polymerization rate is estimated, using time resolved FT-IR spectroscopy, to be 7 times higher on the SiH(4)-modified Phillips catalyst with respect to the unmodified one.
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.
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
Spectroscopic characterization of nanohydroxyapatite synthesized by molten salt method.

PubMed

Gopi, D; Indira, J; Kavitha, L; Kannan, S; Ferreira, J M F

2010-10-01

Hydroxyapatite (HAP) nanopowders were synthesized by molten salt method at 260 degrees C. The as-prepared powders were characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), scanning electron microscope (SEM) and thermo gravimetric analysis (TGA). With the aid of the obtained results the effect of calcining time on the crystallinity, size and morphology of HAP nanopowders is presented. The HAP nanopowders synthesized by molten salt method consist of pure phase of HAP without any impurities and showed the rod-like morphology without detectable decomposition up to 1100 degrees C. Copyright 2010 Elsevier B.V. All rights reserved.
Fabrication of silica hollow particles using yeast cells as a template

NASA Astrophysics Data System (ADS)

Liao, Shenglan; Lin, Liqin; Chen, Xiaofang; Liu, Jingru; Zhang, Biao

2018-04-01

Inorganic hollow particles have attracted great interest in recent years. In this study, silica micro spheres were produced. Yeast cells were used as a biological template. The silica shell was synthesized by the hydrolysis of tetraethoxysilane (TEOS) in water-alcohol mixtures as solvent using ammonia as a catalyst according to the Stoeber process. Various approaches including X-ray diffraction (XRD), scanning electron microscopy (SEM) and Fourier transformed infrared (FT-IR) spectroscopy were used to characterize the products. The results showed that the thermally treated samples were SiO2 hollow microspheres with a diameter varying between 1-5μm.

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.
Synthesis, physicochemical and optical properties of bis-thiosemicarbazone functionalized graphene oxide

NASA Astrophysics Data System (ADS)

Kumar, Santosh; Wani, Mohmmad Y.; Arranja, Claudia T.; Castro, Ricardo A. E.; Paixão, José A.; Sobral, Abilio J. F. N.

2018-01-01

Fluorescent materials are important for low-cost opto-electronic and biomedical sensor devices. In this study we present the synthesis and characterization of graphene modified with bis-thiosemicarbazone (BTS). This new material was characterized using Fourier transform infrared spectroscopy (FT-IR), Ultraviolet-visible (UV-Vis) and Raman spectroscopy techniques. Further evaluation by X-ray diffraction (XRD), thermo-gravimetric analysis (TGA), differential scanning calorimetry (DSC), scanning electron microscopy (SEM) and atomic-force microscopy (AFM) allowed us to fully characterize the morphology of the fabricated material. The average height of the BTSGO sheet is around 10 nm. Optical properties of BTSGO evaluated by photoluminescence (PL) spectroscopy showed red shift at different excitation wavelength compared to graphene oxide or bisthiosemicarbazide alone. These results strongly suggest that BTSGO material could find potential applications in graphene based optoelectronic devices.
Rapid discrimination of extracts of Chinese propolis and poplar buds by FT-IR and 2D IR correlation spectroscopy

NASA Astrophysics Data System (ADS)

Wu, Yan-Wen; Sun, Su-Qin; Zhao, Jing; Li, Yi; Zhou, Qun

2008-07-01

The extract of Chinese propolis (ECP) has recently been adulterated with that of poplar buds (EPB), because most of ECP is derived from the poplar plant, and ECP and EPB have almost identical chemical compositions. It is very difficult to differentiate them by using the chromatographic methods such as high performance liquid chromatography (HPLC) and gas chromatography (GC). Therefore, how to effectively discriminate these two mixtures is a problem to be solved urgently. In this paper, a rapid method for discriminating ECP and EPB was established by the Fourier transform infrared (FT-IR) spectra combined with the two-dimensional infrared correlation (2D IR) analysis. Forty-three ECP and five EPB samples collected from different areas of China were analyzed by the FT-IR spectroscopy. All the ECP and EPB samples tested show similar IR spectral profiles. The significant differences between ECP and EPB appear in the region of 3000-2800 cm -1 of the spectra. Based on such differences, the two species were successfully classified with the soft independent modeling of class analogy (SIMCA) pattern recognition technique. Furthermore, these differences were well validated by a series of temperature-dependent dynamic FT-IR spectra and the corresponding 2D IR plots. The results indicate that the differences in these two natural products are caused by the amounts of long-chain alkyl compounds (including long-chain alkanes, long-chain alkyl esters and long chain alkyl alcohols) in them, rather than the flavonoid compounds, generally recognized as the bioactive substances of propolis. There are much more long-chain alkyl compounds in ECP than those in EPB, and the carbon atoms of the compounds in ECP remain in an order Z-shaped array, but those in EPB are disorder. It suggests that FT-IR and 2D IR spectroscopy can provide a valuable method for the rapid differentiation of similar natural products, ECP and EPB. The IR spectra could directly reflect the integrated chemical compositions of complicated mixtures, and it may be available for use in further chromatographic analysis.
Obtaining titanium dioxide nanoparticles with spherical shape and antimicrobial properties using M. citrifolia leaves extract by hydrothermal method.

PubMed

M, Sundrarajan; K, Bama; M, Bhavani; S, Jegatheeswaran; S, Ambika; A, Sangili; P, Nithya; R, Sumathi

2017-06-01

In this work, we synthesized titanium dioxide (TiO 2 ) nanoparticles using leaf extract of Morinda citrifolia (M. citrifolia) by the advanced hydrothermal method. The synthesized TiO 2 nanoparticles were characterized by X-ray diffraction (XRD), Fourier transmission infrared (FT-IR), Ultraviolet-visible diffuse reflectance (UV-Vis DRS), Ultraviolet-visible spectroscopy (UV-Vis), Raman spectroscopy, and scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM with EDX) techniques. The XRD major peak at 27.3° corresponds to the (110) lattice plane of tetragonal rutile TiO 2 phase and average crystalline size of nanoparticles is 10nm. The FT-IR result confirmed that TiO 2 nanoparticles and the presences of very few amount of anthraquinone and phenolic compounds of the leaf extract. The obtained nanoparticles were also characterized by UV-Vis DRS absorption spectroscopy and an intense band at 423nm clearly reveals the formation of nanoparticles. SEM images with EDX spectra clearly reveal the size of the nanoparticles, between 15 and 19nm in excellent quasi-spherical shape, by virtue of stabilization (capping) agent. The presence of elements-titanium and oxygen was verified with EDX spectrum. Furthermore, the inhibitory activity of green synthesized TiO 2 nanoparticles was tested against human pathogens like Staphylococcus aureus, Escherichia coli, Bacillus subtilis, Pseudomonas aeruginosa, Candida albicans, and Aspergillus niger by the agar well-diffusion method. The TiO 2 nanoparticles exhibited superior antimicrobial activity against Gram-positive bacteria, demonstrating their antimicrobial value against pathogenic diseases. Copyright © 2017 Elsevier B.V. All rights reserved.
Rapid discrimination of cultivated Codonopsis lanceolata in different ages by FT-IR and 2DCOS-IR

NASA Astrophysics Data System (ADS)

Zhu, Yun; Xu, Chang-hua; Huang, Jian; Li, Guo-yu; Liu, Xin-Hu; Sun, Su-qin; Wang, Jin-hui

2014-07-01

Deodeok (Codonopsis lanceolata) root, a traditional Chinese herbal medicine, has been used to treat lung ailments, rheumatism, menstrual disturbance and bruises with a long history in China and some other Asian countries. In this study, four types of Deodeok with different growth years were discriminated and identified by a Tri-step infrared spectroscopy method (Fourier transform-infrared spectroscopy (conventional FT-IR) coupled with second derivative infrared spectroscopy (SD-IR) and two dimensional correlation infrared spectroscopy(2DCOS-IR) under thermal perturbation. Although only small differences were found in the FT-IR spectra of the samples, the positions and intensities of peaks around 1736, 1634, 1246, 1055, 1033, 818, 779 cm-1 could be considered as the key factors for discriminating them. The differences among them were amplified by their SD-IR spectra. The 2DCOS-IR spectra provided obvious dynamic chemical structure information of Deodeok samples, which present different particular auto peak clusters in the range of 875-1130 cm-1 and 1170-1630 cm-1, respectively. It was demonstrated that the content of triterpene were decreasing when C. lanceolata were growing older, but the relative content of saccharides initially increased and decreased significantly afterwards. It indicated a general trend that the content of polysaccharides accumulated with increasing years. Specifically, the content of polysaccharides accumulated in the root of 2-year-old plant was the lowest, 4-years-old was the highest, and then the content decreased gradually. Furthermore, according to the differences of locations and intensities of auto-peaks in 2D-IR spectra, the integral changes of components were revealed. This study offers a promising method inherent with cost-effective and time-saving to characterize and discriminate the complicated system like Deodeok.
Erratum to: Psammoma bodies in two types of human ovarian tumours: a mineralogical study

NASA Astrophysics Data System (ADS)

Meng, Fanlu; Wang, Changqiu; Li, Yan; Lu, Anhuai; Mei, Fang; Liu, Jianying; Du, Jingyun; Zhang, Yan

2015-06-01

Psammoma body (PB) is a common form of calcification in pathological diagnosis and closely relevant to tumours. This paper focuses on the mineralogical characteristics of PBs in ovarian serous cancer and teratoma by using polarization microscope (POM), environmental scanning electron microscope (ESEM), micro-Fourier transform infrared spectroscopy (micro-FT-IR), transmission electron microscope (TEM), micro-area synchrotron radiation X-ray powder diffraction (μ-SRXRD) and fluorescence (μ-SRXRF). Both the PBs in tissues and separated from eight typical cases were investigated. POM and ESEM observation revealed the inside-out growth pattern of PBs. μ-SRXRD and micro-FT-IR results demonstrated the dominant mineral phase of PBs in ovarian serous cancer and teratoma was AB-type carbonate hydroxyapatite (Ca10[(PO4)6-x-y(CO3)x(HPO4)y][(OH)2-u(CO3)u] with 0 ≤ x,y,u ≤ 2). As observed by ESEM and TEM, the layer-rich PBs in teratoma were up to 70 μm and mainly consisted of 5 nm-wide, 5-12 nm-long columnar crystals; the PBs in ovarian serous cancer with a maximum diameter of 35 μm were composed of slightly longer columnar crystals and granulates with 20-100 nm in diameter. The selected area electron diffraction patterns showed dispersed polycrystalline diffraction rings with arching behavior of (002) diffraction, indicating the aggregated nanocrystals grew in the preferred orientation of (002) face. The EDX and μ-SRXRF results together indicated the existence of Na, Mg, Zn and Sr in PBs. These detailed mineralogical characteristics may help uncover the nature of the pathological PBs in ovary.
Psammoma bodies in two types of human ovarian tumours: a mineralogical study

NASA Astrophysics Data System (ADS)

Fanlu, Meng; Changqiu, Wang; Yan, Li; Anhuai, Lu; Fang, Mei; Jianying, Liu; Jingyun, Du; Yan, Zhang

2015-06-01

Psammoma body (PB) is a common form of calcification in pathological diagnosis and closely relevant to tumours. This paper focuses on the mineralogical characteristics of PBs in ovarian serous cancer and teratoma by using polarization microscope (POM), environmental scanning electron microscope (ESEM), micro-Fourier transform infrared spectroscopy (micro-FT-IR), transmission electron microscope (TEM), micro-area synchrotron radiation X-ray powder diffraction (μ-SRXRD) and fluorescence (μ-SRXRF). Both the PBs in tissues and separated from eight typical cases were investigated. POM and ESEM observation revealed the inside-out growth pattern of PBs. μ-SRXRD and micro-FT-IR results demonstrated the dominant mineral phase of PBs in ovarian serous cancer and teratoma was AB-type carbonate hydroxyapatite (Ca10[(PO4)6-x-y(CO3)x(HPO4 2-)y][(OH)2-u(CO3)u] with 0 ≤ x,y,u ≤ 2). As observed by ESEM and TEM, the layer-rich PBs in teratoma were up to 70 μm and mainly consisted of 5 nm-wide, 5-12 nm-long columnar crystals; the PBs in ovarian serous cancer with a maximum diameter of 35 μm were composed of slightly longer columnar crystals and granulates with 20-100 nm in diameter. The selected area electron diffraction patterns showed dispersed polycrystalline diffraction rings with arching behavior of (002) diffraction, indicating the aggregated nanocrystals grew in the preferred orientation of (002) face. The EDX and μ-SRXRF results together indicated the existence of Na, Mg, Zn and Sr in PBs. These detailed mineralogical characteristics may help uncover the nature of the pathological PBs in ovary.
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.
Selective determination of gold(III) ion using CuO microsheets as a solid phase adsorbent prior by ICP-OES measurement.

PubMed

Rahman, Mohammed M; Khan, Sher Bahadar; Marwani, Hadi M; Asiri, Abdullah M; Alamry, Khalid A; Al-Youbi, Abdulrahman O

2013-01-30

We have prepared calcined CuO microsheets (MSs) by a wet-chemical process using reducing agents in alkaline medium and characterized by UV/vis., fourier transform infrared (FT-IR) spectroscopy, powder X-ray diffraction (XRD), and field-emission scanning electron microscopy (FESEM) etc. The detailed structural, compositional, and optical characterizations of the MSs were evaluated by XRD pattern, FT-IR, X-ray photoelectron spectroscopy (XPS), and UV-vis spectroscopy, respectively which confirmed that the obtained MSs are well-crystalline CuO and possessed good optical properties. The CuO MSs morphology was investigated by FESEM, which confirmed that the calcined nanomaterials were sheet-shaped and grown in large-quantity. Here, the efficiency of the CuO MS was applied for a selective adsorption of gold(III) ion prior to its detection by inductively coupled plasma-optical emission spectrometry (ICP-OES). The selectivity of CuO MSs towards various metal ions, including Au(III), Cd(II), Co(II), Cr(III), Fe(III), Pd(II), and Zn(II) was analyzed. Based on the adsorption isotherm study, it was confirmed that the selectivity of MSs phase was mostly towards Au(III) ion. The static adsorption capacity for Au(III) was calculated to be 57.0 mg g(-1). From Langmuir adsorption isotherm, it was confirmed that the adsorption process was mainly monolayer-adsorption onto a surface containing a finite number of adsorption sites. Copyright © 2012 Elsevier B.V. All rights reserved.
Beyond Fourier Transform Infrared Spectroscopy: External Cavity Quantum Cascade Laser-Based Mid-infrared Transmission Spectroscopy of Proteins in the Amide I and Amide II Region.

PubMed

Schwaighofer, Andreas; Montemurro, Milagros; Freitag, Stephan; Kristament, Christian; Culzoni, María J; Lendl, Bernhard

2018-05-24

In this work, we present a setup for mid-IR measurements of the protein amide I and amide II bands in aqueous solution. Employing a latest generation external cavity-quantum cascade laser (EC-QCL) at room temperature in pulsed operation mode allowed implementing a high optical path length of 31 μm that ensures robust sample handling. By application of a data processing routine, which removes occasionally deviating EC-QCL scans, the noise level could be lowered by a factor of 4. The thereby accomplished signal-to-noise ratio is better by a factor of approximately 2 compared to research-grade Fourier transform infrared (FT-IR) spectrometers at equal acquisition times. Employing this setup, characteristic spectral features of three representative proteins with different secondary structures could be measured at concentrations as low as 1 mg mL -1 . Mathematical evaluation of the spectral overlap confirms excellent agreement of the quantum cascade laser infrared spectroscropy (QCL-IR) transmission measurements with protein spectra acquired by FT-IR spectroscopy. The presented setup combines performance surpassing FT-IR spectroscopy with large applicable optical paths and coverage of the relevant spectral range for protein analysis. This holds high potential for future EC-QCL-based protein studies, including the investigation of dynamic secondary structure changes and chemometrics-based protein quantification in complex matrices.
One-step synthesis and characterizations of cerium oxide nanoparticles in an ambient temperature via Co-precipitation method

NASA Astrophysics Data System (ADS)

Pujar, Malatesh S.; Hunagund, Shirajahammad M.; Desai, Vani R.; Patil, Shivaprasadgouda; Sidarai, Ashok H.

2018-04-01

We report the simple Co-precipitation method for the synthesis of Cerium oxide (CeO2) nanoparticles (NPs) in an ambient temperature. We have taken the Cerium (III) nitrate hexahydrate (Ce(NO3)3.6H2O) and Sodium hydroxide (NaOH) as the precursors. The obtained NPs were analyzed using the UV-Vis spectrophotometer, Fourier transform infrared spectroscopy (FT-IR) and X-ray diffraction (XRD). The obtained results signify that UV-Vis spectrum exhibited a well-defined absorption peak at 274 nm and the estimated energy gap (Eg) is 4.05 eV. The FT-IR analysis provides the supporting evidence for the presence of bonding of O-H, nitrates, alcohols and O-Ce-O vibrations. The XRD result reveals that the synthesized CeO2 NPs was crystallite with cubic phase structure and the estimated average crystallite size of CeO2 NPs using Scherer's and W-H method was significantly different due to their assumptions. Further, it is purposed to study their photocatalytic biological activities.
Novel Isoniazid cocrystals with aromatic carboxylic acids: Crystal engineering, spectroscopy and thermochemical investigations

NASA Astrophysics Data System (ADS)

Diniz, Luan F.; Souza, Matheus S.; Carvalho, Paulo S.; da Silva, Cecilia C. P.; D'Vries, Richard F.; Ellena, Javier

2018-02-01

Four novel cocrystals of the anti-tuberculosis drug Isoniazid (INH), including two polymorphs, with the aromatic carboxylic acids p-nitrobenzoic (PNBA), p-cyanobenzoic (PCNBA) and p-aminobenzoic (PABA) were rationally designed and synthesized by solvent evaporation. Aiming to explore the possible supramolecular synthons of this API, these cocrystals were fully characterized by X-ray diffraction (SCXRD, PXRD), spectroscopic (FT-IR) and thermal (TGA, DSC, HSM) techniques. The cocrystal formation was found to be mainly driven by the synthons formed by the pyridine and hydrazide moieties. In both INH-PABA polymorphs, the COOH acid groups are H-bonded to pyridine and hydrazide groups giving rise to the acid⋯pyridine and acid⋯hydrazide heterosynthons. In INH-PNBA and INH-PCNBA cocrystals these acid groups are only related to the pyridine moiety. In addition to the structural study, supramolecular and Hirshfeld surface analysis were also performed based on the structural data. The cocrystals were identified from the FT-IR spectra and their thermal behaviors were studied by a combination of DSC, TGA and HSM techniques.
Experimental and theoretical studies of the molecular structure of 7-Methyl-3-[(3-methyl-3-mesityl-cyclobutyl]-5-phenyl-5H-thiazolo[3,2-α]pyrimidine-6-carboxylic acid ethyl ester

NASA Astrophysics Data System (ADS)

Acar, Betül; Yilmaz, Ibrahim; Çalışkan, Nezihe; Cukurovali, Alaaddin

2017-07-01

In this work, the title molecule, 7-Methyl-3-[(3-methyl-3-mesityl-cyclobutyl]-5-phenyl-5H-thiazolo[3,2-α]pyrimidine-6-carboxylic acid ethyl ester (C30H34N2O2S1), was synthesized and characterized by FT-IR spectroscopy and single crystal X-ray diffraction. The compound crystallizes in the triclinic space group P21/c. with Z = 4, a = 14.1988(6), b = 19.0893(5), c = 10.1325(4) Å, V = 2674.56(17) A3. The optimized structure parameters of the studied molecule was determined theoretically using HF/6-31G(d) and B3LYP/6-31G(d) methods for ground state, and compared with previously reported experimental findings. The calculated harmonic vibrational frequencies are scaled and they are compared with experimental frequencies obtained by FT-IR spectra. The electronic properties, such as HOMO and LUMO energies, and molecular electrostatic potential (MEP) are also performed.
XRD and FTIR studies the effect of heat treatment and doping the transition metal oxide on LiNbO3 and LiNb3O8 nano-crystallite phases in lithium borate glass system.

PubMed

Kashif, Ismail; Soliman, Ashia A; Sakr, Elham M; Ratep, Asmaa

2013-09-01

Glasses of various compositions in the system 90 Li2B4O7-10 Nb2O5 mixed with T.M ions (where T.M is the transition metal) were prepared by quenching technique. Heat-treatment of the parent glasses was performed at 540, 570 and 620 °C, for 5 and 16 h. The glass structure evolution during the controlled crystallization was examined by XRD and FT-IR spectroscopy analysis. The crystalline phases present in the glass ceramics were identified via X-ray diffraction as a function of heat treatment. The FT-IR data propose for these glasses and heat-treated glass network structures mainly built by: di-, tri-, tetra-, penta-and ortho-borate groups. It was found that the quantitative evolution of these various borate species in the glass structures is influenced by the transition metal. A detailed discussion relating to the N4 evolution with the T.M content was made. Copyright © 2013 Elsevier B.V. All rights reserved.
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.
Highly crystalline zinc incorporated hydroxyapatite nanorods' synthesis, characterization, thermal, biocompatibility, and antibacterial study

NASA Astrophysics Data System (ADS)

Udhayakumar, Gayathri; Muthukumarasamy, N.; Velauthapillai, Dhayalan; Santhosh, Shanthi Bhupathi

2017-10-01

Highly crystalline zinc incorporated hydroxyapatite (Zn-HAp) nanorods have been synthesized using microwave irradiation method. To improve bioactivity and crystallinity of pure HAp, zinc was incorporated into it. As-synthesized samples were characterized by Fourier transform-infrared spectroscopy (FT-IR), X-ray diffraction, field-emission scanning electron microscopy (FESEM), energy dispersive X-ray analysis (EDAX), high-resolution transmission electron microscopy (HRTEM), and the thermal and crystallinity behavior of Zn-HAp nanoparticle were studied by thermogravimetry (TGA) and differential scanning calorimetry (DSC). Antibacterial activity of the as-synthesized nanorods was evaluated against two prokaryotic strains ( Escherichia coli and Staphylococcus aureus). The FT-IR studies show the presence of hydroxide and phosphate functional groups. HRTEM and FESEM images showed highly crystalline rod-shaped nanoparticles with the diameter of about 50-60 nm. EDAX revealed the presence of Ca, Zn, P, and O in the prepared samples. The crystallinity and thermal stability were further confirmed by TGA-DSC analysis. The biocompatibility evaluation results promoted that the Zn-HAp nanorods are biologically active apatites and potentially promising bone-substitute biomaterials for orthopaedic application.
Assessment of the Effects Exerted by Acid and Alkaline Solutions on Bone: Is Chemistry the Answer?

PubMed

Amadasi, Alberto; Camici, Arianna; Porta, Davide; Cucca, Lucia; Merli, Daniele; Milanese, Chiara; Profumo, Antonella; Rassifi, Nabila; Cattaneo, Cristina

2017-09-01

The treatment of corpses with extremely acid or basic liquids is sometimes performed in criminal contexts. A thorough characterization by chemical analysis may provide further help to macroscopic and microscopic analysis; 63 porcine bone samples were treated with solutions at different pH (1-14) for immersion periods up to 70 days, as well as in extremely acidic sulfuric acid solutions (9 M/18 M) and extremely basic sodium hydroxide. Inductively coupled optical emission spectrometry (ICP-OES)/plasma mass spectrometry (ICP-MS), Fourier transform infrared spectroscopy (FT-IR), energy dispersive X-ray analysis (EDX), X-ray powder diffraction (XRPD), and scanning electron microscopy (SEM) showed that only the sulfuric acid solution 18 M was able to completely dissolve the sample. In addition, chemical analysis allowed to recognize the contact between bone and substances. Hydrated calcium sulfate arose from extreme pH. The possibility of detecting the presence of human material within the residual solution was demonstrated, especially with FT-IR, ICP-OES, and EDX. © 2017 American Academy of Forensic Sciences.
Antimicrobial activity of biopolymeric thin films containing flavonoid natural compounds and silver nanoparticles fabricated by MAPLE: A comparative study

NASA Astrophysics Data System (ADS)

Cristescu, R.; Visan, A.; Socol, G.; Surdu, A. V.; Oprea, A. E.; Grumezescu, A. M.; Chifiriuc, M. C.; Boehm, R. D.; Yamaleyeva, D.; Taylor, M.; Narayan, R. J.; Chrisey, D. B.

2016-06-01

The purpose of this study was to investigate the interactions between microorganisms, including the planktonic and adherent organisms, and biopolymer (polyvinylpyrrolidone), flavonoid (quercetin dihydrate and resveratrol)-biopolymer, and silver nanoparticles-biopolymer composite thin films that were deposited using matrix assisted pulsed laser evaporation (MAPLE). A pulsed KrF* excimer laser source was used to deposit the aforementioned composite thin films, which were characterized using Fourier transform infrared spectroscopy (FT-IR), infrared microscopy (IRM), scanning electron microscopy (SEM), Grazing incidence X-ray diffraction (GIXRD) and atomic force microscopy (AFM). The antimicrobial activity of thin films was quantified using an adapted disk diffusion assay against Gram-positive and Gram-negative bacteria strains. FT-IR, AFM and SEM studies confirmed that MAPLE may be used to fabricate thin films with chemical properties corresponding to the input materials as well as surface properties that are appropriate for medical use. The silver nanoparticles and flavonoid-containing films exhibited an antimicrobial activity both against Gram-positive and Gram-negative bacterial strains demonstrating the potential use of these hybrid systems for the development of novel antimicrobial strategies.
Polyaniline-Cadmium Ferrite Nanostructured Composite for Room-Temperature Liquefied Petroleum Gas Sensing

NASA Astrophysics Data System (ADS)

Kotresh, S.; Ravikiran, Y. T.; Tiwari, S. K.; Vijaya Kumari, S. C.

2017-08-01

We introduce polyaniline-cadmium ferrite (PANI-CdFe2O4) nanostructured composite as a room-temperature-operable liquefied petroleum gas (LPG) sensor. The structure of PANI and the composite prepared by chemical polymerization was characterized by Fourier-transform infrared (FT-IR) spectroscopy, x-ray diffraction (XRD) analysis, and field-emission scanning electron microscopy. Comparative XRD and FT-IR analysis confirmed CdFe2O4 embedded in PANI matrix with mutual interfacial interaction. The nanostructure of the composite was confirmed by transmission electron microscopy. A simple LPG sensor operable at room temperature, exclusively based on spin-coated PANI-CdFe2O4 nanocomposite, was fabricated with maximum sensing response of 50.83% at 1000 ppm LPG. The response and recovery time of the sensor were 50 s and 110 s, respectively, and it was stable over a period of 1 month with slight degradation of 4%. The sensing mechanism is discussed on the basis of the p- n heterojunction barrier formed at the interface of PANI and CdFe2O4.
Electron paramagnetic resonance and FT-IR spectroscopic studies of glycine anhydride and betaine hydrochloride

NASA Astrophysics Data System (ADS)

Halim Başkan, M.; Kartal, Zeki; Aydın, Murat

2015-12-01

Gamma irradiated powders of glycine anhydride and betaine hydrochloride have been investigated at room temperature by electron paramagnetic resonance (EPR). In these compounds, the observed paramagnetic species were attributed to the R1 and R2 radicals, respectively. It was determined that the free electron interacted with environmental protons and 14N nucleus in both radicals. The EPR spectra of gamma irradiated powder samples remained unchanged at room temperature for two weeks after irradiation. Also, the Fourier Transform Infrared (FT-IR), FT-Raman and thermal analyses of both compounds were investigated. The functional groups in the molecular structures of glycine anhydride and betaine hydrochloride were identified by vibrational spectroscopies (FT-IR and FT-Raman).

[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.
Hierarchical mesosilicalite nanoformulation integrated with cisplatin exhibits target-specific efficient anticancer activity

NASA Astrophysics Data System (ADS)

Jermy, B. Rabindran; Acharya, Sadananda; Ravinayagam, Vijaya; Alghamdi, Hajer Saleh; Akhtar, Sultan; Basuwaidan, Rehab S.

2018-04-01

Hierarchically structured zeolitic ZSM-5 and meso MCM-41 interlinked domain had an impeccable use as catalysis in many applications. The aim of the study was to develop a new drug delivery nanoformulation, specifically, cisplatin/mesosilicalite using top-down approach for cancer therapy. Hierarchical mesosilicalite with variable porosity was synthesized using alkaline molar solution (0.2 and 0.7 M NaOH) and was loaded with cisplatin through equilibrium adsorption technique. Physico-chemical properties of the nanoformulation (IAUM-56—Imam Abdulrahman Bin Faisal University Mesosilicalite-56) were characterized using X-ray diffraction, surface area analysis (BET), Fourier transformed infrared spectroscopy (FT-IR), diffuse reflectance UV-Vis spectroscopy, and transmission electron microscopy. Drug release study and anticancer activity were assayed on HeLa and MCF7 cancer cells using MTT assay. X-ray diffraction pattern showed interrelated meso- and microphases, while BET analysis revealed considerable mesoporosity formation with a remodulation of isotherm hysteresis indicating the presence of hierarchical pores. FT-IR showed the presence of nanozeolitic subunits into mesostructure with a band at about 550 cm-1. IAUM-56 demonstrated high cytotoxic activity against HeLa cancer cells with an LC50 of 0.02 mg/ml, MCF7 cancer cells with an LC50 of 0.05 mg/ml, and less toxic to normal fibroblast cells with an LC50 of approximately ten times higher at 0.5 mg/ml. Overall, IAUM-56 showed a high rate of sustained release of cisplatin imparting target specific cytotoxic effect against tumor cells with at least tenfold lower toxicity on normal fibroblast cells. Our nanoformulation has the potential use in cancer therapy as a targeted drug delivery system.
Evaluation of a setting reaction pathway in the novel composite TiHA-CSD bone cement by FT-Raman and FT-IR spectroscopy

NASA Astrophysics Data System (ADS)

Paluszkiewicz, Czesława; Czechowska, Joanna; Ślósarczyk, Anna; Paszkiewicz, Zofia

2013-02-01

The aim of this study was to determine a setting reaction pathway in a novel, surgically handy implant material, based on calcium sulfate hemihydrate (CSH) and titanium doped hydroxyapatite (TiHA). The previous studies confirmed superior biological properties of TiHA in comparison to the undoped hydroxyapatite (HA) what makes it highly attractive for future medical applications. In this study the three types of titanium modified HA powders: untreated, calcined at 800 °C, sintered at 1250 °C and CSH were used to produce bone cements. The Fourier Transform-InfraRed (FT-IR) spectroscopy and Raman spectroscopy were applied to evaluate processes taking place during the setting of the studied materials. Our results undoubtedly confirmed that the reaction pathways and the phase compositions differed significantly for set cements and were dependent on the initial heat treatment of TiHA powder. Final materials were multiphase composites consisting of calcium sulfate dihydrate, bassanite, tricalcium phosphate, hydroxyapatite and calcium titanate (perovskite). The FT-IR and Scanning Electron Microscopy (SEM) measurements performed after the incubation of the cement samples in the simulated body fluid (SBF), indicate on high bioactive potential of the obtained bone cements.
The study of the changes in the biochemical and mineral contents of bones of Catla catla due to lead intoxication.

PubMed

Palaniappan, P L R M; Krishnakumar, N; Vadivelu, M; Vijayasundaram, V

2010-02-01

In the present study, an attempt has been made to analyze the changes in the biochemical and mineral contents of lead-intoxicated bones of Catla catla at subchronic (15.5 ppm) exposure, and also to determine whether the effects of Pb intoxication can be reversed with the chelating agent meso 2, 3-dimercaptosuccinic acid (DMSA) on the bones of freshwater fingerlings Catla catla by using Fourier transform infrared (FT-IR) spectroscopy, X-ray diffraction (XRD), and atomic absorption spectrophotometer techniques. The FT-IR spectra of the lead-exposed bones show significant alteration in the biochemical constituents. The XRD analysis showed a decrease in crystallinity due to lead exposure. Further, the Ca, Mg, and P contents of the lead-exposed bones were less than those of the control group, and there was an increase in the mineral contents of the bones after DMSA treatment. In conclusion, the present study suggests that the subchronic lead exposure results in severe loss of bone minerals. The overall decrease in the FT-IR band intensity of Pb-exposed bones relative to the control indicates a decrease in the biochemical constituents like proteins and lipids. The increase in the band intensity after treatment with chelating agent DMSA indicates increased biochemical constituents, showing that the subchronic effects of lead can be reversed by DMSA. The amide I bands observed at 1654 cm(-1) in the present study suggest that the protein is dominated by alpha-helical structure.
Structure, spectra and thermal, mechanical, Faraday rotation properties of novel diamagnetic SeO2-PbO-Bi2O3-B2O3 glasses

NASA Astrophysics Data System (ADS)

Chen, Qiuling; Su, Kai; Li, Yantao; Zhao, Zhiwei

2018-06-01

Faraday rotation diamagnetic glass has attracted research attentions in photonics, sensing and magneto optical devices due to their high refractive index, wide transmittance in UV and Fourier transform infrared (FT-IR) range and temperature independent Faraday rotation. Selenite modified heavy metal oxides glasses with composition of xSeO2-(10-x) B2O3-45PbO-45Bi2O3 (x = 0, 1, 5 and 10mol%) and 15%SeO2-40%PbO-45%Bi2O3 have been fabricated by melt-quenching method in present study. The influence of SeO2 on glass forming ability, thermal, mechanical properties and Faraday rotation were evaluated through X-ray Diffraction (XRD), Fourier transforms infrared spectra (FT-IR), Raman, X-ray photoelectron spectroscopy (XPS), differential scanning calorimetry (DSC), Vicker's hardness and Verdet constant measurements. XRD spectra reveal that the good vitrification was achieved for glass with SeO2 amounts ≤10% even without B2O3. FT-IR, Raman and XPS spectra ascertain the existence of characteristic vibration of SeO4, SeO3, PbO4, BiO3 and BO3 units. The incorporation of SeO2 increases the connectivity of glassy network by increasing the Tg, thermal stability and mechanical hardness. The small band gap, high polarizable Se4+ ions and isolated SeO3 units contribute to Faraday rotation improvement.
Analysis of Roman age wall paintings found in Pordenone, Trieste and Montegrotto.

PubMed

Mazzocchin, G A; Agnoli, F; Salvadori, M

2004-10-20

The aim of the present work is the study of many fragments of wall painting from archaeological excavations in three different Roman age sites dating back to the I Century before Common Era: Pordenone (località Torre); Trieste (Crosada) and Padova (Montegrotto). The techniques used were optical microscopy, scanning electron microscopy (SEM), equipped with a EDS microanalysis detector, X-rays powder diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), Fourier transform Raman spectroscopy (FT-Raman) and electron paramagnetic resonance (EPR) spectroscopy. The identified pigments were: cinnabar, hematite, celadonite, glauconite, cuprorivaite (Egyptian blue), yellow and red ochre, calcite, limonite, coal black. In general, the mortar preparation did not correspond to the complex procedure suggested by Vitruvius (De Architectura), but generally showed a porous layer, with crushed grains under the pigment layer. In some cases, two superimposed pigment layers were found: yellow superimposed on both red and pink, black on pink, green on black. The slight differences we found in the use of the pigments in the three studied sites might show that the same technology, culture and taste spread all over the Roman Empire in North Eastern Italy (X(a) Regio Venetia et Histria).
Fourier transform infrared spectroscopy as a metabolite fingerprinting tool for monitoring the phenotypic changes in complex bacterial communities capable of degrading phenol.

PubMed

Wharfe, Emma S; Jarvis, Roger M; Winder, Catherine L; Whiteley, Andrew S; Goodacre, Royston

2010-12-01

The coking process produces great volumes of wastewater contaminated with pollutants such as cyanides, sulfides and phenolics. Chemical and physical remediation of this wastewater removes the majority of these pollutants; however, these processes do not remove phenol and thiocyanate. The removal of these compounds has been effected during bioremediation with activated sludge containing a complex microbial community. In this investigation we acquired activated sludge from an industrial bioreactor capable of degrading phenol. The sludge was incubated in our laboratory and monitored for its ability to degrade phenol over a 48 h period. Multiple samples were taken across the time-course and analysed by Fourier transform infrared (FT-IR) spectroscopy. FT-IR was used as a whole-organism fingerprinting approach to monitor biochemical changes in the bacterial cells during the degradation of phenol. We also investigated the ability of the activated sludge to degrade phenol following extended periods (2-131 days) of storage in the absence of phenol. A reduction was observed in the ability of the microbial community to degrade phenol and this was accompanied by a detectable biochemical change in the FT-IR fingerprint related to cellular phenotype of the microbial community. In the absence of phenol a decrease in thiocyanate vibrations was observed, reflecting the ability of these communities to degrade this substrate. Actively degrading communities showed an additional new band in their FT-IR spectra that could be attributed to phenol degradation products from the ortho- and meta-cleavage of the aromatic ring. This study demonstrates that FT-IR spectroscopy when combined with chemometric analysis is a very powerful high throughput screening approach for assessing the metabolic capability of complex microbial communities. © 2010 Society for Applied Microbiology and Blackwell Publishing Ltd.
Fourier transform-infrared spectroscopic methods for microbial ecology: analysis of bacteria, bacteria-polymer mixtures and biofilms

NASA Technical Reports Server (NTRS)

Nichols, P. D.; Henson, J. M.; Guckert, J. B.; Nivens, D. E.; White, D. C.

1985-01-01

Fourier transform-infrared (FT-IR) spectroscopy has been used to rapidly and nondestructively analyze bacteria, bacteria-polymer mixtures, digester samples and microbial biofilms. Diffuse reflectance FT-IR (DRIFT) analysis of freeze-dried, powdered samples offered a means of obtaining structural information. The bacteria examined were divided into two groups. The first group was characterized by a dominant amide I band and the second group of organisms displayed an additional strong carbonyl stretch at approximately 1740 cm-1. The differences illustrated by the subtraction spectra obtained for microbes of the two groups suggest that FT-IR spectroscopy can be utilized to recognize differences in microbial community structure. Calculation of specific band ratios has enabled the composition of bacteria and extracellular or intracellular storage product polymer mixtures to be determined for bacteria-gum arabic (amide I/carbohydrate C-O approximately 1150 cm-1) and bacteria-poly-beta-hydroxybutyrate (amide I/carbonyl approximately 1740 cm-1). The key band ratios correlate with the compositions of the material and provide useful information for the application of FT-IR spectroscopy to environmental biofilm samples and for distinguishing bacteria grown under differing nutrient conditions. DRIFT spectra have been obtained for biofilms produced by Vibrio natriegens on stainless steel disks. Between 48 and 144 h, an increase in bands at approximately 1440 and 1090 cm-1 was seen in FT-IR spectra of the V. natriegens biofilm. DRIFT spectra of mixed culture effluents of anaerobic digesters show differences induced by shifts in input feedstocks. The use of flow-through attenuated total reflectance has permitted in situ real-time changes in biofilm formation to be monitored and provides a powerful tool for understanding the interactions within adherent microbial consortia.
Rapid identification of Chinese Sauce liquor from different fermentation positions with FT-IR spectroscopy

NASA Astrophysics Data System (ADS)

Li, Changwen; Wei, Jiping; Zhou, Qun; Sun, Suqin

2008-07-01

FT-IR and two-dimensional correlation spectroscopy (2D-IR) technology were applied to discriminate Chinese Sauce liquor from different fermentation positions (top, middle and bottom of fermentation cellar) for the first time. The liquors at top, middle and bottom of fermentation cellar, possessed the characteristic peaks at 1731 cm -1, 1733 cm -1 and 1602 cm -1, respectively. In the 2D correlation infrared spectra, the differences were amplified. A strong auto-peak at 1725 cm -1 showed in the 2D spectra of the Top Liquor, which indicated that the liquor might contain some ester compounds. Different from Top Liquor, three auto-peaks at 1695, 1590 and 1480 cm -1 were identified in 2D spectra of Middle Liquor, which were the characteristic absorption of acid, lactate. In 2D spectra of Bottom Liquor, two auto-peaks at 1570 and 1485 cm -1 indicated that lactate was the major component. As a result, FT-IR and 2D-IR correlation spectra technology provided a rapid and effective method for the quality analysis of the Sauce liquor.
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.
Tetrapeptide-coumarin conjugate 3D networks based on hydrogen-bonded charge transfer complexes: gel formation and dye release.

PubMed

Guo, Zongxia; Gong, Ruiying; Jiang, Yi; Wan, Xiaobo

2015-08-14

Oligopeptide-based derivatives are important synthons for bio-based functional materials. In this article, a Gly-(L-Val)-Gly-(L-Val)-coumarin (GVGV-Cou) conjugate was synthesized, which forms 3D networks in ethanol. The gel nanostructures were characterized by UV-vis spectroscopy, FT-IR spectroscopy, X-ray diffraction (XRD), SEM and TEM. It is suggested that the formation of charge transfer (CT) complexes between the coumarin moieties is the main driving force for the gel formation. The capability of the gel to encapsulate and release dyes was explored. Both Congo Red (CR) and Methylene Blue (MB) can be trapped in the CT gel matrix and released over time. The present gel might be used as a functional soft material for guest encapsulation and release.
Ag-doped CdO nanocatalysts: Preparation, characterization and catechol oxidase activity

NASA Astrophysics Data System (ADS)

El-Kemary, Maged; El-Mehasseb, Ibrahim; El-Shamy, Hany

2018-06-01

Silver doped cadmium oxide (Ag/CdO) nanoparticles with an average size of 41 nm have been successfully synthesized via thermal decomposition and liquid impregnation technique. The structural characterization has been performed by using several spectroscopic techniques, e.g., X-ray diffraction (XRD), scanning electron microscopy (SEM) and fourier-transform infrared (FT-IR). The catechol oxidase has been studied by UV-visible absorption spectroscopy and fourier-transform infrared as well as the mechanism has been assured by cyclic voltammetry and fluorescence spectroscopy. The results indicate that the oxidation does not occur in the presence of unsupported cadmium oxide particles by silver and in the same time, the catechol oxidase activity of silver doped CdO nanoparticles were improved by about three orders of magnitude than silver ions.
New asymmetric and symmetric 2-((pyridin-4-yl)methylenamino)-3 aminomaleo nitrile and 2,3-bis((pyridin-4-yl)methylenamino)maleonitrile Schiff bases: Synthesis, experimental characterization along with theoretical studies

NASA Astrophysics Data System (ADS)

Zare, Nahid; Zabardasti, Abedien; Dusek, Michal; Eigner, Vaclav

2018-07-01

Two novel Schiff bases 2-((pyridin-4-yl)methelenamino)-3-aminomaleonitrile (L1) and 2,3-bis((pyridin-yl)methylenamino)maleonitrile (L2) were synthesized by the condensation of 2,3-diaminomaleonitrile and 4-pyridine carboxaldehyde using the reflux in absolute methanol. The light yellow crystalline precipitates of L1 were used for single-crystal X-ray crystallography. Two ligans L1 and L2 were characterized by UV-Vis, FT-IR and 1H/13C NMR spectroscopy. Also the FT-IR, 1H NMR and 13C NMR spectra of the compounds were calculated at the B3LYP/6-31 + G(d) level of theory. The Schiff base L1 with unit cell parameters: a = 19.8380(9), b = 4.7221(2), c = 12.9703(6) Å, V = 1215.02(9) Å3, Z = 4 crystallizes in the orthorhombic crystal system with space group Pna21. The crystal structure was solved by charge flipping using single crystal X-ray diffraction data collected at 120 K. For both ligands, the experimentally obtained NMR and IR spectra were a good agreement with their calculated counterparts.
Application of MCR-ALS to reveal intermediate conformations in the thermally induced α-β transition of poly-L-lysine monitored by FT-IR spectroscopy

NASA Astrophysics Data System (ADS)

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

2017-10-01

Temperature-induced conformational transitions of poly-L-lysine were monitored with Fourier-transform infrared (FT-IR) spectroscopy between 10 °C and 70 °C. Chemometric analysis of dynamic IR spectra was performed by multivariate curve analysis-alternating least squares (MCR-ALS) of the amide I‧ and amide II‧ spectral region. With this approach, the pure spectral and concentration profiles of the conformational transition were obtained. Beside the initial α-helical, the intermediate random coil/extended helices and the final β-sheet structure, an additional intermediate PLL conformation was identified and attributed to a transient β-sheet structure.
Sulfonated reduced graphene oxide as a highly efficient catalyst for direct amidation of carboxylic acids with amines using ultrasonic irradiation.

PubMed

Mirza-Aghayan, Maryam; Tavana, Mahdieh Molaee; Boukherroub, Rabah

2016-03-01

Sulfonated reduced graphene oxide nanosheets (rGO-SO3H) were prepared by grafting sulfonic acid-containing aryl radicals onto chemically reduced graphene oxide (rGO) under sonochemical conditions. rGO-SO3H catalyst was characterized by Fourier-transform infrared (FT-IR) spectroscopy, Raman spectroscopy, scanning electron microscopy (SEM), X-ray diffraction (XRD), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC) and X-ray photoelectron spectroscopy (XPS). rGO-SO3H catalyst was successfully applied as a reusable solid acid catalyst for the direct amidation of carboxylic acids with amines into the corresponding amides under ultrasonic irradiation. The direct sonochemical amidation of carboxylic acid takes place under mild conditions affording in good to high yields (56-95%) the corresponding amides in short reaction times. Copyright © 2015 Elsevier B.V. All rights reserved.
Attenuated Total Reflection Fourier Transform Infrared Spectroscopy (ATR FT-IR) Mapping Coupled with Multivariate Curve Resolution (MCR) for Studying the Miscibility of Chlorobutyl Rubber/Polyamide-12 Blends.

PubMed

Tang, Yongjiao; Jing, Nan; Zhang, Pudun

2015-11-01

A series of chlorobutyl rubber/polyamide-12 (CIIR/PA-12) blends compatibilized by different amounts of maleic anhydride (MAH) grafted polypropylene (PP-g-MAH) were investigated by attenuated total reflection Fourier transform infrared spectroscopy (ATR FT-IR) mapping. Multivariate curve resolution (MCR) was used to process the FT-IR images. Both the spectra of pure components in the blends and their concentration distributions in a micro-region were acquired. Our results demonstrated that the blend with 15 parts per hundred rubber PP-g-MAH showed the best miscibility. An amide interphase and an imide interphase were inferred by analyzing the spectra of MCR component 3 of the blends with and without PP-g-MAH, respectively. Correspondingly, two different compatibilizing mechanisms were proposed for these blends.
Thermal properties of tannin extracted from Anacardium occidentale L. using TGA and FT-IR spectroscopy.

PubMed

Viswanath, Vinod; Leo, Vincent Vineeth; Prabha, S Sabna; Prabhakumari, C; Potty, V P; Jisha, M S

2016-01-01

The chemical nature of the polyphenols of cashew kernel testa has been determined. Testa contains tannins, which present large molecular complexity and has an ancient use as tanning agents. The use of tannins extracted from cashew testa, considered in many places as a waste, grants an extra value to the cashew. In this work we have analysed through high performance liquid chromatography, infrared spectroscopy (FT-IR) and thermo gravimetric analysis the average molecular weight, main functional groups and thermal properties of tannins extracted from Anacardium occidentale L. The results of these analyses are compared with the commercial grade tannic acid. The FT-IR spectra showed bands characteristic of C = C, C-C and OH bonds. This important bioactive compound present in the cashew nut kernel testa was suggested as an interesting economical source of antioxidants for use in the food and nutraceutical industry.
Application of attenuated total reflectance Fourier transform infrared spectroscopy for determination of cefixime in oral pharmaceutical formulations.

PubMed

Kandhro, Aftab A; Laghari, Abdul Hafeez; Mahesar, Sarfaraz A; Saleem, Rubina; Nelofar, Aisha; Khan, Salman Tariq; Sherazi, S T H

2013-11-01

A quick and reliable analytical method for the quantitative assessment of cefixime in orally administered pharmaceutical formulations is developed by using diamond cell attenuated total reflectance (ATR) Fourier transform infrared (FT-IR) spectroscopy as an easy procedure for quality control laboratories. The standards for calibration were prepared in aqueous medium ranging from 350 to 6000mg/kg. The calibration model was developed based on partial least square (PLS) using finger print region of FT-IR spectrum in the range from 1485 to 887cm(-1). Excellent coefficient of determination (R(2)) was achieved as high as 0.99976 with root mean square error of 44.8 for calibration. The application of diamond cell (smart accessory) ATR FT-IR proves a reliable determination of cefixime in pharmaceutical formulations to assess the quality of the final product. Copyright © 2013 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.
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.

Structural, optical and morphological characterization of Cu-doped α-Fe2O3 nanoparticles synthesized through co-precipitation technique

NASA Astrophysics Data System (ADS)

Lassoued, Abdelmajid; Lassoued, Mohamed Saber; Dkhil, Brahim; Gadri, Abdellatif; Ammar, Salah

2017-11-01

Pure and copper (Cu concentration varying from 2 to 8%) doped hematite (α-Fe2O3) nanocrystals were synthesized through co-precipitation method using simple equipment. X-ray Diffraction (XRD), Transmission Electron Microscopy (TEM), Scanning Electron Microscopy (SEM), Fourier Transform Infra-Red (FT-IR), Raman spectroscopy, Differential Thermal Analysis (DTA), Thermo Gravimetric Analysis (TGA) and Ultraviolet-Visible (UV-Vis) techniques were used to characterize the synthesized samples. XRD measurements confirm that all the prepared nanocrystals consist only in nanocrystalline hematite phase. These results along with TEM and SEM show that the size of the nanoparticles decreases with Cu-doping down to 21 nm. FT-IR confirm the phase purity of the nanoparticles synthesized. The Raman spectroscopy was used not only to prove that we synthesized pure and Cu-doped hematite but also to identify their phonon modes. The TGA showed three mass losses, whereas DTA resulted in three endothermic peaks. The UV-Vis absorption measurements confirm that the decrease of particle size is accompanied by a decrease in the band gap value from 2.12 eV for pure α-Fe2O3 down to 1.91 eV for 8% Cu-doped α-Fe2O3. 8% Cu-doped hematite had the smallest size, the best crystallinity and the lowest band gap.
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.
Integrated gas analyzer for complete monitoring of turbine engine test cells.

PubMed

Markham, James R; Bush, Patrick M; Bonzani, Peter J; Scire, James J; Zaccardi, Vincent A; Jalbert, Paul A; Bryant, M Denise; Gardner, Donald G

2004-01-01

Fourier transform infrared (FT-IR) spectroscopy is proving to be reliable and economical for the quantification of many gas-phase species during testing and development of gas turbine engines in ground-based facilities such as sea-level test cells and altitude test cells. FT-IR measurement applications include engine-generated exhaust gases, facility air provided as input to engines, and ambient air in and around test cells. Potentially, the traditionally used assembly of many gas-specific single gas analyzers will be eliminated. However, the quest for a single instrument capable of complete gas-phase monitoring at turbine engine test cells has previously suffered since the FT-IR method cannot measure infrared-inactive oxygen molecules, a key operational gas to both air-breathing propulsion systems and test cell personnel. To further the quest, the FT-IR sensor used for the measurements presented in this article was modified by integration of a miniature, solid-state electrochemical oxygen sensor. Embedded in the FT-IR unit at a location near the long-effective-optical-path-length gas sampling cell, the amperometric oxygen sensor provides simultaneous, complementary information to the wealth of spectroscopic data provided by the FT-IR method.
Estimation of Cellulose Crystallinity of Lignocelluloses Using Near-IR FT-Raman Spectroscopy and Comparison of the Raman and Segal-WAXS Methods

Treesearch

Umesh P. Agarwal; Richard R. Reiner; Sally A. Ralph

2013-01-01

Of the recently developed univariate and multivariate near-IR FT-Raman methods for estimating cellulose crystallinity, the former method was applied to a variety of lignocelluloses: softwoods, hardwoods, wood pulps, and agricultural residues/fibers. The effect of autofluorescence on the crystallinity estimation was minimized by solvent extraction or chemical treatment...
Synthesis, characterization, nano-sized binuclear nickel complexes, DFT calculations and antibacterial evaluation of new macrocyclic Schiff base compounds

NASA Astrophysics Data System (ADS)

Parsaee, Zohreh; Mohammadi, Khosro

2017-06-01

Some new macrocyclic bridged dianilines tetradentate with N4coordination sphere Schiff base ligands and their nickel(II)complexes with general formula [{Ni2LCl4} where L = (C20H14N2X)2, X = SO2, O, CH2] have been synthesized. The compounds have been characterized by FT-IR, 1H and 13C NMR, mass spectroscopy, TGA, elemental analysis, molar conductivity and magnetic moment techniques. Scanning electron microscopy (SEM) shows nano-sized structures under 100 nm for nickel (II) complexes. NiO nanoparticle was achieved via the thermal decomposition method and analyzed by FT-IR, SEM and X-ray powder diffraction which indicates closeaccordance to standard pattern of NiO nanoparticle. All the Schiff bases and their complexes have been detected in vitro both for antibacterial activity against two gram-negative and two gram-positive bacteria. The nickel(II) complexes were found to be more active than the free macrocycle Schiff bases. In addition, computational studies of three ligands have been carried out at the DFT-B3LYP/6-31G+(d,p) level of theory on the spectroscopic properties, including IR, 1HNMR and 13CNMR spectroscopy. The correlation between the theoretical and the experimental vibrational frequencies, 1H NMR and 13C NMR of the ligands were 0.999, 0.930-0.973 and 0.917-0.995, respectively. Also, the energy gap was determined and by using HOMO and LUMO energy values, chemical hardness-softness, electronegativity and electrophilic index were calculated.
Monitoring wheat mitochondrial compositional and respiratory changes using Fourier transform mid-infrared spectroscopy in response to agrochemical treatments

NASA Astrophysics Data System (ADS)

Pedersen, Matthew; Wegner, Casey; Phansak, Piyaporn; Sarath, Gautam; Gaussoin, Roch; Schlegel, Vicki

2017-02-01

Fungicides and plant growth regulators can impact plant growth outside of their effects on fungal pathogens. Although many of these chemicals are inhibitors of mitochondrial oxygen uptake, information remains limited as to whether they are able to modify other mitochondrial constituents. Fourier transform mid-infrared spectroscopy (FT-mIR) offers a high sample throughput method to comparatively and qualitatively evaluate the effects of exogenously added compounds on mitochondrial components. Therefore the objective of this study was to determine the ability of FT-mIR to detect effects mitochondrial fractions isolated from wheat (Triticum aestivum L.) seedlings in response to several agrochemical treatments, with an emphasis on fungicides. The accessed need was to develop FT-mIR analytical and statistical routines as an effective approach to differentiate spectra obtained from chemically-treated or untreated mitochondria. An NADH-dependent oxygen uptake approach was initially used as a comparative method to determine whether the fungicides (azoxystrobin, boscalid, cyazofamid, fluazinam, isopyrazam, and pyraclostrobin) and the plant growth regulator, (trinexapac-ethyl) reduced respiration inhibition on isolated mitochondria. Pyraclostrobin was the most effective inhibitor, whereas amisulbrom did not impact oxygen uptake. However, hierarchical clustering of FT-mIR spectra of isolated mitochondria treated with these different compounds separated into clades consistent with each of their expected mode of action. Analysis of the FT-mIR amide protein region indicated that amisulbrom and pyraclostrobin interacted with the isolated wheat mitochondria. Both chemicals were statistically different from the control signifying that respiration was indeed influenced by these treatments. Moreover, the entire FT-mIR region showed differences in various biological bands thereby providing additional information on mitochondria responses to agrochemicals, if so warranted.
Green synthesis of silver nanoparticles using tannins

NASA Astrophysics Data System (ADS)

Raja, Pandian Bothi; Rahim, Afidah Abdul; Qureshi, Ahmad Kaleem; Awang, Khalijah

2014-09-01

Colloidal silver nanoparticles were prepared by rapid green synthesis using different tannin sources as reducing agent viz. chestnut (CN), mangrove (MG) and quebracho (QB). The aqueous silver ions when exposed to CN, MG and QB tannins were reduced which resulted in formation of silver nanoparticles. The resultant silver nanoparticles were characterized using UV-Visible, X-ray diffraction (XRD), scanning electron microscopy (SEM/EDX), and transmission electron microscopy (TEM) techniques. Furthermore, the possible mechanism of nanoparticles synthesis was also derived using FT-IR analysis. Spectroscopy analysis revealed that the synthesized nanoparticles were within 30 to 75 nm in size, while XRD results showed that nanoparticles formed were crystalline with face centered cubic geometry.
Copolymers of polyaniline and poly-o-toluidine: Electrochemical synthesis and characterization

NASA Astrophysics Data System (ADS)

Yadav, Pooja C.; Deshmukh, Megha A.; Patil, Harshada K.; Bodkhe, Gajanan A.; Sayyad, Pasha W.; Ingle, Nikesh N.; Shirsat, Mahendra D.

2018-05-01

In the present study we have reported Electrochemical polymerization of poly(Aniline) (PANI), Poly(O-Toluidine) (POT) and poly(Aniline-co-O-Toluidine) (PAOT) copolymers. Electrochemical Synthesis of PANI, POT and Poly(Aniline-co-O-Toluidine) was done by using Cyclic Voltammetry technique. The morphological study done by Atomic Force Microscopy (AFM) which shows that formation of uniform granular structure and topographic changes in each respective thin film. Spectroscopic characterization was done by FTIR spectroscopy. The FT-IR study revealed the formation of PANI/POT/Poly(Aniline co O-Toluidine) with a absorption band are reported. For structural information done by X-ray diffraction(XRD) Characterization.
DOE Office of Scientific and Technical Information (OSTI.GOV)

Mascarenhas, N. P., E-mail: naveenmascarenhas@gmail.com; Crasta, V.; Gonsalves, R. A.

To enhance the physical and mechanical properties of Chitosan (CS) and to improve the functionality of CS towards some specific applications, we have blended CS with polystyrene (PS) to form blended films. The Fourier Transform Infrared Spectroscopy (FT-IR) has been performed on the prepared films to confirm functional groups and formation of the blends. Thermal analysis (TGA and DSC) is carried out to study thermal stability of the blended films. From X-ray diffraction (XRD) studies, the material reveals amorphous nature and hence it may be used for adsorption process. The versatility of the blends, such as film-forming ability, hydrophilicity, biodegradabilitymore » and biocompatibility are comparable with the existing blends.« less
Infrared and Raman spectroscopic methods for characterization of Taxus baccata L.--Improved taxane isolation by accelerated quality control and process surveillance.

PubMed

Gudi, Gennadi; Krähmer, Andrea; Koudous, Iraj; Strube, Jochen; Schulz, Hartwig

2015-10-01

Different yew species contain poisonous taxane alkaloids which serve as resources for semi-synthesis of anticancer drugs. The highly variable amounts of taxanes demand new methods for fast characterization of the raw plant material and the isolation of the target structures during phyto extraction. For that purpose, applicability of different vibrational spectroscopy methods in goods receipt of raw plant material and in process control was investigated and demonstrated in online tracking isolation and purification of the target taxane 10-deacetylbaccatin III (10-DAB) during solvent extraction. Applying near (NIRS) and mid infrared spectroscopy (IRS) the amount of botanical impurities in mixed samples of two different yew species (R(2)=0.993), the leave-to-wood ratio for Taxus baccata material (R(2)=0.94) and moisture in dried yew needles (R(2)=0.997) can be quantified. By partial least square analysis (PCA) needles of different Coniferales species were successfully discriminated by Attenuated Total Reflectance-Fourier-Transform Infrared Spectroscopy (ATR-FT-IR). The analytical potential of ATR-FT-IR and Fourier Transform-Raman Spectroscopy (FT-RS) in process control of extraction and purification of taxanes is demonstrated for determination of the water content in methanolic yew extracts (R(2)=0.999) and for quantification of 10-DAB (R(2)=0.98) on a highly sophisticated level. The decrease of 10-DAB in the plant tissue during extraction was successfully visualized by FT-IR imaging of thin cross sections providing new perspectives for process control and design. Copyright © 2015 Elsevier B.V. All rights reserved.
Combining Raman and FT-IR spectroscopy with quantitative isotopic labeling for differentiation of E. coli cells at community and single cell levels.

PubMed

Muhamadali, Howbeer; Chisanga, Malama; Subaihi, Abdu; Goodacre, Royston

2015-04-21

There is no doubt that the contribution of microbially mediated bioprocesses toward maintenance of life on earth is vital. However, understanding these microbes in situ is currently a bottleneck, as most methods require culturing these microorganisms to suitable biomass levels so that their phenotype can be measured. The development of new culture-independent strategies such as stable isotope probing (SIP) coupled with molecular biology has been a breakthrough toward linking gene to function, while circumventing in vitro culturing. In this study, for the first time we have combined Raman spectroscopy and Fourier transform infrared (FT-IR) spectroscopy, as metabolic fingerprinting approaches, with SIP to demonstrate the quantitative labeling and differentiation of Escherichia coli cells. E. coli cells were grown in minimal medium with fixed final concentrations of carbon and nitrogen supply, but with different ratios and combinations of (13)C/(12)C glucose and (15)N/(14)N ammonium chloride, as the sole carbon and nitrogen sources, respectively. The cells were collected at stationary phase and examined by Raman and FT-IR spectroscopies. The multivariate analysis investigation of FT-IR and Raman data illustrated unique clustering patterns resulting from specific spectral shifts upon the incorporation of different isotopes, which were directly correlated with the ratio of the isotopically labeled content of the medium. Multivariate analysis results of single-cell Raman spectra followed the same trend, exhibiting a separation between E. coli cells labeled with different isotopes and multiple isotope levels of C and N.
Activation and thermodynamic parameter study of the heteronuclear C=O···H-N hydrogen bonding of diphenylurethane isomeric structures by FT-IR spectroscopy using the regularized inversion of an eigenvalue problem.

PubMed

Spegazzini, Nicolas; Siesler, Heinz W; Ozaki, Yukihiro

2012-08-02

The doublet of the ν(C=O) carbonyl band in isomeric urethane systems has been extensively discussed in qualitative terms on the basis of FT-IR spectroscopy of the macromolecular structures. Recently, a reaction extent model was proposed as an inverse kinetic problem for the synthesis of diphenylurethane for which hydrogen-bonded and non-hydrogen-bonded C=O functionalities were identified. In this article, the heteronuclear C=O···H-N hydrogen bonding in the isomeric structure of diphenylurethane synthesized from phenylisocyanate and phenol was investigated via FT-IR spectroscopy, using a methodology of regularization for the inverse reaction extent model through an eigenvalue problem. The kinetic and thermodynamic parameters of this system were derived directly from the spectroscopic data. The activation and thermodynamic parameters of the isomeric structures of diphenylurethane linked through a hydrogen bonding equilibrium were studied. The study determined the enthalpy (ΔH = 15.25 kJ/mol), entropy (TΔS = 14.61 kJ/mol), and free energy (ΔG = 0.6 kJ/mol) of heteronuclear C=O···H-N hydrogen bonding by FT-IR spectroscopy through direct calculation from the differences in the kinetic parameters (δΔ(‡)H, -TδΔ(‡)S, and δΔ(‡)G) at equilibrium in the chemical reaction system. The parameters obtained in this study may contribute toward a better understanding of the properties of, and interactions in, supramolecular systems, such as the switching behavior of hydrogen bonding.
Analysis and identification of two reconstituted tobacco sheets by three-level infrared spectroscopy

NASA Astrophysics Data System (ADS)

Wu, Xian-xue; Xu, Chang-hua; Li, Ming; Sun, Su-qin; Li, Jin-ming; Dong, Wei

2014-07-01

Two kinds of reconstituted tobacco (RT) from France (RTF) and China (RTC) were analyzed and identified by a three-level infrared spectroscopy method (Fourier-transform infrared spectroscopy (FT-IR) coupled with second derivative infrared spectroscopy (SD-IR) and two-dimensional infrared correlation spectroscopy (2D-IR)). The conventional IR spectra of RTF parallel samples were more consistent than those of RTC according to their overlapped parallel spectra and IR spectra correlation coefficients. FT-IR spectra of both two RTs were similar in holistic spectral profile except for small differences around 1430 cm-1, indicating that they have similar chemical constituents. By analysis of SD-IR spectra of RTFs and RTCs, more distinct fingerprint features, especially peaks at 1106 (1110), 1054 (1059) and 877 (874) cm-1, were disclosed. Even better reproducibility of five SD-IR spectra of RTF in 1750-1400 cm-1 could be seen intuitively from their stacked spectra and could be confirmed by further similarity evaluation of SD-IR spectra. Existence of calcium carbonate and calcium oxalate could be easily observed in two RTs by comparing their spectra with references. Furthermore, the 2D-IR spectra provided obvious, vivid and intuitive differences of RTF and RTC. Both two RTs had a pair of strong positive auto-peaks in 1600-1400 cm-1. Specifically, the autopeak at 1586 cm-1 in RTF was stronger than the one around 1421 cm-1, whereas the one at 1587 cm-1 in RTC was weaker than that at 1458 cm-1. Consequently, the RTs of two different brands were analyzed and identified thoroughly and RTF had better homogeneity than RTC. As a result, three-level infrared spectroscopy method has proved to be a simple, convenient and efficient method for rapid discrimination and homogeneousness estimation of RT.
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.
Fourier transform ion cyclotron resonance mass spectrometry

NASA Astrophysics Data System (ADS)

Marshall, Alan G.

1998-06-01

As for Fourier transform infrared (FT-IR) interferometry and nuclear magnetic resonance (NMR) spectroscopy, the introduction of pulsed Fourier transform techniques revolutionized ion cyclotron resonance mass spectrometry: increased speed (factor of 10,000), increased sensitivity (factor of 100), increased mass resolution (factor of 10,000-an improvement not shared by the introduction of FT techniques to IR or NMR spectroscopy), increased mass range (factor of 500), and automated operation. FT-ICR mass spectrometry is the most versatile technique for unscrambling and quantifying ion-molecule reaction kinetics and equilibria in the absence of solvent (i.e., the gas phase). In addition, FT-ICR MS has the following analytically important features: speed (~1 second per spectrum); ultrahigh mass resolution and ultrahigh mass accuracy for analysis of mixtures and polymers; attomole sensitivity; MSn with one spectrometer, including two-dimensional FT/FT-ICR/MS; positive and/or negative ions; multiple ion sources (especially MALDI and electrospray); biomolecular molecular weight and sequencing; LC/MS; and single-molecule detection up to 108 Dalton. Here, some basic features and recent developments of FT-ICR mass spectrometry are reviewed, with applications ranging from crude oil to molecular biology.
Analysis of hard-to-cook red and black common beans using Fourier transform infrared spectroscopy.

PubMed

Maurer, Giselle A; Ozen, Banu F; Mauer, Lisa J; Nielsen, S Suzanne

2004-03-24

Extracted fractions from black and red common beans (Phaseolus vulgaris) were studied using Fourier transform infrared spectroscopy (FT-IR). Beans were stored under three conditions: control at 4 degrees C; hard-to-cook (HTC) at 29 degrees C, 65% RH for 3.5 months; and refrigerated at 2 degrees C, 79% RH for 3.5 months after a HTC period (called HTC-refrigerated). Two fractions isolated from the beans, the soluble pectin fraction (SPF) and the water insoluble residue of the cell wall (WIRCW), were analyzed using diffuse reflectance (DRIFTS) FT-IR. The soaking water and cooking water from the beans were also studied using attenuated total reflectance (ATR) FT-IR. The DRIFTS FT-IR results from the SPF and WIRCW fractions were consistent with previously published data for Carioca beans showing that in general, more phenolic compounds were associated with the SPF of HTC beans than in the control beans. Results also showed that HTC-refrigerated beans had higher concentrations of phenolic compounds than control beans in the SPF. The ATR FT-IR results for soaking and cooking waters from the HTC-refrigerated and HTC beans had higher concentrations of absorbing compounds than the control beans, indicating that they lost more constituents to the water. Additionally, results indicate that the mechanism(s) for reversibility of the HTC defect could be different than the one(s) involved in the development of the defect.
The Scope Of Fourier Transform Infrared (FTIR)

NASA Astrophysics Data System (ADS)

Hirschfeld, T.

1981-10-01

Three auarters of a century after its inception, a generation after its advantages were recognized, and a decade after its first commercialization, FT-IR dominates the growth of the IR market, and reigns alone over its high performance end. What lies ahead for FT-IR now? On one hand, the boundary between it and the classical scanning spectrometers is becoming fuzzy, as gratings attempt to use as much of FT-IR's computer technology as they can handle, and smaller FT systems invade the medium cost instrument range. On the other hand, technology advances in IR detectors, non-Fourier interference devices, and the often announced tunable laser are at long last getting set to make serious inroads in the field (although not necessarily in the manner most of us expected). However, the dominance of FT-IR as the leading edge of IR spectroscopy seems assured for a good many years. The evolution of FT-IR will be dominated by demands not yet fully satisfied such as rapid sample turnover, better quantitation, automated interpretation, higher GC-IR sensitivity, improved LC-IR, and, above all else, reliability and ease of use. These developments will be based on multiple small advances in hardware, large advances in the way systems are put together, and the traditional yearly revolutionary advances of the computer industry. The big question in the field will, however, still be whether our ambition and our skill can continue to keep up with the advances of our tools. It will be fun.
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%.
Differentiation between probiotic and wild-type Bacillus cereus isolates by antibiotic susceptibility test and Fourier transform infrared spectroscopy (FT-IR).

PubMed

Mietke, Henriette; Beer, W; Schleif, Julia; Schabert, G; Reissbrodt, R

2010-05-30

Animal feed often contains probiotic Bacillus strains used as feed additives. Spores of the non-pathogenic B. cereus var. toyoi (product name Toyocerin) are used. Distinguishing between toxic wild-type Bacillus cereus strains and this probiotic strain is essential for evaluating the quality and risk of feed. Bacillus cereus CIP 5832 (product name Paciflor was used as probiotic strain until 2001. The properties of the two probiotic strains are quite similar. Differentiating between probiotic strains and wild-type B. cereus strains is not easy. ss-lactam antibiotics such as penicillin and cefamandole exhibit an inhibition zone in the agar diffusion test of probiotic B. cereus strains which are not seen for wild-type strains. Therefore, performing the agar diffusion test first may make sense before FT-IR testing. When randomly checking these strains by Fourier transform infrared spectroscopy (FT-IR), the probiotic B. cereus strains were separated from wild-type B. cereus/B. thuringiensis/B. mycoides/B. weihenstephanensis strains by means of hierarchical cluster analysis. The discriminatory information was contained in the spectral windows 3000-2800 cm(-1) ("fatty acid region"), 1200-900 cm(-1) ("carbohydrate region") and 900-700 cm(-1) ("fingerprint region"). It is concluded that FT-IR spectroscopy can be used for the rapid quality control and risk analysis of animal feed containing probiotic B. cereus strains. (c) 2010 Elsevier B.V. All rights reserved.
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.

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.
Application of mid-infrared spectroscopy in analyzing different segmented production of Angelica by AB-8 macroporous resin

NASA Astrophysics Data System (ADS)

Guo, Yizhen; Wang, Jingjuan; Lu, Lina; Sun, Suqin; Liu, Yang; Xiao, Yao; Qin, Youwen; Xiao, Lijuan; Wen, Haoran; Qu, Lei

2016-01-01

As complicated mixture systems, chemical components of Angelica are very difficult to identify and discriminate, so as not to control its quality effectively. In recent years, Mid-infrared spectroscopy has been innovatively employed to identify and assess the quality of Traditional Chinese medicine (TCM) products. In this paper, the macroscopic IR fingerprint method including Fourier transform infrared spectroscopy (FT-IR), the second derivative infrared spectroscopy (SD-IR) and two-dimensional correlation infrared spectroscopy (2D-IR), are applied to study and identify Angelica raw material, the decoction and different segmented production of AB-8 macroporous resin. FT-IR spectrum indicates that Angelica raw material is rich in sucrose and the correlation coefficient is 0.8465. The decoction of Angelica contains varieties of polysaccharides components and the content is gradually decreased with increasing concentration of ethanol. In addition, the decoction of Angelica contains a certain amount of protein components and 50% ethanol eluate has more protein than other eluates. Their second derivative spectra amplify the differences and reveal the potentially characteristic IR absorption bands, then we conclude that the decoction of Angelica contains a certain amount of ferulic acid and ligustilide. And 30% ethanol eluate, 50% ethanol eluate and 70% ethanol eluate are similar to ligustilide. Further, 2D-IR spectra enhance the spectral resolution and obtain much new information for discriminating the similar complicated samples. It is demonstrated that the above three-step infrared spectroscopy could be applicable for effective, visual and accurate analysis and identification of very complicated and similar mixture systems of traditional Chinese medicines.
Chemometric compositional analysis of phenolic compounds in fermenting samples and wines using different infrared spectroscopy techniques.

PubMed

Aleixandre-Tudo, Jose Luis; Nieuwoudt, Helene; Aleixandre, Jose Luis; du Toit, Wessel

2018-01-01

The wine industry requires reliable methods for the quantification of phenolic compounds during the winemaking process. Infrared spectroscopy appears as a suitable technique for process control and monitoring. The ability of Fourier transform near infrared (FT-NIR), attenuated total reflectance mid infrared (ATR-MIR) and Fourier transform infrared (FT-IR) spectroscopies to predict compositional phenolic levels during red wine fermentation and aging was investigated. Prediction models containing a large number of samples collected over two vintages from several industrial fermenting tanks as well as wine samples covering a varying number of vintages were validated. FT-NIR appeared as the most accurate technique to predict the phenolic content. Although slightly less accurate models were observed, ATR-MIR and FT-IR can also be used for the prediction of the majority of phenolic measurements. Additionally, the slope and intercept test indicated a systematic error for the three spectroscopies which seems to be slightly more pronounced for HPLC generated phenolics data than for the spectrophotometric parameters. However, the results also showed that the predictions made with the three instruments are statistically comparable. The robustness of the prediction models was also investigated and discussed. Copyright © 2017 Elsevier B.V. All rights reserved.
Deposition of GdVO4:Eu3+ nanoparticles on silica nanospheres by a simple sol gel method

NASA Astrophysics Data System (ADS)

Liu, Guixia; Hong, Guangyan; Wang, Jinxian; Dong, Xiangting

2006-07-01

The deposition and coating of GdVO4:Eu3+ nanoparticles on spherical silica was carried out using a simple sol-gel method at low temperature. The GdVO4:Eu3+-coated silica composites obtained were characterized by differential thermal analysis (DTA), thermogravimetric (TG) analysis, x-ray diffraction (XRD), Fourier-transform IR spectroscopy (FT-IR), transmission electron microscopy (TEM), x-ray photoelectron spectroscopy (XPS), photoluminescence spectra, and kinetic decay. It is found that the ~5 nm GdVO4:Eu3+ nanoparticles coating the silica spheres are crystal in the as-prepared samples and the crystallinity increases with increasing annealing temperature. The composites obtained are spherical in shape with an average size of 100 nm. The GdVO4:Eu3+ nanoparticles are linked with silica cores by a chemical bond. The photoluminescence spectra of the obtained GdVO4:Eu3+-coated silica composites are similar to those of the bulk GdVO4:Eu3+ phosphors. The strongest peak is near 617 nm, which indicates that Eu3+ is located in the low symmetry site with non-inversion centre.
Surface segregation of additives on SnO 2 based powders and their relationship with macroscopic properties

NASA Astrophysics Data System (ADS)

Pereira, Gilberto J.; Castro, Ricardo H. R.; Hidalgo, Pilar; Gouvêa, Douglas

2002-07-01

Surface properties of ceramic powders frequently play an important role in producing high-quality, high-performance, and reliable ceramic products. These properties are related to the surface bond types and interactions with the surroundings. Oxide surfaces generally contain adsorbed hydroxyl groups and modifications in the chemical composition of the surface may be studied by infrared spectroscopy. In this work, we prepared SnO 2 containing Fe or Mg ions by organic chemical route derived from Pechini's method. The prepared powders were characterized by infrared spectroscopy (FT-IR), X-ray diffraction (XRD), dynamic electrophoretic mobility and surface area determination. Results demonstrated that the studied additives segregate onto the oxide surface and modify the hydroxyl IR bands of the adsorbed hydroxyl groups. These surface modifications change some macroscopic properties of the powder such as the isoelectric point (IEP) in aqueous suspensions and the final specific surface area. The increase of the surface area with additive concentration is supposedly due to the reduction of surface energy of the powders when additives segregate on the powder surface.
Chemically functionalized ZnS quantum dots as new optical nanosensor of herbicides

NASA Astrophysics Data System (ADS)

Masteri-Farahani, M.; Mahdavi, S.; Khanmohammadi, H.

2018-03-01

Surface chemical functionalization of ZnS quantum dots (ZnS-QDs) with cysteamine hydrochloride resulted in the preparation of an optical nanosensor for detection of herbicides. Characterization of the functionalized ZnS-QDs was performed with physicochemical methods such as x-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared (FT-IR) spectroscopy, energy dispersive x-ray (EDX) analysis, ultraviolet-visible (UV–vis) and photoluminescence (PL) spectroscopies. The optical band gap of the functionalized ZnS-QDs was determined by using Tauc plot as 4.1 eV. Addition of various herbicides resulted in the linearly fluorescence quenching of the functionalized ZnS-QDs according to the Stern-Volmer equation. The functionalized ZnS-QDs can be used as simple, rapid, and inexpensive nanosensor for practical detection and measurement of various herbicides.
Green synthesis and spectral characterization of silver nanoparticles from Lakshmi tulasi (Ocimum sanctum) leaf extract

NASA Astrophysics Data System (ADS)

Subba Rao, Y.; Kotakadi, Venkata S.; Prasad, T. N. V. K. V.; Reddy, A. V.; Sai Gopal, D. V. R.

2013-02-01

A simple method for the green synthesis of silver nanoparticles (AgNPs) using aqueous extract of Lakshmi tulasi (Ocimum sanctum) leaf as a reducing and stabilizing agent. AgNPs were rapidly synthesized using aqueous extract of tulasi leaf with AgNO3 solution within 15 min. The green synthesized AgNPs were characterized using physic-chemical techniques viz., UV-Vis, X-ray diffraction (XRD), scanning electron microscope (SEM) coupled with X-ray energy dispersive spectroscopy (EDX) and Fourier transform-infrared spectroscopy (FT-IR). Characterization data reveals that the particles were crystalline in nature and triangle shaped with an average size of 42 nm. The zeta potential of AgNPs were found to be -55.0 mV. This large negative zeta potential value indicates repulsion among AgNPs and their dispersion stability.
Green synthesis of silver nanoparticles using Alternanthera dentata leaf extract at room temperature and their antimicrobial activity

NASA Astrophysics Data System (ADS)

Kumar, Deenadayalan Ashok; Palanichamy, V.; Roopan, Selvaraj Mohana

2014-06-01

A green rapid biogenic synthesis of silver nanoparticles AgNPs using Alternanthera dentata (A. dentata) aqueous extract was demonstrated in this present study. The formation of silver nanoparticles was confirmed by Surface Plasmon Resonance (SPR) at 430 nm using UV-visible spectrophotometer. The reduction of silver ions to silver nanoparticles by A. dentata extract was completed within 10 min. Synthesized nanoparticles were characterized using UV-visible spectroscopy; Fourier transformed infrared spectroscopy (FT-IR), X-ray diffraction (XRD), scanning electron microscopy and transmission electron microscopy (TEM). The extracellular silver nanoparticles synthesis by aqueous leaf extract demonstrates rapid, simple and inexpensive method comparable to chemical and microbial methods. The colloidal solution of silver nanoparticles were found to exhibit antibacterial activity against Escherichia coli, Pseudomonas aeruginosa, Klebsiella pneumonia and, Enterococcus faecalis.
A simple and facile synthesis of MPA capped CdSe and CdSe/CdS core/shell nanoparticles

NASA Astrophysics Data System (ADS)

Sukanya, D.; Sagayaraj, P.

2015-06-01

II-VI semiconductor nanostructures, in particular, CdSe quantum dots have drawn a lot of attention because of their promising potential applications in biological tagging, photovoltaic, display devices etc. due to their excellent optical properties, high emission quantum yield, size dependent emission wavelength and high photostability. In this paper, we describe the synthesis and properties of mercaptopropionic acid capped CdSe and CdSe/CdS nanoparticles through a simple and efficient co-precipitation method followed by hydrothermal treatment. The growth process, characterization and the optical absorption as a function of wavelength for the synthesized MPA capped CdSe and CdSe/CdS nanoparticles have been determined using X-ray diffraction study (XRD), Ultraviolet-Visible spectroscopy (UV-Vis), Fourier transform infrared spectroscopy (FT-IR) and High Resolution Transmission Electron Microscopy (HRTEM).
Preparation of hollow magnetite microspheres and their applications as drugs carriers

PubMed Central

2012-01-01

Hollow magnetite microspheres have been synthesized by a simple process through a template-free hydrothermal approach. Hollow microspheres were surface modified by coating with a silica nanolayer. Pristine and modified hollow microparticles were characterized by field-emission electron microscopy, transmission electron microscopy, X-ray diffraction, X-ray photoelectron spectroscopy, FT-IR and Raman spectroscopy, and VSM magnetometry. The potential application of the modified hollow magnetite microspheres as a drug carrier was evaluated by using Rhodamine B and methotrexate as model drugs. The loading and release kinetics of both molecules showed a clear pH and temperature dependent profile. Graphical abstract Hollow magnetite microspheres have been synthesized. Load-release experiments with Rhodamine-B as a model drug and with Methotrexate (chemotherapy drug used in treating certain types of cancer) demonstrated the potential applications of these nanostructures in biomedical applications. PMID:22490731
Defect-Induced Luminescence of a Self-Activated Borophosphate Phosphor

NASA Astrophysics Data System (ADS)

Han, Bing; Liu, Beibei; Dai, Yazhou; Zhang, Jie

2018-05-01

A self-activated borophosphate phosphor Ba3BPO7 was prepared via typical solid-state reaction in thermal-carbon reduction atmosphere. The structural and luminescence properties were investigated using x-ray powder diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, and photoluminescence spectroscopy. Upon excitation with ultraviolet (UV) light, the as-prepared phosphor shows bright greenish-yellow emission with a microsecond-level fluorescence lifetime, which could result from the oxygen vacancies produced in the process of solid-state synthesis. The possible luminescence mechanism is proposed. Through the introduction of defects in the host, this work realizes visible luminescence in a pure borophosphate compound that does not contain any rare earth or transition metal activators, so it is helpful to develop defect-related luminescent materials in view of energy conservation and environmental protection for sustainable development.
Adsorption of dodecylamine hydrochloride on graphene oxide in water

NASA Astrophysics Data System (ADS)

Chen, Peng; Li, Hongqiang; Song, Shaoxian; Weng, Xiaoqing; He, Dongsheng; Zhao, Yunliang

Cationic surfactants in water are difficult to be degraded, leading to serious water pollution. In this work, graphene oxide (GO) was used as an adsorbent for removing Dodecylamine Hydrochloride (DACl), a representative cationic surfactant. X-ray diffraction (XRD), FT-IR spectroscopy and atomic force microscope (AFM) were used to characterize the prepared GO. The adsorption of DACl on GO have been investigated through measurements of adsorption capacity, zeta potential, FTIR, and X-ray photoelectron spectroscopy (XPS). The experimental results have shown that the adsorption kinetics could be described as a rate-limiting pseudo second-order process, and the adsorption isotherm agreed well with the Freundlich model. GO was a good adsorbent for DACl removal, compared with coal fly ash and powdered activated carbon. The adsorption process was endothermic, and could be attributed to electrostatic interaction and hydrogen bonding between DACl and GO.
Synthesis of porous nanocrystalline NiO with hexagonal sheet-like morphology by homogeneous precipitation method

NASA Astrophysics Data System (ADS)

Sharma, Ravi Kant; Ghose, Ranjana

2015-04-01

Porous nanocrystalline NiO has been synthesized by a simple homogeneous precipitation method in short time at low calcination temperature without using any surfactant, chelating or gelating agents. The porous nanocrystalline NiO with a hexagonal sheet-like morphology were obtained by calcination of Ni(OH)2 nanoflakes at 500 °C. The calcination temperature strongly influences the morphology, crystallite size, specific surface area, pore volume and optical band gap of the samples. The samples were characterized using powder X-ray diffraction, thermal gravimetric analysis, FT-IR spectroscopy, UV-Visible diffuse reflectance spectroscopy, surface area measurements, field emission scanning electron microscopy coupled with energy dispersive X-ray analysis and transmission electron microscopy. The chemical activity of the samples was tested by catalytic reduction of 4-nitrophenol with NaBH4.
Visible light driven photocatalytic degradation of methylene blue using novel camphor sulfonic acid doped polycarbazole/g-C3N4 nanocomposite

NASA Astrophysics Data System (ADS)

Praveena, P.; Dhanavel, S.; Sangamithirai, D.; Narayanan, V.; Stephen, A.

2018-04-01

A novel polycabazole(PCz)/graphitic carbon nitride(g-C3N4) nanocomposite was synthesized via chemical oxidative polymerization method. In the present work, camphor sulfonic acid (CSA) was used as a dopantand ammonium peroxydisulphate (APS) was used as an oxidizing agent. The PCz/g-C3N4 nanocompositewas characterizedusing X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR) and UV-Visible spectroscopy (UV-Vis). The obtained results confirm the successful formation of PCz/g-C3N4 nanocomposite. Visible light induced photocatalytic activity of the novel catalyst was demonstrated using methylene blue as a target pollutant. The results suggestthat PCz/g-C3N4 nanocomposite can be used as an effective catalyst for the degradation of organic pollutants from waste water.
Thermal and Optical Properties of New Poly(amide-imide)/Nanocomposite Reinforced by Layer Silicate Containing Diphenyl Ether Moieties

NASA Astrophysics Data System (ADS)

Faghihi, Khalil; Faramarzi, Ellahe; Shabanian, Meisam

2011-04-01

New poly(amide-imide)-montmorillonite reinforced nanocomposites containing Bis(4-N-trimellitylimido) diphenyl ether moiety in the main chain were synthesized by a convenient solution intercalation technique. Poly(amide-imide) (PAI) 4 was synthesized by the direct polycondensation reaction of Bis(4-N-trimellitylimido) diphenyl ether 3 with 4,4'-diamino diphenyl ether 2 in the presence of triphenyl phosphite (TPP), CaCl2, pyridine and N-methyl-2-pyrrolidone (NMP). Morphology and structure of the resulting PAI-nanocomposite films 4a and 4b with 10 and 20 mass% silicate particles respectively, were characterized by FT-IR spectroscopy, X-ray diffraction (XRD) and scanning electron microscopy (SEM). The properties of nanocomposites films were investigated by using Uv-vis spectroscopy, thermogravimetric analysis (TGA) and water uptake measurements.
Studies on the chemical synthesis and characterization of lead oxide nanoparticles with different organic capping agents

NASA Astrophysics Data System (ADS)

Arulmozhi, K. T.; Mythili, N.

2013-12-01

Lead oxide (PbO) nanoparticles were chemically synthesized using Lead (II) acetate as precursor. The effects of organic capping agents such as Oleic acid, Ethylene Diamine Tetra Acetic acid (EDTA) and Cetryl Tri Methyl Butoxide (CTAB) on the size and morphology of the nanoparticles were studied. Characterization techniques such as X-ray diffraction (XRD), Fourier Transform-Infrared spectroscopy (FT-IR), Photoluminescence (PL) Field Emission Scanning Electron Microscopy (FE-SEM), Energy Dispersive Spectroscopy (EDS) and Transmission Electron Microscopy (TEM) were used to analyse the prepared nanoparticles for their physical, structural and optical properties. The characterization studies reveal that the synthesized PbO nanoparticles had well defined crystalline structure and sizes in the range of 25 nm to 36 nm for capping agents used and 40 nm for pure PbO nanoparticles.
Spontaneous grafting: a novel approach to graft diazonium cations on gold nanoparticles in aqueous medium and their self-assembly on electrodes.

PubMed

Kesavan, Srinivasan; John, S Abraham

2014-08-15

The spontaneous grafting of aminophenyl groups on gold nanoparticles (AuNPs) by reaction with in situ generated 4-aminophenyl diazonium cations (APD) in an aqueous medium was described. The spontaneous grafting was likely to proceed by transfer of electrons from AuNPs to the APD cations to form an aminophenyl radical and subsequent attachment with AuNPs. The aminophenyl (AP) functionalized gold nanoparticles (AP-AuNPs) were characterized by UV-visible spectroscopy, high resolution-transmission electron microscopy (HR-TEM), X-ray diffraction, FT-IR spectroscopy, X-ray photoelectron spectroscopy (XPS) and surface-enhanced Raman spectroscopy (SERS). The absence of characteristic vibrational bands corresponding to diazonium group in the FT-IR spectrum confirmed the reduction of the aminophenyl diazonium cations at the surface of AuNPs. The spontaneous attachment of AP on AuNPs was confirmed by XPS from the observed binding energy values for -NH2 at 399.4 eV and -N=N- at 400.2 eV. The SERS spectrum reveals the presence Au-C (437 cm(-1)) bond on AP-AuNPs. Further, the AP-AuNPs were self-assembled on GC/ITO electrode (AP-AuNPs modified electrode) with the aid of free amine groups present on the surface of AP-AuNPs via Michael's nucleophilic addition reaction. The AP-AuNPs modified electrode was characterized by cyclic voltammetry, impedance spectroscopy, UV-visible spectroscopy and scanning electron microscopy. Impedance studies show that the electron transfer reaction of [Fe(CN)6](3-/4-) was higher at the AP-AuNPs modified electrode (1.81×10(-4) cm s(-1)) than at bare (3.77×10(-5) cm s(-1)) GC electrode. Finally, the electrocatalytic activity of the AP-AuNPs modified electrode was demonstrated by studying the oxidation of dopamine (DA). Copyright © 2014 Elsevier Inc. All rights reserved.
Structural and DC electrical resistivity, magnetic properties of Co0.5M0.5Fe2O4 (M= Ni, Zn, and Mg) ferrite nanoparticles

NASA Astrophysics Data System (ADS)

Ramakrishna, A.; Murali, N.; Mammo, Tulu Wegayehu; Samatha, K.; Veeraiah, V.

2018-04-01

Inverse spinel structured nanoparticles of cobalt ferrite partially substituted by divalent cations of Ni, Zn, and Mg have been synthesized through sol-gel auto combustion route. Structural parameters are studied by powder X-ray diffraction at the diffraction angle range of 10-80°; and FT-IR spectroscopy in the wavenumber range of 1600-400 cm-1. Lattice parameters were calculated from the (hkl) values of the diffraction planes and interplanar spacing and found to be in the range of 8.3659-8.4197 Å. The surface morphology and crystalline nature are studied using scanning electron microscopy and also using HRTEM. The magnetic properties are analyzed through vibrating sample magnetometer. High saturation magnetization of 90.12 emu/g has been achieved from Co-Zn sample whereas high coercive force of 883.45 Oe is achieved in Co-Ni sample. A two-probe DC resistivity was measured in temperature ranges of 300-450 K.
A novel route for synthesis of nanocrystalline hydroxyapatite from eggshell waste.

PubMed

Siva Rama Krishna, D; Siddharthan, A; Seshadri, S K; Sampath Kumar, T S

2007-09-01

The eggshell waste has been value engineered to a nanocrystalline hydroxyapatite (HA) by microwave processing. To highlight the advantages of eggshell as calcium precursor in the synthesis of HA (OHA), synthetic calcium hydroxide was also used to form HA (SHA) following similar procedure and were compared with a commercially available pure HA (CHA). All the HAs were characterized by X-ray powder diffraction (XRD) method, Fourier transform infrared (FT-IR) spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and specific surface area measurements. Nanocrystalline nature of OHA is revealed through characteristic broad peaks in XRD patterns, platelets of length 33-50 nm and width 8-14 nm in TEM micrograph and size calculations from specific surface area measurements. FT-IR spectra showed characteristic bands of HA and additionally peaks of carbonate ions. The cell parameter calculations suggest the formation of carbonated HA of B-type. The OHA exhibits superior sinterability in terms of hardness and density than both SHA and CHA may be due to larger surface area of its spherulite structure. The in vitro dissolution study shows longer stability in phosphate buffer and cell culture test using osteoblast cells establishes biocompatibility of OHA.
Development of solid dispersions of artemisinin for transdermal delivery.

PubMed

Shahzad, Yasser; Sohail, Sadia; Arshad, Muhammad Sohail; Hussain, Talib; Shah, Syed Nisar Hussain

2013-11-30

Solid dispersions of the poorly soluble drug artemisinin were developed using polymer blends of polyvinylpyrrolidone (PVP) and polyethylene glycol (PEG) with the aim of enhancing solubility and in vitro permeation of artemisinin through skin. Formulations were characterised using a combination of molecular dynamics (MD) simulations, differential scanning calorimetry (DSC), X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FT-IR). Solubility of artemisinin was determined in two solvents: de-ionised water and phosphate buffered saline (PBS; pH 7.4), while in vitro drug permeation studies were carried out using rabbit skin as a model membrane. MD simulations revealed miscibility between the drug and polymers. DSC confirmed the molecular dispersion of the drug in the polymer blend. Decrease in crystallinity of artemisinin with respect to polymer content and the absence of specific drug-polymer interactions were confirmed using XRD and FT-IR, respectively. The solubility of artemisinin was dramatically enhanced for the solid dispersions, as was the permeation of artemisinin from saturated solid-dispersion vehicles relative to that from saturated solutions of the pure drug. The study suggests that high energy solid forms of artemisinin could possibly enable transdermal delivery of artemisinin. Copyright © 2013 Elsevier B.V. All rights reserved.

Eco-friendly synthesis of cuprous oxide (Cu2O) nanoparticles and improvement of their solar photocatalytic activities

NASA Astrophysics Data System (ADS)

Kerour, A.; Boudjadar, S.; Bourzami, R.; Allouche, B.

2018-07-01

In this work, we have synthesized cuprous oxide (Cu2O) nanoparticles with octahedral and spherical like shapes by an ecofriendly, simple and coast effective method, by using the aqueous extract of Aloe vera and copper sulfate as solvent and precursor respectively. The effect of Aloe vera aqueous extract concentration on the morphological, structural and optical properties of as synthesized nanoparticles was studied by Scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform (FT-IR) spectroscopy and UV-visible diffuse reflectance. The SEM images showing octahedral and spherical agglomeration of nanoparticles. The cubic structure of Cu2O was confirmed by XRD analysis, the crystallites size depends to the concentration of Aloe vera aqueous extract with an average size ranged between 24 and 61 nm. The FT-IR vibration measurements valid the presence of pure Cu2O in the samples. The UV-visible spectra show that the prepared cuprous oxide (Cu2O) has a gap energy estimated from 2.5 to 2.62 eV. The photocatalytic activities of the as-prepared material were highly improvement by the fast degradation of methylene blue in aqueous solution at room temperature under solar simulator irradiation.
Vibrational spectroscopy for imaging single microbial cells in complex biological samples

DOE PAGES

Harrison, Jesse P.; Berry, David

2017-04-13

Here, vibrational spectroscopy is increasingly used for the rapid and non-destructive imaging of environmental and medical samples. Both Raman and Fourier-transform infrared (FT-IR) imaging have been applied to obtain detailed information on the chemical composition of biological materials, ranging from single microbial cells to tissues. Due to its compatibility with methods such as stable isotope labeling for the monitoring of cellular activities, vibrational spectroscopy also holds considerable power as a tool in microbial ecology. Chemical imaging of undisturbed biological systems (such as live cells in their native habitats) presents unique challenges due to the physical and chemical complexity of themore » samples, potential for spectral interference, and frequent need for real-time measurements. This Mini Review provides a critical synthesis of recent applications of Raman and FT-IR spectroscopy for characterizing complex biological samples, with a focus on developments in single-cell imaging. We also discuss how new spectroscopic methods could be used to overcome current limitations of singlecell analyses. Given the inherent complementarity of Raman and FT-IR spectroscopic methods, we discuss how combining these approaches could enable us to obtain new insights into biological activities either in situ or under conditions that simulate selected properties of the natural environment.« less
Vibrational spectroscopy for imaging single microbial cells in complex biological samples

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

Harrison, Jesse P.; Berry, David

Here, vibrational spectroscopy is increasingly used for the rapid and non-destructive imaging of environmental and medical samples. Both Raman and Fourier-transform infrared (FT-IR) imaging have been applied to obtain detailed information on the chemical composition of biological materials, ranging from single microbial cells to tissues. Due to its compatibility with methods such as stable isotope labeling for the monitoring of cellular activities, vibrational spectroscopy also holds considerable power as a tool in microbial ecology. Chemical imaging of undisturbed biological systems (such as live cells in their native habitats) presents unique challenges due to the physical and chemical complexity of themore » samples, potential for spectral interference, and frequent need for real-time measurements. This Mini Review provides a critical synthesis of recent applications of Raman and FT-IR spectroscopy for characterizing complex biological samples, with a focus on developments in single-cell imaging. We also discuss how new spectroscopic methods could be used to overcome current limitations of singlecell analyses. Given the inherent complementarity of Raman and FT-IR spectroscopic methods, we discuss how combining these approaches could enable us to obtain new insights into biological activities either in situ or under conditions that simulate selected properties of the natural environment.« less
Spectroscopic characterization of zinc oxide nanorods synthesized by solid-state reaction

NASA Astrophysics Data System (ADS)

Prasad, Virendra; D'Souza, Charlene; Yadav, Deepti; Shaikh, A. J.; Vigneshwaran, Nadanathangam

2006-09-01

Well-crystallized zinc oxide nanorods have been fabricated by single step solid-state reaction using zinc acetate and sodium hydroxide, at room temperature. The sodium lauryl sulfate (SLS) stabilized zinc oxide nanorods were characterized by using X-ray diffraction, Fourier transform infrared spectroscopy, transmission electron microscopy and photoluminescence spectroscopy. The X-ray diffraction revealed the wurtzite structure of zinc oxide. The size estimation by XRD and TEM confirmed that the ZnO nanorods are made of single crystals. The growth of zinc oxide crystals into rod shape was found to be closely related to its hexagonal nature. The mass ratio of SLS:ZnO in the nanorods was found to be 1:10 based on the thermogravimetric analysis. Blue shift of photoluminescence emission was noticed in the ZnO nanorods when compared to that of ZnO bulk. FT-IR analysis confirmed the binding of SLS with ZnO nanorods. Apart from ease of preparation, this method has the advantage of eco-friendliness since the solvent and other harmful chemicals were eliminated in the synthesis protocol.
Green synthesis of soya bean sprouts-mediated superparamagnetic Fe 3O 4 nanoparticles

NASA Astrophysics Data System (ADS)

Cai, Yan; Shen, Yuhua; Xie, Anjian; Li, Shikuo; Wang, Xiufang

2010-10-01

Superparamagnetic Fe 3O 4 nanoparticles were first synthesized via soya bean sprouts (SBS) templates under ambient temperature and normal atmosphere. The reaction process was simple, eco-friendly, and convenient to handle. The morphology and crystalline phase of the nanoparticles were determined from scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED), and X-ray diffraction (XRD) spectra. The effect of SBS template on the formation of Fe 3O 4 nanoparticles was investigated using X-ray photoemission spectroscopy (XPS) and Fourier-transform infrared spectroscopy (FT-IR). The results indicate that spherical Fe 3O 4 nanoparticles with an average diameter of 8 nm simultaneously formed on the epidermal surface and the interior stem wall of SBS. The SBS are responsible for size and morphology control during the whole formation of Fe 3O 4 nanoparticles. In addition, the superconducting quantum interference device (SQUID) results indicate the products are superparamagnetic at room temperature, with blocking temperature ( TB) of 150 K and saturation magnetization of 37.1 emu/g.
Synthesis and luminescence properties of cinnamide based nanohybrid materials containing Eu (II) ions

NASA Astrophysics Data System (ADS)

Kiran Kumar, A. B. V.; Jayasimhadri, M.; Cha, Hyeongrae; Chen, Kuangcai; Lim, Jae-Min; Lee, Yong-Ill

2011-07-01

In the present work, the cinnamide based organic-inorganic hybrid luminescent materials were prepared by using sol-gel technique, in which both the components are covalently linked via Si-C bonds. The organic precursor N-(3-(triethoxysilyl)propyl)cinnamide (Cn-Si) was synthesized by (3-aminopropyl) triethoxysilane being reacted with cinnamoyal chloride. Finally, novel hybrid materials were prepared successfully through hydrolysis and polycondensation processes between the alkoxide groups of precursors Cn-Si and tetraethylorthosilane (TEOS) in the presence of europium nitrate. We have characterized thoroughly the prepared samples using FT-IR, thermal analysis (TGA/DTA), X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), energy-dispersive spectroscopy (EDS) and photoluminescence (PL) spectroscopy. The results indicate that these materials exhibit the excellent thermal stability up to 350 °C. The X-ray diffraction patterns confirmed the amorphous nature of the developed materials. The rare-earth doped hybrid materials have exhibited an intense green emission at 530 nm with CIE chromaticity coordinates (0.4801, 0.4669). Whereas, the un-doped one gives some remarkable blue emission properties under UV excitation.
FT-IR spectroscopy combined with DFT calculation to explore solvent effects of vinyl acetate

NASA Astrophysics Data System (ADS)

Chen, Yi; Zhang, Hui; Liu, Qing

The infrared vibration frequencies of vinyl acetate (VAc) in 18 different solvents were theoretically computed at Density Function Theory (DFT) B3LYP/6-311G* level based on Polarizable Continuum Model (PCM) and experimentally recorded by FT-IR spectroscopy. The solvent-induced long-range bulk electrostatic solvation free energies of VAc (ΔGelec) were calculated by the SMD model. The Cdbnd O stretching vibration frequencies of VAc were utilized as a measure of the chemical reactivities of the Cdbnd C group in VAc. The calculated and experimental Cdbnd O stretching vibration frequencies of VAc (νcal(Cdbnd O) and νexp(Cdbnd O)) were correlated with empirical solvent parameters including the KBM equation, the Swain equation and the linear solvation energy relationships (LSER). Through ab initio calculation, assignments of the two Cdbnd O absorption bands of VAc in alcohol solvents were achieved. The PCM, SMD and ab initio calculation offered supporting evidence to explain the FT-IR experimental observations from differing aspects.
Rapid and quantitative detection of the microbial spoilage of meat by fourier transform infrared spectroscopy and machine learning.

PubMed

Ellis, David I; Broadhurst, David; Kell, Douglas B; Rowland, Jem J; Goodacre, Royston

2002-06-01

Fourier transform infrared (FT-IR) spectroscopy is a rapid, noninvasive technique with considerable potential for application in the food and related industries. We show here that this technique can be used directly on the surface of food to produce biochemically interpretable "fingerprints." Spoilage in meat is the result of decomposition and the formation of metabolites caused by the growth and enzymatic activity of microorganisms. FT-IR was exploited to measure biochemical changes within the meat substrate, enhancing and accelerating the detection of microbial spoilage. Chicken breasts were purchased from a national retailer, comminuted for 10 s, and left to spoil at room temperature for 24 h. Every hour, FT-IR measurements were taken directly from the meat surface using attenuated total reflectance, and the total viable counts were obtained by classical plating methods. Quantitative interpretation of FT-IR spectra was possible using partial least-squares regression and allowed accurate estimates of bacterial loads to be calculated directly from the meat surface in 60 s. Genetic programming was used to derive rules showing that at levels of 10(7) bacteria.g(-1) the main biochemical indicator of spoilage was the onset of proteolysis. Thus, using FT-IR we were able to acquire a metabolic snapshot and quantify, noninvasively, the microbial loads of food samples accurately and rapidly in 60 s, directly from the sample surface. We believe this approach will aid in the Hazard Analysis Critical Control Point process for the assessment of the microbiological safety of food at the production, processing, manufacturing, packaging, and storage levels.
Structural and magnetic properties of nanocrystalline NiFe2O4 thin film prepared by spray pyrolysis technique

NASA Astrophysics Data System (ADS)

Chavan, Apparao R.; Chilwar, R. R.; Shisode, M. V.; Hivrekar, Mahesh M.; Mande, V. K.; Jadhav, K. M.

2018-05-01

The nanocrystalline NiFe2O4 thin film has been prepared using a spray pyrolysis technique on glass substrate. The prepared thin film was characterized by using X-ray diffraction (XRD), Fourier transform Infrared spectroscopy (FTIR), and Field Emission-Scanning Electron Microscopy (FE-SEM) characterization techniques for the structural and microstructural analysis. The magnetic property was measured using vibrating sample magnetometer (VSM) at room temperature. X-ray diffraction studies show the formation of single phase spinel structure of the thin film. The octahedral and tetrahedral vibration in the sample was studied by Fourier transform infrared (FT-IR) spectra. Magnetic hysteresis loop was recorded for thin film at room temperature. At 15 kOe, saturation magnetization (Ms) was found to increase while coercivity (Hc) decreases with thickness of the NiFe2O4 thin film.
Rare earth-doped lead borate glasses and transparent glass-ceramics: structure-property relationship.

PubMed

Pisarski, W A; Pisarska, J; Mączka, M; Lisiecki, R; Grobelny, Ł; Goryczka, T; Dominiak-Dzik, G; Ryba-Romanowski, W

2011-08-15

Correlation between structure and optical properties of rare earth ions in lead borate glasses and glass-ceramics was evidenced by X-ray-diffraction, Raman, FT-IR and luminescence spectroscopy. The rare earths were limited to Eu(3+) and Er(3+) ions. The observed BO(3)↔BO(4) conversion strongly depends on the relative PbO/B(2)O(3) ratios in glass composition, giving important contribution to the luminescence intensities associated to (5)D(0)-(7)F(2) and (5)D(0)-(7)F(1) transitions of Eu(3+). The near-infrared luminescence and up-conversion spectra for Er(3+) ions in lead borate glasses before and after heat treatment were measured. The more intense and narrowing luminescence lines suggest partial incorporation of Er(3+) ions into the orthorhombic PbF(2) crystalline phase, which was identified using X-ray diffraction analysis. Copyright © 2010 Elsevier B.V. All rights reserved.
Efficient mechanochemical bifunctional nanocatalysts for the conversion of isoeugenol to vanillin

NASA Astrophysics Data System (ADS)

Ostovar, Somayeh; Franco, Ana; Puente-Santiago, Alain R.; Pinilla-de Dios, María; Rodríguez-Padrón, Daily; Shaterian, Hamid R.; Luque, Rafael

2018-04-01

A novel highly functionalized nanocatalyst composed of iron containing SBA-15 material modified with sulfonic acid groups was synthesized by a mechanochemical approach. A full characterization of the obtained nanoreactor was performed by N2 physisorption isotherms analysis, transmission electron microscopy (TEM), X-ray powder diffraction (XRD) and Fourier-Infrared Spectroscopy (FT-IR). The mechanochemically synthesized nanocatalyst displays a high isoeugenol conversion to vanillin under mild conditions using H2O2 as oxidizing agent. Interestingly, this conversion resulted to be higher than that one obtained with the same material synthesized by an impregnation method. Additionally, the nanoreactor showed excellent reusability over four successive runs under the studied reaction conditions.
Enhanced corrosion resistance of strontium hydroxyapatite coating on electron beam treated surgical grade stainless steel

NASA Astrophysics Data System (ADS)

Gopi, D.; Rajeswari, D.; Ramya, S.; Sekar, M.; R, Pramod; Dwivedi, Jishnu; Kavitha, L.; Ramaseshan, R.

2013-12-01

The surface of 316L stainless steel (316L SS) is irradiated by high energy low current DC electron beam (HELCDEB) with energy of 500 keV and beam current of 1.5 mA followed by the electrodeposition of strontium hydroxyapatite (Sr-HAp) to enhance its corrosion resistance in physiological fluid. The coatings were characterised by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR) and High resolution scanning electron microscopy (HRSEM). The Sr-HAp coating on HELCDEB treated 316L SS exhibits micro-flower structure. Electrochemical results show that the Sr-HAp coating on HELCDEB treated 316L SS possesses maximum corrosion resistance in Ringer's solution.
Applications of FT-IR spectroscopy to the studies of esterification and crosslinking of cellulose by polycarboxylic acids: Part II. The performance of the crosslinked cotton fabrics

NASA Astrophysics Data System (ADS)

Wei, Weishu; Yang, Charles Q.

1998-06-01

Durable press finishing processes are commonly used in the textile industry to produce wrinkle-free cotton fabrics and garments. A durable press finishing agent forms covalent bands with cellulosic hydroxyl groups, thus crosslinking the cellulose molecules. The crosslinking of cellulose increases wrinkle resistance of the treated cotton fabric and reduces fabric mechanical strength. Wrinkle recovery angle (WRA) and tensile strength are the two most important parameters used to evaluate the performance of the crosslinked cotton fabrics and garments. In this study, we investigated the correlation between WRA and tensile strength on one hand, and the amount of crosslinkages formed by the crosslinking agents including dimethyloldihydroxylethyleneurea (DMDHEU) and 1,2,3,4-butanetetracarboxylic acid (BTCA) determined by FT-IR spectroscopy on the other hand. Linear regression curves between the carbonyl band absorbance, and WRA and tensile strength of the treated cotton fabric were developed. The data indicated that FT-IR spectroscopy is a reliable technique for predicting the performance of durable press finished cotton fabrics, therefore can be used as a convenient instrumental method for quality control in the textile and garment industry.
Chapter 1.1 Crystallinity of Nanocellulose Materials by Near-IR FT-Raman Spectroscopy

Treesearch

Umesh P. Agarwal; Richard S. Reiner; Sally A. Ralph

2013-01-01

Considering that crystallinity is one of the important properties that influence the end use of cellulose nanomaterials, it is important that the former be measured accurately. Recently, a new method based on near-IR FTRaman spectroscopy was proposed to determine cellulose I crystallinity. It was reported that in the Raman spectrum of cellulose materials, the...
Preparation and characterization of solid dispersion freeze-dried efavirenz - polyvinylpyrrolidone K-30.

PubMed

Fitriani, Lili; Haqi, Alianshar; Zaini, Erizal

2016-01-01

The aim of this research is to prepare and characterize solid dispersion of efavirenz - polyvinylpyrrolidone (PVP) K-30 by freeze drying to increase its solubility. Solid dispersion of efavirenz - PVP K-30 was prepared by solvent evaporation method with ratio 2:1, 1:1, and 1:2 and dried using a freeze dryer. Characterizations were done by scanning electron microscopy (SEM), powder X-ray diffraction analysis, differential thermal analysis (DTA), and Fourier transform infrared (FT-IR) spectroscopy. Solubility test was carried out in CO2-free distilled water, and efavirenz assay was conducted using high-performance liquid chromatography with acetonitrile:acetic acid (80:20) as the mobile phases. Powder X-ray diffractogram showed a decrease in the peak intensity, which indicated the crystalline altered to amorphous phase. DTA thermal analysis showed a decrease in the melting point of the solid dispersion compared to intact efavirenz. SEM results indicated the changes in the morphology of the crystal into an amorphous form compared to pure components. FT-IR spectroscopy analysis showed a shift wavenumber of the spectrum efavirenz and PVP K-30. The solubility of solid dispersion at ratio 2:1, 1:1, and 1:2 was 6.777 μg/mL, 6.936 μg/mL, and 14,672 μg/mL, respectively, whereas the solubility of intact efavirenz was 0.250 μg/mL. In conclusion, the solubility of solid dispersion increased significantly (P < 0.05).
Green synthesis of silver nanoparticles using Cordia dichotoma fruit extract and its enhanced antibacterial, anti-biofilm and photo catalytic activity

NASA Astrophysics Data System (ADS)

Bharathi, Devaraj; Vasantharaj, Seerangaraj; Bhuvaneshwari, V.

2018-05-01

The present study describes the antibacterial, anti-biofilm and photo catalytic activity of silver nanoparticles synthesized using Cordia dichotoma fruits (Cd-AgNPs) for the first time. The phyto-synthesized Cd-AgNPs were characterized by UV-Visible spectroscopy, Field emission-scanning electron microscopy (FE-SEM), Transmission electron microscopy (TEM), Energy dispersive x-ray spectrometer (EDX), Fourier transform infrared spectroscopy (FT-IR), and x-ray diffraction (XRD). FE-SEM and TEM observation showed that the average size of 2–60 nm with spherical shape of Cd-AgNPs and the presence of phyto-compounds which are responsible for capping and reduction were studied by FT-IR. XRD studies revealed the face-centered cubic structure of Cd-AgNPs. The synthesized Cd-AgNPs showed significant antibacterial activity against Gram-positive Staphylococcus aureus and Gram-negative Escherichia coli, assayed using agar well diffusion method. Phyto-synthesized Cd-AgNPs exhibited more than 90% inhibition of biofilm activity formed by S. aureus and E. coli. Furthermore, photocatalytic degradation of crystal violet (CV) under UV light irradiation using Cd-AgNPs was performed. Synthesized Cd-AgNPs exhibited ∼85% degradation activity for CV. Collectively, our findings suggest that C.dichotoma is a green source for the eco-friendly synthesis of Cd-AgNPs, which further can be used as a novel biocidal agent against bacterial pathogens and a potent photo catalytic agent.
Synthesis and characterization of arsenic-doped cysteine-capped thoria-based nanoparticles

NASA Astrophysics Data System (ADS)

Pereira, F. J.; Díez, M. T.; Aller, A. J.

2013-09-01

Thoria materials have been largely used in the nuclear industry. Nonetheless, fluorescent thoria-based nanoparticles provide additional properties to be applied in other fields. Thoria-based nanoparticles, with and without arsenic and cysteine, were prepared in 1,2-ethanediol aqueous solutions by a simple precipitation procedure. The synthesized thoria-based nanoparticles were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy dispersive X-ray spectrometry (ED-XRS), Raman spectroscopy, Fourier transform infrared (FT-IR) spectroscopy and fluorescence microscopy. The presence of arsenic and cysteine, as well as the use of a thermal treatment facilitated fluorescence emission of the thoria-based nanoparticles. Arsenic-doped and cysteine-capped thoria-based nanoparticles prepared in 2.5 M 1,2-ethanediol solutions and treated at 348 K showed small crystallite sizes and strong fluorescence. However, thoria nanoparticles subjected to a thermal treatment at 873 K also produced strong fluorescence with a very narrow size distribution and much smaller crystallite sizes, 5 nm being the average size as shown by XRD and TEM. The XRD data indicated that, even after doping of arsenic in the crystal lattice of ThO2, the samples treated at 873 K were phase pure with the fluorite cubic structure. The Raman and FT-IR spectra shown the most characteristics vibrational peaks of cysteine together with other peaks related to the bonds of this molecule to thoria and arsenic when present.
Purification, characterization and antioxidant properties of a novel polysaccharide extracted from Sorghum bicolor (L.) seeds in sausage.

PubMed

Ben Slima, Sirine; Ktari, Naourez; Trabelsi, Imen; Moussa, Hafedh; Makni, Iskandar; Ben Salah, Riadh

2018-01-01

A novel polysaccharide named Sorghum Water-Soluble Polysaccharide (SWSP) was purified from Sorghum bicolor (L.) seeds. It was structurally characterized by high performance liquid chromatography (HPLC), thin layer chromatography (TLC), Fourier transform-infrared spectroscopy analysis (FT-IR), X-ray diffraction (XRD) and mass spectroscopy (MS). HPLC and TLC showed that SWSP is a glucose polymer. The FT-IR spectrum proved the polysaccharide characteristic band of SWSP. XRD and microscopy analyses revealed that SWSP is a semi-crystalline polymer. Functional properties of SWSP were determined based on Water Holding Capacity (WHC), Oil Holding Capacity (OHC) and emulsification properties. SWSP showed good WHC and OHC, recorded at 3.01±0.03 and 1.02±0.03g/g, respectively and exhibited excellent emulsion properties even after 168h (61.5±0.02%). The effect of SWSP on oxidative stability of sausage during storage up to 12days at 4°C was investigated. Results showed a high rate (P<0.05) of oxymyoglobin and low lipid oxidation. The antioxidant activities of SWSP were also studied in vitro. Results demonstrated that the polysaccharides exhibited interesting 1,1-diphenyl-2-picrylhydrazyl (DPPH), ABTS radical scavenging, and ß-carotene bleaching inhibition activities. Overall, this natural polysaccharide was proved to enhance the oxidation stability of sausages, since it can efficiently substitute synthetic antioxidants in meat industry. Copyright © 2017 Elsevier B.V. All rights reserved.
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.
Catalytic and antibacterial properties of silver nanoparticles green biosynthesized using soluble green tea powder

NASA Astrophysics Data System (ADS)

Xu, Wei; Fan, Yapei; Liu, Xinfang; Luo, Denglin; Liu, Huan; Yang, Ningning

2018-04-01

Silver nanoparticles (Ag NPs) were green fabricated using soluble green tea powder (SGTP) as stabilizer and reducing agent. The properties and morphology of Ag NPs were investigated through UV–visible spectroscopy, field emission transmission electron microscope (FE-TEM) and fourier transform infrared (FT-IR). The spectroscopy showed surface plasmon resonance around at 420 nm revealing the synthesis of Ag NPs. FE-TEM results confirmed that the Ag NPs are spherical and face-centered cubic structure. FT-IR spectroscopy identified the role of various functional groups in the nanoparticle synthesis. The one spot biosynthesized Ag NPs showed favourable antibacterial properties on Escherichia coli and Staphyloccocus aureus, and excellent catalytic reduction of 4-nitrophenol. This work provided a feasible, green method to fabricate Ag NPs with promising photocatalytic and antimicrobial activities.

Synthesis and structural characterization of magnetic cadmium sulfide-cobalt ferrite nanocomposite, and study of its activity for dyes degradation under ultrasound

NASA Astrophysics Data System (ADS)

Farhadi, Saeed; Siadatnasab, Firouzeh

2016-11-01

Cadmium sulfide-cobalt ferrite (CdS/CFO) nanocomposite was easily synthesized by one-step hydrothermal decomposition of cadmium diethyldithiocarbamate complex on the CoFe2O4 nanoparticles at 200 °C. Spectroscopic techniques of powder X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FT-IR), UV-visible spectroscopy, field emission scanning electron microscopy (FESEM), energy-dispersive X-ray spectroscopy (EDX), Brunauer-Emmett-Teller (BET), and magnetic measurements were applied for characterizing the structure and morphology of the product. The results of FT-IR, XRD and EDX indicated that the CdS/CFO was highly pure. SEM and TEM results revealed that the CdS/CFO nanocomposite was formed from nearly uniform and sphere-like nanoparticles with the size of approximately 20 nm. The UV-vis absorption spectrum of the CdS/CFO nanocomposite showed the band gap of 2.21 eV, which made it suitable for sono-/photo catalytic purposes. By using the obtained CdS/CFO nanocomposite, an ultrasound-assisted advanced oxidation process (AOP) has been developed for catalytic degradation of methylene blue (MB), Rhodamine B (RhB), and methyl orange (MO)) in the presence of H2O2 as a green oxidant. CdS/CFO nanocomposite exhibited excellent sonocatalytic activity, so that, dyes were completely degraded in less than 10 min. The influences of crucial factors such as the H2O2 amount and catalyst dosage on the degradation efficiency were evaluated. The as-prepared CdS/CFO nanocomposite exhibited higher catalytic activity than pure CdS nanoparticles. Moreover, the magnetic property of CoFe2O4 made the nanocomposite recyclable.
Control of the shape and size of iron oxide (α-Fe2O3) nanoparticles synthesized through the chemical precipitation method

NASA Astrophysics Data System (ADS)

Lassoued, Abdelmajid; Dkhil, Brahim; Gadri, Abdellatif; Ammar, Salah

Hematite (α-Fe2O3) nanoparticles were synthesized via a simple chemical precipitation method. The impact of varying the concentration of precursor on the crystalline phase, size and morphology of α-Fe2O3 products was explored. The characteristic of the synthesized hematite nanoparticles were evaluated by X-ray diffraction (XRD), Transmission Electron Microscopy (TEM), Scanning Electron Microscopy (SEM), Fourier Transform Infra-Red (FT-IR) spectroscopy, Raman spectroscopy, Differential Thermal Analysis (DTA), Thermo Gravimetric Analysis (TGA), Ultraviolet-Visible (UV-Vis) analysis and Photoluminescence (PL). XRD data revealed a rhombohedral (hexagonal) structure with the space group R-3c in all samples. Uniform spherical like morphology was confirmed by TEM and SEM. The result revealed that the particle sizes were varied between 21 and 82 nm and that the increase in precursor concentration (FeCl3, 6H2O) is accompanied by an increase in the particle size of 21 nm for pure α-Fe2O3 synthesized with [Fe3+] = 0.05 M at 82 nm for pure α-Fe2O3 synthesized with [Fe3+] = 0.4 M. FT-IR confirms the phase purity of the nanoparticles synthesized. The Raman spectroscopy was used not only to prove that we have synthesized pure hematite but also to identify their phonon modes. The thermal behavior of compound was studied by using TGA/DTA results: The TGA showed three mass losses, whereas DTA resulted in three endothermic peaks. Besides, the optical investigation revealed that samples have an optical gap of about 2.1 eV and that this value varies as a function of the precursor concentration.
Sonochemical synthesis of terbium tungstate for developing high power supercapacitors with enhanced energy densities.

PubMed

Sobhani-Nasab, Ali; Rahimi-Nasrabadi, Mehdi; Naderi, Hamid Reza; Pourmohamadian, Vafa; Ahmadi, Farhad; Ganjali, Mohammad Reza; Ehrlich, Hermann

2018-07-01

Sonochemically prepared nanoparticles of terbium tungstate (TWNPs) were evaluated through scanning electron microscopy (SEM), thermogravimetric analysis (TGA), X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FT-IR), UV-Vis spectroscopy, and the optimal products were further characterized in terms of their electrochemical properties using conventional and continuous cyclic voltammetry (CV, and CCV), galvanostatic charge/discharge technique, and electrochemical impedance spectroscopy (EIS). The CV studies indicated the TWNPs to have specific capacitance (SC) values of 336 and 205 F g -1 at 1 and 200 mV s -1 , and galvanostatic charge-discharge tests revealed the SC of the TWNP-based electrodes to be 300 F g -1 at 1 Ag -1 . Also continuous cyclic voltammetry evaluations proved the sample as having a capacitance retention value of 95.3% after applying 4000 potential cycles. In the light of the results TWNPs were concluded as favorable electrode materials for use in hybrid vehicle systems. Copyright © 2018 Elsevier B.V. All rights reserved.
Investigation of optical properties and the photocatalytic activity of synthesized YbYO4 nanoparticles and YbVO4/NiWO4 nanocomposites by polymeric capping agents

NASA Astrophysics Data System (ADS)

Pourmasoud, Saeid; Sobhani-Nasab, Ali; Behpour, Mohsen; Rahimi-Nasrabadi, Mehdi; Ahmadi, Farhad

2018-04-01

YbVO4 nanoparticles YbVO4/NiWO4 nanocomposites were synthesized by simple and new method. The effect of various polymeric capping agents such as Tween 80, Tween 20 and PEG on the shape and size of YbVO4/NiWO4 nanocomposites were investigated. YbVO4/NiWO4 nanocomposites were analyzed through some techniques including, X-ray diffraction (XRD), Fourier-transform infrared (FT-IR) spectroscopy, vibrating sample magnetometer (VSM), thermogravimetry differential thermal analysis (TG-DTA), transmission electron microscopy (TEM), field emission electron microscopy (FESEM), ultraviolet-visible spectroscopy (UV-Vis), and energy-dispersive X-ray spectroscopy (EDX). This attempt is the first study on the photocatalytic performance of the YbVO4/NiWO4 nanocomposites in various conditions such as size of particles and kind of dyes (rhodamine B (Rh B), methylene blue (MB), methyl orange (MO), and phenol red (Ph R)), under visible light.
Influence of the ultrasound-assisted synthesis of Cu-BTC metal-organic frameworks nanoparticles on uptake and release properties of rifampicin.

PubMed

Abbasi, Amir Reza; Rizvandi, Maryam

2018-01-01

In this work, we study uptake and release properties of rifampicin (denoted henceforth as Rif) from ultrasound-assisted synthesis Cu-BTC nanoparticles in comparison with bulk Cu-BTC and activated carbon. To explore the absorption ability of the Cu-BTC to Rif, fresh sample of Cu-BTC was immersed in an aqueous solution of Rif and were monitored in real time with UV/vis spectroscopy. Results show that the adsorbed quantity of Rif over nano Cu-BTC (denoted henceforth as I) is much higher than those over a bulk Cu-BTC (denoted henceforth as II) and activated carbon. In compound I and all of the nano-MOFs the channel length is decreased so that the amount of adsorption is increased a little. The samples were characterized with X-ray powder diffraction (XRD), Scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR), and UV/vis spectroscopy. Copyright © 2017 Elsevier B.V. All rights reserved.
Synthesis, optical properties and efficient photocatalytic activity of CdO/ZnO hybrid nanocomposite

NASA Astrophysics Data System (ADS)

Reddy, Ch Venkata; Babu, B.; Shim, Jaesool

2018-01-01

Pure CdO, ZnO and CdO/ZnO hybrid nanocomposite photocatalyst were synthesized using simple co-precipitation technique and studied in detail. The synthesized photocatalysts were characterized using several measurements such as X-ray diffraction (XRD), high-resolution transmission electron microscopy (HRTEM), surface analysis (BET), diffuse reflectance UV-vis spectroscopy, X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, FT-IR, TG-DTA and photoluminescence (PL). The XRD results revealed that the hexagonal and cubic crystal structure of CdO and ZnO nanoparticles. The optical response for the composite showed the presence of separate absorption signature for CdO and ZnO in the visible region at about 510 nm and 360 nm respectively. The CdO/ZnO hybrid nanocomposite photocatalyst exhibited enhanced photocatalytic degradation activity compared to pristine CdO and ZnO. The enhanced photocatalytic activity may be due to the higher specific surface area and significantly reduced the electron-hole recombination rate.
Synthesis and Characterization of Highly Intercalated Graphite Bisulfate

NASA Astrophysics Data System (ADS)

Salvatore, Marcella; Carotenuto, Gianfranco; De Nicola, Sergio; Camerlingo, Carlo; Ambrogi, Veronica; Carfagna, Cosimo

2017-03-01

Different chemical formulations for the synthesis of highly intercalated graphite bisulfate have been tested. In particular, nitric acid, potassium nitrate, potassium dichromate, potassium permanganate, sodium periodate, sodium chlorate, and hydrogen peroxide have been used in this synthesis scheme as the auxiliary reagent (oxidizing agent). In order to evaluate the presence of delamination, and pre-expansion phenomena, and the achieved intercalation degree in the prepared samples, the obtained graphite intercalation compounds have been characterized by scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), X-ray powder diffraction (XRD), infrared spectroscopy (FT-IR), micro-Raman spectroscopy ( μ-RS), and thermal analysis (TGA). Delamination and pre-expansion phenomena were observed only for nitric acid, sodium chlorate, and hydrogen peroxide, while the presence of strong oxidizers (KMnO4, K2Cr2O7) led to stable graphite intercalation compounds. The largest content of intercalated bisulfate is achieved in the intercalated compounds obtained from NaIO4 and NaClO3.
Green synthesis of the Pd nanoparticles supported on reduced graphene oxide using barberry fruit extract and its application as a recyclable and heterogeneous catalyst for the reduction of nitroarenes.

PubMed

Nasrollahzadeh, Mahmoud; Sajadi, S Mohammad; Rostami-Vartooni, Akbar; Alizadeh, Mohammad; Bagherzadeh, Mojtaba

2016-03-15

Through this manuscript the green synthesis of palladium nanoparticles supported on reduced graphene oxide (Pd NPs/RGO) under the mild conditions through reduction of the graphene oxide and Pd(2+) ions using barberry fruit extract as reducing and stabilizing agent is reported. The as-prepared Pd NPs/RGO was characterized by UV-vis spectroscopy, X-ray diffraction (XRD), Fourier transformed infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM) and energy dispersive X-ray spectroscopy (EDS). The Pd NPs/RGO could be used as an efficient and heterogeneous catalyst for reduction of nitroarenes using sodium borohydride in an environmental friendly medium. Excellent yields of products were obtained with a wide range of substrates and the catalyst was recycled multiple times without any significant loss of its catalytic activity. Copyright © 2015 Elsevier Inc. All rights reserved.
Green synthesis of size controllable gold nanoparticles

NASA Astrophysics Data System (ADS)

Mohan Kumar, Kesarla; Mandal, Badal Kumar; Kiran Kumar, Hoskote A.; Maddinedi, Sireesh Babu

2013-12-01

A facile rapid green eco-friendly method to synthesize gold nanoparticles (Au NPs) of tunable size using aqueous Terminalia arjuna fruit extracts has been demonstrated herein. Formation of Au NPs was confirmed by Surface Plasmon Resonance (SPR) study at 528 nm using UV-visible spectrophotometer. The time of reduction, size and morphological variations of Au NPs were studied with varying quantities of T. arjuna fruit aqueous extracts. Synthesized Au NPs were characterized using UV-visible spectroscopy, Fourier transformed infrared spectroscopy (FT-IR), powder X-ray diffraction (XRD), transmission electron microscopy (TEM) and Energy dispersive X-ray spectroscopy (EDAX). Polyphenols responsible for reduction of Au3+ to Au0 were identified using High Performance Liquid Chromatography (HPLC) as ascorbic acid, gallic acid and pyrogallol. The oxidized forms of polyphenols formed coordination with surface of Au NPs which protected their further growth and aggregation. We also propose a plausible mechanism how to tune size and shape of Au NPs by varying the quantity of extracts. Thus obtained Au NPs were stable for more than four months.
Synthesis and Characterization of Highly Intercalated Graphite Bisulfate.

PubMed

Salvatore, Marcella; Carotenuto, Gianfranco; De Nicola, Sergio; Camerlingo, Carlo; Ambrogi, Veronica; Carfagna, Cosimo

2017-12-01

Different chemical formulations for the synthesis of highly intercalated graphite bisulfate have been tested. In particular, nitric acid, potassium nitrate, potassium dichromate, potassium permanganate, sodium periodate, sodium chlorate, and hydrogen peroxide have been used in this synthesis scheme as the auxiliary reagent (oxidizing agent). In order to evaluate the presence of delamination, and pre-expansion phenomena, and the achieved intercalation degree in the prepared samples, the obtained graphite intercalation compounds have been characterized by scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), X-ray powder diffraction (XRD), infrared spectroscopy (FT-IR), micro-Raman spectroscopy (μ-RS), and thermal analysis (TGA). Delamination and pre-expansion phenomena were observed only for nitric acid, sodium chlorate, and hydrogen peroxide, while the presence of strong oxidizers (KMnO 4 , K 2 Cr 2 O 7 ) led to stable graphite intercalation compounds. The largest content of intercalated bisulfate is achieved in the intercalated compounds obtained from NaIO 4 and NaClO 3 .
Achillea millefolium L. extract mediated green synthesis of waste peach kernel shell supported silver nanoparticles: Application of the nanoparticles for catalytic reduction of a variety of dyes in water.

PubMed

Khodadadi, Bahar; Bordbar, Maryam; Nasrollahzadeh, Mahmoud

2017-05-01

In this paper, silver nanoparticles (Ag NPs) are synthesized using Achillea millefolium L. extract as reducing and stabilizing agents and peach kernel shell as an environmentally benign support. FT-IR spectroscopy, UV-Vis spectroscopy, X-ray Diffraction (XRD), Field emission scanning electron microscopy (FESEM), Energy Dispersive X-ray Spectroscopy (EDS), Thermo gravimetric-differential thermal analysis (TG-DTA) and Transmission Electron Microscopy (TEM) were used to characterize peach kernel shell, Ag NPs, and Ag NPs/peach kernel shell. The catalytic activity of the Ag NPs/peach kernel shell was investigated for the reduction of 4-nitrophenol (4-NP), Methyl Orange (MO), and Methylene Blue (MB) at room temperature. Ag NPs/peach kernel shell was found to be a highly active catalyst. In addition, Ag NPs/peach kernel shell can be recovered and reused several times with no significant loss of its catalytic activity. Copyright © 2017 Elsevier Inc. All rights reserved.
Mechanochemical solvent-free in situ synthesis of drug-loaded {Cu2(1,4-bdc)2(dabco)}n MOFs for controlled drug delivery

NASA Astrophysics Data System (ADS)

Nadizadeh, Zahra; Naimi-Jamal, M. Reza; Panahi, Leila

2018-03-01

In the present study, ibuprofen-loaded nano metal-organic frameworks (NMOFs) {Cu2(1,4-bdc)2(dabco)}n and {Cu2(1,4-bdc-NH2)2(dabco)}n (bdc=benzenedicarboxylic acid, and dabco=diazabicyclooctane) were synthesized by ball-milling at room temperature in 2 h. The produced drug-loaded Cu-NMOFs were studied as ibuprofen drug delivery system and exhibited well-defined drug release behavior, exceptionally high drug loading capacities and the ability to entrap the model drug. The loading efficiency for ibuprofen was determined about 50.54% and 50.27%, respectively. The drug release of NMOFs was also monitored, and all of the loaded drug was released in 1 day. The NMOFs were characterized by FT-IR spectroscopy, X-ray powder diffraction (XRPD), thermogravimetric analysis (TGA), SEM (scanning electron microscopy), transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy (EDS), inductively coupled plasma (ICP), UV-vis spectroscopy and N2 adsorption porosimetry (BET&BJH).
Classification of edible oils and modeling of their physico-chemical properties by chemometric methods using mid-IR spectroscopy

NASA Astrophysics Data System (ADS)

Luna, Aderval S.; da Silva, Arnaldo P.; Ferré, Joan; Boqué, Ricard

This research work describes two studies for the classification and characterization of edible oils and its quality parameters through Fourier transform mid infrared spectroscopy (FT-mid-IR) together with chemometric methods. The discrimination of canola, sunflower, corn and soybean oils was investigated using SVM-DA, SIMCA and PLS-DA. Using FT-mid-IR, DPLS was able to classify 100% of the samples from the validation set, but SIMCA and SVM-DA were not. The quality parameters: refraction index and relative density of edible oils were obtained from reference methods. Prediction models for FT-mid-IR spectra were calculated for these quality parameters using partial least squares (PLS) and support vector machines (SVM). Several preprocessing alternatives (first derivative, multiplicative scatter correction, mean centering, and standard normal variate) were investigated. The best result for the refraction index was achieved with SVM as well as for the relative density except when the preprocessing combination of mean centering and first derivative was used. For both of quality parameters, the best results obtained for the figures of merit expressed by the root mean square error of cross validation (RMSECV) and prediction (RMSEP) were equal to 0.0001.
Novel preparation of highly photocatalytically active copper chromite nanostructured material via a simple hydrothermal route

PubMed Central

Beshkar, Farshad; Zinatloo-Ajabshir, Sahar; Bagheri, Samira; Salavati-Niasari, Masoud

2017-01-01

Highly photocatalytically active copper chromite nanostructured material were prepared via a novel simple hydrothermal reaction between [Cu(en)2(H2O)2]Cl2 and [Cr(en)3]Cl3.3H2O at low temperature, without adding any pH regulator or external capping agent. The as-synthesized nanostructured copper chromite was analyzed by transmission electron microscopy (TEM), UV–vis diffuse reflectance spectroscopy, energy dispersive X-ray microanalysis (EDX), scanning electron microscopy (SEM), X-ray diffraction (XRD) and Fourier transform infrared (FT-IR) spectroscopy. Results of the morphological investigation of the as-synthesized products illustrate that the shape and size of the copper chromite depended on the surfactant sort, reaction duration and temperature. Moreover, the photocatalytic behavior of as-obtained copper chromite was evaluated by photodegradation of acid blue 92 (anionic dye) as water pollutant. PMID:28582420
The fabrication of visible light responsive Ag-SiO2 co-doped TiO2 thin films by the sol-gel method

NASA Astrophysics Data System (ADS)

Dam Le, Duy; Dung Dang, Thi My; Thang Chau, Vinh; Chien Dang, Mau

2010-03-01

In this study we have successfully deposited Ag-SiO2 co-doped TiO2 thin films on glass substrates by the sol-gel method. After being coated by a dip coating method, the film was transparent, smooth and had strong adhesion on the glass surface. The deposited film was characterized by x-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), ultraviolet-visible spectroscopy (UV-Vis), a scanning electron microscope (SEM) and atomic force microscope (AFM) to investigate its crystallization, transmittance and surface structure. The antifogging ability is explained by the contact angle of water on the surface of the glass substrates under visible-light. The obtained results show that Ag-SiO2 co-doped TiO2 film has potential applications for self cleaning and anti-bacterial ceramic tiles.
Anchoring of Cu(II) onto surface of porous metal-organic framework through post-synthesis modification for the synthesis of benzimidazoles and benzothiazoles

NASA Astrophysics Data System (ADS)

Kardanpour, Reihaneh; Tangestaninejad, Shahram; Mirkhani, Valiollah; Moghadam, Majid; Mohammadpoor-Baltork, Iraj; Zadehahmadi, Farnaz

2016-03-01

Efficient synthesis of various benzimidazoles and benzothiazoles under mild conditions catalyzed by Cu(II) anchored onto UiO-66-NH2 metal organic framework is reported. In this manner, first, the aminated UiO-66 was modified with thiophene-2-carbaldehyde and then the prepared Schiff base was reacted with CuCl2. The prepared catalyst was characterized by FT-IR, UV-vis, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), N2 adsorption, inductively coupled plasma atomic emission spectroscopy (ICP-AES) and field emission scanning electron microscopy (FE-SEM). The UiO-66-NH2-TC-Cu was applied as a highly efficient catalyst for synthesis of benzimidazole and benzothiazole derivatives by the reaction of aldehydes with 1,2-diaminobenzene or 2-aminothiophenol. The Cu(II)-containing MOF was reused several times without any appreciable loss of its efficiency.
Green synthesis of silver nanoparticles using Alternanthera dentata leaf extract at room temperature and their antimicrobial activity.

PubMed

Kumar, Deenadayalan Ashok; Palanichamy, V; Roopan, Selvaraj Mohana

2014-06-05

A green rapid biogenic synthesis of silver nanoparticles AgNPs using Alternanthera dentata (A. dentata) aqueous extract was demonstrated in this present study. The formation of silver nanoparticles was confirmed by Surface Plasmon Resonance (SPR) at 430nm using UV-visible spectrophotometer. The reduction of silver ions to silver nanoparticles by A. dentata extract was completed within 10min. Synthesized nanoparticles were characterized using UV-visible spectroscopy; Fourier transformed infrared spectroscopy (FT-IR), X-ray diffraction (XRD), scanning electron microscopy and transmission electron microscopy (TEM). The extracellular silver nanoparticles synthesis by aqueous leaf extract demonstrates rapid, simple and inexpensive method comparable to chemical and microbial methods. The colloidal solution of silver nanoparticles were found to exhibit antibacterial activity against Escherichia coli, Pseudomonas aeruginosa, Klebsiella pneumonia and, Enterococcus faecalis. Copyright © 2014 Elsevier B.V. All rights reserved.
The alterations in high density polyethylene properties with gamma irradiation

NASA Astrophysics Data System (ADS)

Zaki, M. F.; Elshaer, Y. H.; Taha, Doaa. H.

2017-10-01

In the present investigation, high density polyethylene (HDPE) polymer has been used to study the alterations in its properties under gamma-irradiation. Physico-chemical properties have been investigated with different spectroscopy techniques, Fourier Transform Infrared spectroscopy (FTIR), X-ray diffraction (XRD), biocompatibility properties, as well as, mechanical properties change. The FT-IR analysis shows the formation of new band at 1716 cm-1 that is attributed to the oxidation of irradiated polymer chains, which is due to the formation of carbonyl groups (C˭O). XRD patterns show that a decrease in the crystallite size and increase in the Full Width at Half Maximum (FWHM). This means that the crystallinity of irradiated samples is decreased with increase in gamma dose. The contact angle measurements show an increase in the surface free energy as the gamma irradiation increases. The measurements of mechanical properties of irradiated HDPE samples were discussed.
In vitro and in vivo anti-inflammatory properties of green synthesized silver nanoparticles using Viburnum opulus L. fruits extract.

PubMed

Moldovan, Bianca; David, Luminita; Vulcu, Adriana; Olenic, Liliana; Perde-Schrepler, Maria; Fischer-Fodor, Eva; Baldea, Ioana; Clichici, Simona; Filip, Gabriela Adriana

2017-10-01

A green, rapid and cost effective method for the bio-synthesis of silver nanoparticles (AgNPs), using polyphenols present in European cranberry bush fruit extracts was developed. The obtained AgNPs were characterized by ultra-violet visible spectroscopy (UV-VIS), Fourier transform - infrared spectroscopy (FT-IR), transmission electron microscopy (TEM) and X-ray diffraction patterns (XRD). The average size of the spherical AgNPs was found to be 25nm. The anti-inflammatory effect of the biomaterials was investigated, both in vitro (on HaCaT cell line, exposed to UVB radiation) and in vivo (on acute inflammation model in Wistar rats). Our results support the conclusion that the photosynthesized silver nanoparticles present a potent anti-inflammatory activity and could be successfully used as therapeutic tools for treatment of inflammation. Copyright © 2017 Elsevier B.V. All rights reserved.
Using IR spectroscopy to determine biodiesel conversion

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

Tirla, Cornelia; Dooling, Thomas; Smith, Rachel B.

This project’s aim was to develop a way to use Infrared (IR) Spectroscopy to determine the extent of the conversion of oil to biodiesel produced during a typical transesterification process. The most reliable method of biodiesel analysis is gas chromatography with flame ionization detector (GC-FID) analysis. This analysis is not ideal for the educational or field applications since it is time intensive and requires expensive, specialized equipment. The use of the FT-IR is faster and more affordable. A calibration curve was created by comparing data on the purity of biodiesel samples obtained from the GC-FID analysis to the ratio ofmore » the absorbances at 1197 cm -1 to 1166 cm -1 from the FT-IR spectrum. For field application, a similar method was developed using a portable IR spectrometer, the InfraSpecTM VFA-IR spectrometer. As a result, the data collected gave a good linear fit for % purity of the samples and can be used as a method for monitoring the conversion of different types of oils to biodiesel and determining the purity of biodiesel produced from oil.« less

Using IR spectroscopy to determine biodiesel conversion

DOE PAGES

Tirla, Cornelia; Dooling, Thomas; Smith, Rachel B.; ...

2013-01-01

This project’s aim was to develop a way to use Infrared (IR) Spectroscopy to determine the extent of the conversion of oil to biodiesel produced during a typical transesterification process. The most reliable method of biodiesel analysis is gas chromatography with flame ionization detector (GC-FID) analysis. This analysis is not ideal for the educational or field applications since it is time intensive and requires expensive, specialized equipment. The use of the FT-IR is faster and more affordable. A calibration curve was created by comparing data on the purity of biodiesel samples obtained from the GC-FID analysis to the ratio ofmore » the absorbances at 1197 cm -1 to 1166 cm -1 from the FT-IR spectrum. For field application, a similar method was developed using a portable IR spectrometer, the InfraSpecTM VFA-IR spectrometer. As a result, the data collected gave a good linear fit for % purity of the samples and can be used as a method for monitoring the conversion of different types of oils to biodiesel and determining the purity of biodiesel produced from oil.« less
Validation of ATR FT-IR to identify polymers of plastic marine debris, including those ingested by marine organisms.

PubMed

Jung, Melissa R; Horgen, F David; Orski, Sara V; Rodriguez C, Viviana; Beers, Kathryn L; Balazs, George H; Jones, T Todd; Work, Thierry M; Brignac, Kayla C; Royer, Sarah-Jeanne; Hyrenbach, K David; Jensen, Brenda A; Lynch, Jennifer M

2018-02-01

Polymer identification of plastic marine debris can help identify its sources, degradation, and fate. We optimized and validated a fast, simple, and accessible technique, attenuated total reflectance Fourier transform infrared spectroscopy (ATR FT-IR), to identify polymers contained in plastic ingested by sea turtles. Spectra of consumer good items with known resin identification codes #1-6 and several #7 plastics were compared to standard and raw manufactured polymers. High temperature size exclusion chromatography measurements confirmed ATR FT-IR could differentiate these polymers. High-density (HDPE) and low-density polyethylene (LDPE) discrimination is challenging but a clear step-by-step guide is provided that identified 78% of ingested PE samples. The optimal cleaning methods consisted of wiping ingested pieces with water or cutting. Of 828 ingested plastics pieces from 50 Pacific sea turtles, 96% were identified by ATR FT-IR as HDPE, LDPE, unknown PE, polypropylene (PP), PE and PP mixtures, polystyrene, polyvinyl chloride, and nylon. Published by Elsevier Ltd.
Toward the characterization of biological toxins using field-based FT-IR spectroscopic instrumentation

NASA Astrophysics Data System (ADS)

Schiering, David W.; Walton, Robert B.; Brown, Christopher W.; Norman, Mark L.; Brewer, Joseph; Scott, James

2004-12-01

IR spectroscopy is a broadly applicable technique for the identification of covalent materials. Recent advances in instrumentation have made Fourier Transform infrared (FT-IR) spectroscopy available for field characterization of suspect materials. Presently, this instrumentation is broadly deployed and used for the identification of potential chemical hazards. This discussion concerns work towards expanding the analytical utility of field-based FT-IR spectrometry in the characterization of biological threats. Two classes of materials were studied: biologically produced chemical toxins which were non-peptide in nature and peptide toxin. The IR spectroscopic identification of aflatoxin-B1, trichothecene T2 mycotoxin, and strychnine was evaluated using the approach of spectral searching against large libraries of materials. For pure components, the IR method discriminated the above toxins at better than the 99% confidence level. The ability to identify non-peptide toxins in mixtures was also evaluated using a "spectral stripping" search approach. For the mixtures evaluated, this method was able to identify the mixture components from ca. 32K spectral library entries. Castor bean extract containing ricin was used as a representative peptide toxin. Due to similarity in protein spectra, a SIMCA pattern recognition methodology was evaluated for classifying peptide toxins. In addition to castor bean extract the method was validated using bovine serum albumin and myoglobin as simulants. The SIMCA approach was successful in correctly classifying these samples at the 95% confidence level.
Intercalation of IR absorber into layered double hydroxides: Preparation, thermal stability and selective IR absorption

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

Zhu, Haifeng; Tang, Pinggui; Feng, Yongjun, E-mail: yjfeng@mail.buct.edu.cn

2012-03-15

Highlights: Black-Right-Pointing-Pointer PMIDA anions were intercalated into Mg{sub 2}Al-NO{sub 3} LDH by anion-exchange method. Black-Right-Pointing-Pointer The prepared material has highly selective IR absorption property in 9-11 {mu}m. Black-Right-Pointing-Pointer The obtained material has practical applications as heat-retaining additive. -- Abstract: N-phosphonomethyl aminodiacetic acid (PMIDA) was intercalated into the interlayer spacing of layered double hydroxides (LDH) by an anion-exchange method. The intercalated LDHs were characterized by various techniques such as powder X-ray diffraction (XRD), FT-IR spectroscopy, elemental analysis and simultaneous thermogravimetric and mass spectrometry (TG-MS) in details. The results show the formation of Mg{sub 2}Al-PMIDA LDH based on the expansion of d-spacingmore » from 0.89 nm to 1.22 nm and the disappearance of the characteristic IR absorption band at 1384 cm{sup -1} for NO{sub 3}{sup -} anions. The incorporation of Mg{sub 2}Al-PMIDA LDH into the low density polyethylene (LDPE) as an additive enhances the selectivity of IR absorption in the main wavelength region 9-11 {mu}m for radiant heat loss at night. Mg{sub 2}Al-PMIDA LDH as a heat-retaining additive has practical application in agricultural plastic films.« less
Non-intercalative, deoxyribose binding of boric acid to calf thymus DNA.

PubMed

Ozdemir, Ayse; Gursaclı, Refiye Tekiner; Tekinay, Turgay

2014-05-01

The present study characterizes the effects of the boric acid binding on calf thymus DNA (ct-DNA) by spectroscopic and calorimetric methods. UV-Vis absorbance spectroscopy, circular dichroism (CD) spectroscopy, transmission electron microscopy (TEM), isothermal titration calorimetry (ITC), and Fourier transform infrared (FT-IR) spectroscopy were employed to characterize binding properties. Changes in the secondary structure of ct-DNA were determined by CD spectroscopy. Sizes and morphologies of boric acid-DNA complexes were determined by transmission electron microscopy (TEM). The kinetics of boric acid binding to calf thymus DNA (ct-DNA) was investigated by isothermal titration calorimetry (ITC). ITC results revealed that boric acid exhibits a moderate affinity to ct-DNA with a binding constant (K a) of 9.54 × 10(4) M(-1). FT-IR results revealed that boric acid binds to the deoxyribose sugar of DNA without disrupting the B-conformation at tested concentrations.
Cu-based metal-organic framework/activated carbon composites for sulfur compounds removal

NASA Astrophysics Data System (ADS)

Fan, Hui-Ling; Shi, Rui-Hua; Zhang, Zhen-Rong; Zhen, Tian; Shangguan, Ju; Mi, Jie

2017-02-01

MOF-199 was modified by incorporating activated carbon (AC) during its synthesis under hydrothermal conditions to improve its performance in the removal of hydrogen sulfide (H2S) and dimethyl sulfide (CH3SCH3). A variety of different characterization techniques including X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, nitrogen adsorption/desorption isotherms, scanning electron microscopy (SEM), pyridine adsorption infrared spectroscopy (Py-IR), thermogravimetric- mass spectroscopy (TG-MS) and X-ray photoelectron spectroscopy (XPS) were used to analyze the fresh and exhausted composites. It was found that the composites, which have an amount of AC of less than 2%, had the same morphology as those of pristine MOF-199, but exhibited a more ordered crystallinity structure as well as higher surface area. The composite with 2% AC incorporation showed highest sulfur capacity of 8.46 and 8.53% for H2S and CH3SCH3, respectively, which increased by 51 and 41% compared to that of MOF-199. This improvement was attributed to the formation of more micropores and especially the increased number of unsaturated copper metal sites, as revealed by Py-IR. It is suggested the chemical reaction was apparent during adsorption of H2S, which resulted in the formation of CuS and the collapse of the MOF structure. Whereas reversible chemisorption was found for CH3SCH3 adsorption, as testified by TG-MS and fixed-bed regeneration. Exhausted MAC-2 can be almost totally regenerated by high temperature 180 °C nitrogen purge, indicating a promising adsorbent for CH3SCH3 removal.
Geographic identification of Boletus mushrooms by data fusion of FT-IR and UV spectroscopies combined with multivariate statistical analysis

NASA Astrophysics Data System (ADS)

Yao, Sen; Li, Tao; Li, JieQing; Liu, HongGao; Wang, YuanZhong

2018-06-01

Boletus griseus and Boletus edulis are two well-known wild-grown edible mushrooms which have high nutrition, delicious flavor and high economic value distributing in Yunnan Province. In this study, a rapid method using Fourier transform infrared (FT-IR) and ultraviolet (UV) spectroscopies coupled with data fusion was established for the discrimination of Boletus mushrooms from seven different geographical origins with pattern recognition method. Initially, the spectra of 332 mushroom samples obtained from the two spectroscopic techniques were analyzed individually and then the classification performance based on data fusion strategy was investigated. Meanwhile, the latent variables (LVs) of FT-IR and UV spectra were extracted by partial least square discriminant analysis (PLS-DA) and two datasets were concatenated into a new matrix for data fusion. Then, the fusion matrix was further analyzed by support vector machine (SVM). Compared with single spectroscopic technique, data fusion strategy can improve the classification performance effectively. In particular, the accuracy of correct classification of SVM model in training and test sets were 99.10% and 100.00%, respectively. The results demonstrated that data fusion of FT-IR and UV spectra can provide higher synergic effect for the discrimination of different geographical origins of Boletus mushrooms, which may be benefit for further authentication and quality assessment of edible mushrooms.
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.
Differentiation and identification of grape-associated black aspergilli using Fourier transform infrared (FT-IR) spectroscopic analysis of mycelia.

PubMed

Kogkaki, Efstathia A; Sofoulis, Manos; Natskoulis, Pantelis; Tarantilis, Petros A; Pappas, Christos S; Panagou, Efstathios Z

2017-10-16

The purpose of this study was to evaluate the potential of FT-IR spectroscopy as a high-throughput method for rapid differentiation among the ochratoxigenic species of Aspergillus carbonarius and the non-ochratoxigenic or low toxigenic species of Aspergillus niger aggregate, namely A. tubingensis and A. niger isolated previously from grapes of Greek vineyards. A total of 182 isolates of A. carbonarius, A. tubingensis, and A. niger were analyzed using FT-IR spectroscopy. The first derivative of specific spectral regions (3002-2801cm -1 , 1773-1550cm -1 , and 1286-952cm -1 ) were chosen and evaluated with respect to absorbance values. The average spectra of 130 fungal isolates were used for model calibration based on Discriminant analysis and the remaining 52 spectra were used for external model validation. This methodology was able to differentiate correctly 98.8% in total accuracy in both model calibration and validation. The per class accuracy for A. carbonarius was 95.3% and 100% for model calibration and validation, respectively, whereas for A. niger aggregate the per class accuracy amounted to 100% in both cases. The obtained results indicated that FT-IR could become a promising, fast, reliable and low-cost tool for the discrimination and differentiation of closely related fungal species. Copyright © 2017 Elsevier B.V. All rights reserved.
Geographic identification of Boletus mushrooms by data fusion of FT-IR and UV spectroscopies combined with multivariate statistical analysis.

PubMed

Yao, Sen; Li, Tao; Li, JieQing; Liu, HongGao; Wang, YuanZhong

2018-06-05

Boletus griseus and Boletus edulis are two well-known wild-grown edible mushrooms which have high nutrition, delicious flavor and high economic value distributing in Yunnan Province. In this study, a rapid method using Fourier transform infrared (FT-IR) and ultraviolet (UV) spectroscopies coupled with data fusion was established for the discrimination of Boletus mushrooms from seven different geographical origins with pattern recognition method. Initially, the spectra of 332 mushroom samples obtained from the two spectroscopic techniques were analyzed individually and then the classification performance based on data fusion strategy was investigated. Meanwhile, the latent variables (LVs) of FT-IR and UV spectra were extracted by partial least square discriminant analysis (PLS-DA) and two datasets were concatenated into a new matrix for data fusion. Then, the fusion matrix was further analyzed by support vector machine (SVM). Compared with single spectroscopic technique, data fusion strategy can improve the classification performance effectively. In particular, the accuracy of correct classification of SVM model in training and test sets were 99.10% and 100.00%, respectively. The results demonstrated that data fusion of FT-IR and UV spectra can provide higher synergic effect for the discrimination of different geographical origins of Boletus mushrooms, which may be benefit for further authentication and quality assessment of edible mushrooms. Copyright © 2018 Elsevier B.V. All rights reserved.
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.
Using FT-IR Spectroscopy to Elucidate the Structures of Ablative Polymers

NASA Technical Reports Server (NTRS)

Fan, Wendy

2011-01-01

The composition and structure of an ablative polymer has a multifaceted influence on its thermal, mechanical and ablative properties. Understanding the molecular level information is critical to the optimization of material performance because it helps to establish correlations with the macroscopic properties of the material, the so-called structure-property relationship. Moreover, accurate information of molecular structures is also essential to predict the thermal decomposition pathways as well as to identify decomposition species that are fundamentally important to modeling work. In this presentation, I will describe the use of infrared transmission spectroscopy (FT-IR) as a convenient tool to aid the discovery and development of thermal protection system materials.
Physical Identification of Binary System of Gliclazide-Hydrophilic Polymers Using X-Ray Diffraction

NASA Astrophysics Data System (ADS)

Rachmawati, H.; Yatinasari, Faizatun, Syarie, S. A.

2008-03-01

The formation of binary system in pharmaceutical solid state is aimed to improve the physicochemical characteristics of active compound, such as its solubility. To identify the physical change of the binary system including crystallinity or particle morphology, there are many methods can be applied. In present report, we study the physical interaction of the binary system of gliclazide and hydrophilic polymers. In this binary system, gliclazide was either dispersed or mixed with polyvinyl pirrolidone (PVP K30) or polyethylene glycol (PEG 6000). The dispersion system of gliclazide in the polymeric carriers was prepared by solvation-evaporation method, using dichloromethane/methylene chloride as an organic solvent. The physical characterization of both dispersed and mixed of gliclazide was studied using X-ray diffraction at interval 6-50 °/2θ. As a comparison, the same procedure was performed for pure gliclazide. To confirm the diffractogram of this binary system, Fourier Transform Infrared (FT-IR) spectroscopy was carried out as well. Both diffarctogram and FT-IR spectra revealed that there was no new compound formed in the solid dispersion system of gliclazide:PEG 6000 and gliclazide:PVP K30. In contrast, the solubility as well as the dissolution rate of gliclazide in the presence of both hydrophilic polymers was increased as compared to pure gliclazide. We conclude therefore that solvatation followed by evaporation of gliclazide in the presence of either PEG 6000 or PVP K30 did not alter its crystalline characteristic. The improved of gliclazide solubility in the binary system might due to other mechanism such as increased in the wettability and the hydrophylicity effect of the polymers.
Spinel NixZn1-xFe2O4 (0.0 ≤ x ≤ 1.0) nano-photocatalysts: Synthesis, characterization and photocatalytic degradation of methylene blue dye

NASA Astrophysics Data System (ADS)

Padmapriya, G.; Manikandan, A.; Krishnasamy, V.; Jaganathan, Saravana Kumar; Antony, S. Arul

2016-09-01

Spinel NixZn1-xFe2O4 (x = 0.0 to 1.0) nanoparticles were successfully synthesized by a simple microwave combustion method (MCM) using metal nitrates as raw materials and glycine as the fuel. The structural, morphological and opto-magnetic properties of the spinel NixZn1-xFe2O4 ferrites were determined by X-ray diffraction (XRD), Fourier transform infrared (FT-IR), high resolution scanning electron microscopy (HR-SEM), energy dispersive X-ray (EDX) spectroscopy, high resolution transmission electron microscopy (HR-TEM), selected area electron diffraction (SAED) pattern, UV-Visible diffuse reflectance spectroscopy (DRS), photoluminescence (PL) spectroscopy and vibrating sample magnetometer (VSM). Powder XRD, and EDX analysis was confirmed the formation of pure phase of spinel ferrites. HR-SEM and HR-TEM analysis was confirmed the formation of sphere like-particle morphology of the samples with smaller agglomeration. VSM analysis clearly showed the superparamagnetic and ferromagnetic nature of the samples. The Ms value is 3.851 emu/g for undoped ZnFe2O4 sample and it increased with increase in Ni content. Photo-catalytic degradation (PCD) of methylene blue (MB) dye using the samples were carried out and observed good PCD results.
Synthesis, characterization and solubility of a new anthelmintic salt: Mebendazole nitrate

NASA Astrophysics Data System (ADS)

Gutiérrez, Eduardo L.; Souza, Matheus S.; Diniz, Luan F.; Ellena, Javier

2018-06-01

Salt formation approach was taken to improve Mebendazole (MBZ) solubility. MBZ polymorph A was easily recrystallized as a 1:1 nitrate salt (MBZ N) in methanol. Single crystal X-ray diffraction data show that MBZ N crystallizes in the P 1 bar space group. By strong intermolecular H-bonding interactions, MBZ is associated with a nitrate anion forming a supramolecular R22(8) synthon. Crystal packing is stabilized by these H-bonds, through which each nitrate connects two molecules of MBZ forming chains along the b axis. The vibrational behavior studied by micro FT-Raman and FT-IR spectroscopy is consistent with the crystal structure. Thermal analysis of the salt indicates that the compound is stable up to 150 °C, when an almost simultaneous elimination of HNO3 and CO2 occurs. MBZ N equilibrium solubility was evaluated in hydrochloric acid 0.1 M solution and compared with those of MBZ A and C. An improvement in a factor of 5 and 1.22 was found respectively.
Synthesis of N-doped potassium tantalate perovskite material for environmental applications

NASA Astrophysics Data System (ADS)

Rao, Martha Purnachander; Nandhini, Vellangattupalayam Ponnusamy; Wu, Jerry J.; Syed, Asad; Ameen, Fuad; Anandan, Sambandam

2018-02-01

Nitrogen containing potassium tantalate perovskite material has been synthesized by the solvothermal method using urea (CH4N2O) as a nitrogen source. The as-prepared sample was characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), diffuse reflectance spectroscopy (DRS), scanning electron microscope (SEM), and energy-dispersive X-ray spectroscopy (EDX) and X-ray photoelectron spectroscopy (XPS). The particle size of nitrogen containing KTaO3 observed from SEM images was found to be 100-150 nm. Doping KTaO3 with nitrogen causes reduction of band gap from 3.5 to 2.54 eV. The incorporation of Nitrogen into the crystal lattice of KTaO3 not only extended the absorption of light from UV (ultraviolet) region to visible region and also enhanced the photocatalytic activity. As prepared nitrogen containing KTaO3 samples exhibit cubic-like morphology and noticed efficient photocatalytic activity towards methylene blue dye degradation under visible light illumination. The intermediates formed during photodegradation were identified by mass spectrometry (GC-MS) and proposed suitable degradation pathway.
The existence of imidazoline corrosion inhibitors

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

Martin, J.A.; Valone, F.W.

1985-05-01

Spectroscopic methods, i.e., Fourier transform infrared (FT-IR), carbon-13 nuclear magnetic reasonance (/sup 13/C NMR), and ultraviolet (UV) spectroscopy, were used to investigate the actual chemical composition of oilfield corrosion inhibitors. Inhibitor formulations consisting of an amide or imidazoline reacted with a dimer-trimer acid, along with an ethoxylated surfactant and an aromatic solvent, were used for these studies. /sup 13/C NMR and FT-IR spectra of these inhibitors, as well as spectra of pure imidazolines, showed that the imidazoline functional group was fairly rapidly hydrolyzed to the amide form. For instance, in FT-IR studies, the imine functional group decreased in intensity asmore » a function of time. Coincident with this was an increase in the intensities of the vibrational resonances attributed to the amide functionality. The relative molar ratio of imidazoline to amide in a corrosion inhibitor could be calculated via UV spectroscopy. Within a 20 day interval after inhibitor synthesis, this ratio decreased by a factor greater than 20. These results, as well as a discussion of their economic impact on oilfield corrosion inhibitor formulation, are presented in this paper.« less
Distinguishing ovarian maturity of farmed white sturgeon (Acipenser transmontanus) by Fourier transform infrared spectroscopy: a potential tool for caviar production management.

PubMed

Lu, Xiaonan; Webb, Molly; Talbott, Mariah; Van Eenennaam, Joel; Palumbo, Amanda; Linares-Casenave, Javier; Doroshov, Serge; Struffenegger, Peter; Rasco, Barbara

2010-04-14

Fourier transform infrared spectroscopy (FT-IR, 4000-400 cm(-1)) was applied to blood plasma of farmed white sturgeon (N = 40) to differentiate and predict the stages of ovarian maturity. Spectral features of sex steroids (approximately 3000 cm(-1)) and vitellogenin (approximately 1080 cm(-1)) were identified. Clear segregation of maturity stages (previtellogenesis, vitellogenesis, postvitellogenesis, and follicular atresia) was achieved using principal component analysis (PCA). Progression of oocyte development in the late phase of vitellogenesis was also monitored using PCA based on changes in plasma concentrations of sex steroid and lipid content. The observed oocyte polarization index (PI, a measure of nuclear migration) was correlated with changes in plasma sex steroid levels revealed by FT-IR PCA results. A partial least squares (PLS) model predicted PI values within the range 0.12-0.40 (R = 0.95, SEP = 2.18%) from differences in spectral features. These results suggest that FT-IR may be a good tool for assessing ovarian maturity in farmed sturgeon and will reduce the need for the invasive ovarian biopsy required for PI determination.
Volatility-dependent 2D IR correlation analysis of traditional Chinese medicine ‘Red Flower Oil’ preparation from different manufacturers

NASA Astrophysics Data System (ADS)

Wu, Yan-Wen; Sun, Su-Qin; Zhou, Qun; Tao, Jia-Xun; Noda, Isao

2008-06-01

As a traditional Chinese medicine (TCM), 'Red Flower Oil' preparation is widely used as a household remedy in China and Southeast Asia. Usually, the preparation is a mixture of several plant essential oils with different volatile features, such as wintergreen oil, turpentine oil and clove oil. The proportions of these plant essential oils in 'Red Flower Oil' vary from different manufacturers. Thus, it is important to develop a simple and rapid evaluation method for quality assurance of the preparations. Fourier transform infrared (FT-IR) was applied and two-dimensional correlation infrared spectroscopy (2D IR) based on the volatile characteristic of samples was used to enhance the resolution of FT-IR spectra. 2D IR technique could, not only easily provide the composition and their volatile sequences in 'Red flower Oil' preparations, but also rapidly discriminate the subtle differences in products from different manufacturers. Therefore, FT-IR combined with volatility-dependent 2D IR correlation analysis provides a very fast and effective method for the quality control of essential oil mixtures in TCM.
Imaging of lipids in atherosclerotic lesion in aorta from ApoE/LDLR-/- mice by FT-IR spectroscopy and Hierarchical Cluster Analysis.

PubMed

P Wrobel, Tomasz; Mateuszuk, Lukasz; Chlopicki, Stefan; Malek, Kamilla; Baranska, Malgorzata

2011-12-21

Spectroscopy-based approaches can provide an insight into the biochemical composition of a tissue sample. In the present work Fourier transform infrared (FT-IR) spectroscopy was used to develop a reliable methodology to study the content of free fatty acids, triglycerides, cholesteryl esters as well as cholesterol in aorta from mice with atherosclerosis (ApoE/LDLR(-/-) mice). In particular, distribution and concentration of palmitic, oleic and linoleic acid derivatives were analyzed. Spectral analysis of pure compounds allowed for clear discrimination between free fatty acids and other similar moieties based on the carbonyl band position (1699-1710 cm(-1) range). In order to distinguish cholesteryl esters from triglycerides a ratio of carbonyl band to signal at 1010 cm(-1) was used. Imaging of lipids in atherosclerotic aortic lesions in ApoE/LDLR(-/-) mice was followed by Hierarchical Cluster Analysis (HCA). The aorta from C57Bl/6J control mice (fed with chow diet) was used for comparison. The measurements were completed with an FT-IR spectrometer equipped with a 128 × 128 FPA detector. In cross-section of aorta from ApoE/LDLR(-/-) mice a region of atherosclerotic plaque was clearly identified by HCA, which was later divided into 2 sub-regions, one characterized by the higher content of cholesterol, while the other by higher contents of cholesteryl esters. HCA of tissues deposited on normal microscopic glass, hence limited to the 2200-3800 cm(-1) spectral range, also identified a region of atherosclerotic plaque. Importantly, this region correlates with the area stained by standard histological staining for atherosclerotic plaque (Oil Red O). In conclusion, the use of FT-IR and HCA may provide a novel tool for qualitative and quantitative analysis of contents and distribution of lipids in atherosclerotic plaque.

Application of spectroscopic techniques for the study of the surface changes in poplar wood and possible implications in conservation of wooden artefacts

NASA Astrophysics Data System (ADS)

Pelosi, C.; Agresti, G.; Calienno, L.; Lo Monaco, A.; Picchio, R.; Santamaria, U.; Vinciguerra, V.

2013-05-01

The aim of this work is to study the surface modifications of poplar (Populus spp.) wood by reflectance spectrophotometry and Fourier Transform Infrared (FT-IR) spectroscopy in order to understand the mechanisms that cause the changes and to suggest possible solutions to avoid the degradation phenomena. Since colour changes on wood surfaces are due to photo degradation of its chemical constituents, the study of the relationship between CIELAB colour changes and changes in chemical composition due to irradiation is of practical importance both in cultural heritage and in contemporary artefacts and objects. Concerning the surface protection of wood, starting from the results obtained by testing different commercial products, the attention has been focused on Linfoil®, a novel organic preservative/consolidant product that seems to attract a great interest in the field of conservation of wooden artefacts. Linfoil® was chosen and analysed in order to understand its composition and its time stability using reflectance spectrophotometry, FT-IR spectroscopy and analytical pyrolysis coupled to a gas chromatographic-mass spectrometric system. Colour monitoring allowed to find that wood surface colour undergoes an important variation due to photo-irradiation, occurring within the first 24 hours and mainly due to L* decrease and b* increase. Though Linfoil® treatment modifies wood colour, nevertheless it seems to protect wood surface by reducing the yellowish. FT-IR spectroscopy allowed to investigate the rate of photo-degradation of wood surface due to lignin oxidation. The most important result is that a correlation of the colour changes may be derived with the photo-degradation of lignin obtained by FT-IR analysis.
Evaluation of Polymerization Efficacy in Composite Resins via FT-IR Spectroscopy and Vickers Microhardness Test.

PubMed

Jafarzadeh, Tahereh-Sadat; Erfan, Mohammad; Behroozibakhsh, Marjan; Fatemi, Mostafa; Masaeli, Reza; Rezaei, Yashar; Bagheri, Hossein; Erfan, Yasaman

2015-01-01

Background and aims. Polymerization efficacy affects the properties and performance of composite resin restorations.The purpose of this study was to evaluate the effectiveness of polymerization of two micro-hybrid, two nano-hybrid and one nano-filled ormocer-based composite resins, cured by two different light-curing systems, using Fourier transformation infrared (FT-IR) spectroscopy and Vickers microhardness testing at two different depths (top surface, 2 mm). Materials and methods. For FT-IR spectrometry, five cylindrical specimens (5mm in diameter × 2 mm in length) were prepared from each composite resin using Teflon molds and polymerized for 20 seconds. Then, 70-μm wafers were sectioned at the top surface and at2mm from the top surface. The degree of conversion for each sample was calculated using FT-IR spectroscopy. For Vickers micro-hardness testing, three cylindrical specimens were prepared from each composite resin and polymerized for 20 seconds. The Vickers microhardness test (Shimadzu, Type M, Japan) was performed at the top and bottom (depth=2 mm) surfaces of each specimen. Three-way ANOVA with independent variables and Tukey tests were performed at 95% significance level. Results. No significant differences were detected in degree of conversion and microhardness between LED and QTH light-curing units except for the ormocer-based specimen, CeramX, which exhibited significantly higher DC by LED. All the composite resins showed a significantly higher degree of conversion at the surface. Microhardness was not significantly affected by depth, except for Herculite XRV Ultra and CeramX, which showed higher values at the surface. Conclusion. Composite resins containing nano-particles generally exhibited more variations in degree of conversion and microhardness.
Evaluation of Polymerization Efficacy in Composite Resins via FT-IR Spectroscopy and Vickers Microhardness Test

PubMed Central

Jafarzadeh, Tahereh-Sadat; Erfan, Mohammad; Behroozibakhsh, Marjan; Fatemi, Mostafa; Masaeli, Reza; Rezaei, Yashar; Bagheri, Hossein; Erfan, Yasaman

2015-01-01

Background and aims. Polymerization efficacy affects the properties and performance of composite resin restorations.The purpose of this study was to evaluate the effectiveness of polymerization of two micro-hybrid, two nano-hybrid and one nano-filled ormocer-based composite resins, cured by two different light-curing systems, using Fourier transformation infrared (FT-IR) spectroscopy and Vickers microhardness testing at two different depths (top surface, 2 mm). Materials and methods. For FT-IR spectrometry, five cylindrical specimens (5mm in diameter × 2 mm in length) were prepared from each composite resin using Teflon molds and polymerized for 20 seconds. Then, 70-μm wafers were sectioned at the top surface and at2mm from the top surface. The degree of conversion for each sample was calculated using FT-IR spectroscopy. For Vickers micro-hardness testing, three cylindrical specimens were prepared from each composite resin and polymerized for 20 seconds. The Vickers microhardness test (Shimadzu, Type M, Japan) was performed at the top and bottom (depth=2 mm) surfaces of each specimen. Three-way ANOVA with independent variables and Tukey tests were performed at 95% significance level. Results. No significant differences were detected in degree of conversion and microhardness between LED and QTH light-curing units except for the ormocer-based specimen, CeramX, which exhibited significantly higher DC by LED. All the composite resins showed a significantly higher degree of conversion at the surface. Microhardness was not significantly affected by depth, except for Herculite XRV Ultra and CeramX, which showed higher values at the surface. Conclusion. Composite resins containing nano-particles generally exhibited more variations in degree of conversion and microhardness. PMID:26889359
In Vivo Fiber-Optic Raman Mapping Of Metastases In Mouse Brains

NASA Astrophysics Data System (ADS)

Stelling, A.; Kirsch, M.; Steiner, G.; Krafft, C.; Schackert, G.; Salzer, R.

2010-08-01

Vibrational spectroscopy, in particular Raman spectroscopy, has potential applications in the field of in vivo diagnostics. Raman and FT-IR spectroscopy analyze the complete biochemical information at any given pixel within the visual field. Here we demonstrate the feasibility of performing Raman spectroscopic measurements on living mice brains using a fiber-optic probe with a nominal spatial resolution of 60 μm. The objectives of this study were to 1) evaluate preclinical models, namely murine brain slices containing experimental tumors, 2) optimize the preparation of pristine brain tissue to obtain reference information, to 3) optimize the conditions for introducing a fiber-optic probe to acquire Raman maps in vivo, and 4) to transfer results obtained from human brain tumors to an animal model. Disseminated brain metastases of malignant melanomas were induced by injecting tumor cells into the carotid artery of mice. The procedure mimicked hematogenous tumor spread in one brain hemisphere while the other hemisphere remained tumor free. Three series of sections were prepared consecutively from whole mouse brains: pristine, 2-mm thick sections for Raman mapping and dried, thin sections for FT-IR imaging, hematoxylin and eosin-stained thin sections for histopathological assessment. Raman maps were collected serially using a spectrometer coupled to a fiber-optic probe. FT-IR images were recorded using a spectrometer with a multi-channel detector. The FT-IR images and the Raman maps were evaluated by multivariate data analysis. The results obtained from the thin section studies were employed to guide measurements of murine brains in vivo. Raman maps with an acquisition time of over an hour could be performed on the living animals. No damage to the tissue was observed.
Microstructures as IR-sensors with Staphylococcus aureus bacteria

NASA Astrophysics Data System (ADS)

Baikova, T. V.; Danilov, P. A.; Gonchukov, S. A.; Yermachenko, V. M.; Ionin, A. A.; Khmelnitskii, R. A.; Kudryashov, S. I.; Nguyen, T. T. H.; Rudenko, A. A.; Saraeva, I. N.; Svistunova, T. S.; Zayarny, D. A.

2017-09-01

Using a micro-hole grating in a supported silver film as a laser-fabricated novel optical platform for surface-enhanced IR absoprtion/reflection spectroscopy, characteristic absorption bands of Staphylococcus aureus, especially - its buried carotenoid fragments - were detected in FT-IR spectra with 10-fold analytical enhancement, paving the way to spectral express-identification of the pathogenic microorganisms.
Preparation and characterization of bee venom-loaded PLGA particles for sustained release.

PubMed

Park, Min-Ho; Jun, Hye-Suk; Jeon, Jong-Woon; Park, Jin-Kyu; Lee, Bong-Joo; Suh, Guk-Hyun; Park, Jeong-Sook; Cho, Cheong-Weon

2016-12-14

Bee venom-loaded poly(lactic-co-glycolic acid) (PLGA) particles were prepared by double emulsion-solvent evaporation, and characterized for a sustained-release system. Factors such as the type of organic solvent, the amount of bee venom and PLGA, the type of PLGA, the type of polyvinyl alcohol, and the emulsification method were considered. Physicochemical properties, including the encapsulation efficiency, drug loading, particle size, zeta-potential and surface morphology were examined by Fourier transform infrared (FT-IR) spectroscopy, differential scanning calorimetry (DSC), and X-ray diffraction (XRD). The size of the bee venom-loaded PLGA particles was 500 nm (measured using sonication). Zeta-potentials of the bee venom-loaded PLGA particles were negative owing to the PLGA. FT-IR results demonstrated that the bee venom was completely encapsulated in the PLGA particles, indicated by the disappearance of the amine and amide peaks. In addition, sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE) analysis indicated that the bee venom in the bee venom-loaded PLGA particles was intact. In vitro release of the bee venom from the bee venom-loaded PLGA particles showed a sustained-release profile over 1 month. Bee venom-loaded PLGA particles can help improve patients' quality of life by reducing the number of injections required.
Preparation and characterization of adefovir dipivoxil-stearic acid cocrystal with enhanced physicochemical properties.

PubMed

Seo, Jeong-Woong; Hwang, Kyu-Min; Lee, Sung-Hoon; Kim, Dong-Wook; Park, Eun-Seok

2017-06-11

The objectives of this study were to prepare cocrystal composed of adefovir dipivoxil (AD) and stearic acid (SA) and to investigate the enhanced properties of the cocrystal. The cocrystal was prepared by antisolvent precipitation and characterized by scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR), X-ray powder diffraction (XRPD), and differential scanning calorimetry (DSC). The enhanced properties were evaluated by dissolution testing, permeability studies, and powder rheology analysis. The AD raw material has a cuboid-like crystal and the cocrystal has a needle shape. In the FT-IR study, there were bathochromic shifts caused by the hydrogen bonding. The melting point of the cocrystal was 52.9 °C, which was lower than that of AD. The XRPD pattern also had distinct differences, supporting the formation of a new crystalline form. The cocrystal showed changes in the lattice energy and the solvation strength, which caused an enhanced dissolution. The permeability was increased due to the SA, which acts as a P-gp inhibitor. The tabletability was enhanced due to the altered crystal habit. In conclusion, cocrystal containing AD and SA was successfully prepared, presenting advantages such as enhanced solubility, tabletability, and permeability. The use of the cocrystal is a desirable approach for the improved physicochemical properties.
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.
Cyanide bridged hetero-metallic polymeric complexes: Syntheses, vibrational spectra, thermal analyses and crystal structures of complexes [M(1,2-dmi)2Ni(μ-CN)4]n (M = Zn(II) and Cd(II))

NASA Astrophysics Data System (ADS)

Kürkçüoğlu, Güneş Süheyla; Sayın, Elvan; Şahin, Onur

2015-12-01

Two cyanide bridged hetero-metallic complexes of general formula, [M(1,2-dmi)2Ni(μ-CN)4]n (1,2-dmi = 1,2-dimethylimidazole and M = Zn(II) or Cd(II)) have been synthesized and characterized by vibrational (FT-IR and Raman) spectroscopy, single crystal X-ray diffraction, thermal analyses and elemental analyses. The crystallographic analyses reveal that the complexes, [Zn(1,2-dmi)2Ni(μ-CN)4] (1) and [Cd(1,2-dmi)2Ni(μ-CN)4] (2), have polymeric 2D networks. In the complexes, four cyanide groups of [Ni(CN)4]2- coordinated to the adjacent M(II) ions and distorted octahedral geometries of complexes are completed by two nitrogen atoms of trans 1,2-dmi ligands. The structures of 1 and 2 are similar and linked via intermolecular hydrogen bonding, C-H⋯Ni interactions to give rise to 3D networks. Vibration assignments are given for all the observed bands and the spectral features also supported to the crystal structures of heteronuclear complexes. The FT-IR and Raman spectra of the complexes are very much consistent with the structural data presented.
Enhancement of solubility and antidiabetic effects of Repaglinide using spray drying technique in STZ-induced diabetic rats.

PubMed

Varshosaz, Jaleh; Minayian, Mohsen; Ahmadi, Mahdieh; Ghassami, Erfaneh

2017-09-01

The purpose of the study was to enhance the solubility of the poorly water-soluble drug, Repaglinide using spray drying based solid dispersion technique by different carriers including Eudragit E100, hydroxyl propyl cellulose Mw 80 000 and poly vinyl pyrollidone K30. Optimization of the best formulation was carried out according to drug solubility, release profile, particle size and angle of repose of the solid dispersions. The optimized sample was characterized using X-ray powder diffraction (XRPD), differential scanning calorimetry (DSC) and Fourier transform infrared spectroscopy (FT-IR). The morphology of the dispersions was studied by SEM. The blood glucose lowering effect of spray dried solid dispersions was studied in normal and streptozocin-induced diabetic rats. The results showed that Eudragit E100 in 1:3 ratio could enhance drug solubility by 100-fold. DSC studies indicated a marked change in melting point of the drug possibly due to strong hydrogen bonds between the drug and Eudragit, while FT-IR study did not show obvious interactions between them. According to XRPD results Repaglinide converted to an amorphous state in the spray dried dispersions. Spray dried Repaglinide reduced the blood glucose level significantly during the 8 h of obtaining blood samples in comparison with untreated drug (p < 0.05).
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
Detection of metanil yellow contamination in turmeric using FT-Raman and FT-IR spectroscopy

USDA-ARS?s Scientific Manuscript database

Turmeric is well known for its medicinal value and is often used in Asian cuisine. Economically motivated contamination of turmeric by chemicals such as metanil yellow has been repeatedly reported. Although traditional technologies can detect such contaminants in food, high operational costs and ope...
Determination of residual solvents and investigation of their effect on ampicillin trihydrate crystal structure.

PubMed

Nojavan, Saeed; Ghassempour, Alireza; Bashour, Yosef; Darbandi, Masoud Khalilian; Ahmadi, Seyyed Hamid

2005-01-04

In the present work, the relationship between residual solvents concentration and ampicillin trihydrate crystals stability has been investigated. The amounts of residual solvents determined by GC, X-ray powder diffraction (XRPD) and Fourier transform infrared spectroscopy (FT-IR) were used for characterization of solid state. The obtained results have shown good relationship between concentration of methylene chloride (as a critical residue solvent) and degree of ampicillin trihydrate crystallinity. As with the increasing methylene chloride concentration in the sample the degree of crystallinity decreased after stability test. From this relationship, critical concentration of methylene chloride into the ampicillin trihydrate is obtained and the results can be used for improving the large-scale production of ampicillin trihydrate.
Photodegradation of methyl red under visible light by mesoporous carbon nitride

NASA Astrophysics Data System (ADS)

Hu, Yueyue; Zhang, Min; Xiao, Zaozao; Jiang, Tao; Yan, Bing; Li, Jian

2018-02-01

Mesoporous carbon nitride (mpg-C3N4) with tunable microstructure has been successfully prepared through a simple polymerization reaction of cyanamide by a nano hard-templating approach. The obtained materials have been characterized using X-ray diffraction (XRD), N2 adsorption, and Fourier transform infrared (FT-IR) spectroscopy. The results show that the pore diameter of the mpg-C3N4 materials can be easily tuned from 3.8 to 10.5 nm. The mpg-C3N4 materials are demonstrated to exhibit much higher visible light photocatalytic activity than that of g-C3N4 for the degradation of aqueous methyl red (MR). The high surface areas and large pore volume contributed to the efficient visible light photocatalytic activity.
Nanocrystalline hydroxyapatite doped with selenium oxyanions: a new material for potential biomedical applications.

PubMed

Kolmas, Joanna; Oledzka, Ewa; Sobczak, Marcin; Nałęcz-Jawecki, Grzegorz

2014-06-01

Selenium-substituted hydroxyapatites containing selenate SeO4(2-) or selenite SeO3(2-) ions were synthesized using a wet precipitation method. The selenium content was determined by atomic absorbance spectrometry. The raw, unsintered powders were also characterized using powder X-ray diffraction, middle-range FT-IR spectroscopy and transmission electron microscopy with energy-dispersive X-ray spectroscopic microanalysis. The synthesized apatites were found to be pure and nanocrystalline with a crystal size similar to that in bone mineral. The incorporation of selenium oxyanions into the crystal lattice was confirmed. The toxicity of hydroxyapatites containing selenite or selenate ions was evaluated with a protozoan assay and bacterial luminescence test. Copyright © 2014 Elsevier B.V. All rights reserved.
A novel ultrasonication method in the preparation of zirconium impregnated cellulose for effective fluoride adsorption.

PubMed

Barathi, M; Kumar, A Santhana Krishna; Rajesh, N

2014-05-01

In the present work, we propose for the first time a novel ultrasound assisted methodology involving the impregnation of zirconium in a cellulose matrix. Fluoride from aqueous solution interacts with the cellulose hydroxyl groups and the cationic zirconium hydroxide. Ultrasonication ensures a green and quick alternative to the conventional time intensive method of preparation. The effectiveness of this process was confirmed by comprehensive characterization of zirconium impregnated cellulose (ZrIC) adsorbent using Fourier transform infrared spectroscopy (FT-IR), energy dispersive X-ray spectrometry (EDX) and X-ray diffraction (XRD) studies. The study of various adsorption isotherm models, kinetics and thermodynamics of the interaction validated the method. Copyright © 2013 Elsevier B.V. All rights reserved.
Effect of supramolecular structures on thermoplastic zein-lignin bionanocomposites.

PubMed

Oliviero, Maria; Verdolotti, Letizia; Di Maio, Ernesto; Aurilia, Marco; Iannace, Salvatore

2011-09-28

The effect of alkaline lignin (AL) and sodium lignosulfonate (LSS) on the structure of thermoplastic zein (TPZ) was studied. Protein structural changes and the nature of the physical interaction between lignin and zein were investigated by means of X-ray diffraction and Fourier transform infrared (FT-IR) spectroscopy and correlated with physical properties. Most relevant protein structural changes were observed at low AL concentration, where strong H-bondings between the functional groups of AL and the amino acids in zein induced a destructuring of inter- and intramolecular interactions in α-helix, β-sheet, and β-turn secondary structures. This destructuring allowed for an extensive protein conformational modification which, in turn, resulted in a strong improvement of the physical properties of the bionanocomposite.
In situ surface treatment of nanocrystalline MFe2O4 (M = Co, Mg, Mn, Ni) spinel ferrites using linseed oil

NASA Astrophysics Data System (ADS)

Gherca, Daniel; Cornei, Nicoleta; Mentré, Olivier; Kabbour, Houria; Daviero-Minaud, Sylvie; Pui, Aurel

2013-12-01

This paper reports the synthesis by coprecipitation method of MFe2O4 nanoparticles using linseed oil as the in-situ surfactant. The decomposition process of the precursors and the formation process of MFe2O4 were investigated by thermogravimetric analysis and differential thermal analysis (TG-DTA). The crystal structure and surface morphology were examined by means of X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR) and scanning electron microscopy (SEM) analysis. The results demonstrate that the surface of MFe2O4 with a diameter in the range 5-13 nm, is activated with hydrophilic groups of the surfactant which coat them and enhance the stability. Magnetic properties are discussed.
Differentiation of Body Fluid Stains on Fabrics Using External Reflection Fourier Transform Infrared Spectroscopy (FT-IR) and Chemometrics.

PubMed

Zapata, Félix; de la Ossa, Ma Ángeles Fernández; García-Ruiz, Carmen

2016-04-01

Body fluids are evidence of great forensic interest due to the DNA extracted from them, which allows genetic identification of people. This study focuses on the discrimination among semen, vaginal fluid, and urine stains (main fluids in sexual crimes) placed on different colored cotton fabrics by external reflection Fourier transform infrared spectroscopy (FT-IR) combined with chemometrics. Semen-vaginal fluid mixtures and potential false positive substances commonly found in daily life such as soaps, milk, juices, and lotions were also studied. Results demonstrated that the IR spectral signature obtained for each body fluid allowed its identification and the correct classification of unknown stains by means of principal component analysis (PCA) and soft independent modeling of class analogy (SIMCA). Interestingly, results proved that these IR spectra did not show any bands due to the color of the fabric and no substance of those present in daily life which were analyzed, provided a false positive. © The Author(s) 2016.
Facile preparation and characterization of pH sensitive Mt/CMC nanocomposite hydrogel beads for propranolol controlled release.

PubMed

Farhadnejad, Hassan; Mortazavi, Seyed Alireza; Erfan, Mohammad; Darbasizadeh, Behzad; Motasadizadeh, Hamidreza; Fatahi, Yousef

2018-05-01

The main aim of the present study was to design pH-sensitive nanocomposite hydrogel beads, based on carboxymethyl cellulose (CMC) and montmorillonite (Mt)-propranolol (PPN) nanohybrid, and evaluate whether the prepared nanocomposite beads could potentially be used as oral drug delivery systems. PPN-as a model drug-was intercalated into the interlayer space of Mt clay mineral via the ion exchange procedure. The resultant nanohybrid (Mt-PPN) was applied to fabricate nanocomposite hydrogel beads by association with carboxymethyl cellulose. The characterization of test samples was performed using different techniques: X-Ray Diffraction (XRD), IR spectroscopy (FT-IR), thermal gravity analysis (TGA), and scanning electron microscopy (SEM). The drug encapsulation efficiency was evaluated by UV-vis spectroscopy, and was found to be high for Mt/CMC beads. In vitro drug release test was performed in the simulated gastrointestinal conditions to evaluate the efficiency of Mt-PPN/CMC nanocomposite beads as a controlled-release drug carrier. The drug release profiles indicated that the Mt-PPN/CMC nanocomposite beads had high stability against stomach acid and a sustained- and controlled-release profile for PPN under the simulated intestinal conditions. Copyright © 2018 Elsevier B.V. All rights reserved.

Single-source-precursor synthesis of dense SiC/HfCxN1-x-based ultrahigh-temperature ceramic nanocomposites

NASA Astrophysics Data System (ADS)

Wen, Qingbo; Xu, Yeping; Xu, Binbin; Fasel, Claudia; Guillon, Olivier; Buntkowsky, Gerd; Yu, Zhaoju; Riedel, Ralf; Ionescu, Emanuel

2014-10-01

A novel single-source precursor was synthesized by the reaction of an allyl hydrido polycarbosilane (SMP10) and tetrakis(dimethylamido)hafnium(iv) (TDMAH) for the purpose of preparing dense monolithic SiC/HfCxN1-x-based ultrahigh temperature ceramic nanocomposites. The materials obtained at different stages of the synthesis process were characterized via Fourier transform infrared (FT-IR) as well as nuclear magnetic resonance (NMR) spectroscopy. The polymer-to-ceramic transformation was investigated by means of MAS NMR and FT-IR spectroscopy as well as thermogravimetric analysis (TGA) coupled with in situ mass spectrometry. Moreover, the microstructural evolution of the synthesized SiHfCN-based ceramics annealed at different temperatures ranging from 1300 °C to 1800 °C was characterized by elemental analysis, X-ray diffraction, Raman spectroscopy and transmission electron microscopy (TEM). Based on its high temperature behavior, the amorphous SiHfCN-based ceramic powder was used to prepare monolithic SiC/HfCxN1-x-based nanocomposites using the spark plasma sintering (SPS) technique. The results showed that dense monolithic SiC/HfCxN1-x-based nanocomposites with low open porosity (0.74 vol%) can be prepared successfully from single-source precursors. The average grain size of both HfC0.83N0.17 and SiC phases was found to be less than 100 nm after SPS processing owing to a unique microstructure: HfC0.83N0.17 grains were embedded homogeneously in a β-SiC matrix and encapsulated by in situ formed carbon layers which acted as a diffusion barrier to suppress grain growth. The segregated Hf-carbonitride grains significantly influenced the electrical conductivity of the SPS processed monolithic samples. While Hf-free polymer-derived SiC showed an electrical conductivity of ca. 1.8 S cm-1, the electrical conductivity of the Hf-containing material was analyzed to be ca. 136.2 S cm-1.A novel single-source precursor was synthesized by the reaction of an allyl hydrido polycarbosilane (SMP10) and tetrakis(dimethylamido)hafnium(iv) (TDMAH) for the purpose of preparing dense monolithic SiC/HfCxN1-x-based ultrahigh temperature ceramic nanocomposites. The materials obtained at different stages of the synthesis process were characterized via Fourier transform infrared (FT-IR) as well as nuclear magnetic resonance (NMR) spectroscopy. The polymer-to-ceramic transformation was investigated by means of MAS NMR and FT-IR spectroscopy as well as thermogravimetric analysis (TGA) coupled with in situ mass spectrometry. Moreover, the microstructural evolution of the synthesized SiHfCN-based ceramics annealed at different temperatures ranging from 1300 °C to 1800 °C was characterized by elemental analysis, X-ray diffraction, Raman spectroscopy and transmission electron microscopy (TEM). Based on its high temperature behavior, the amorphous SiHfCN-based ceramic powder was used to prepare monolithic SiC/HfCxN1-x-based nanocomposites using the spark plasma sintering (SPS) technique. The results showed that dense monolithic SiC/HfCxN1-x-based nanocomposites with low open porosity (0.74 vol%) can be prepared successfully from single-source precursors. The average grain size of both HfC0.83N0.17 and SiC phases was found to be less than 100 nm after SPS processing owing to a unique microstructure: HfC0.83N0.17 grains were embedded homogeneously in a β-SiC matrix and encapsulated by in situ formed carbon layers which acted as a diffusion barrier to suppress grain growth. The segregated Hf-carbonitride grains significantly influenced the electrical conductivity of the SPS processed monolithic samples. While Hf-free polymer-derived SiC showed an electrical conductivity of ca. 1.8 S cm-1, the electrical conductivity of the Hf-containing material was analyzed to be ca. 136.2 S cm-1. Electronic supplementary information (ESI) available: Raman spectroscopy characterization of the SiHfCN-based ceramics. See DOI: 10.1039/c4nr03376k
Detection of creatinine enriched on a surface imprinted polystyrene film using FT-ATR-IR.

PubMed

Sreenivasan, K

2006-01-01

The surface of polystyrene (PS) was chemically modified by coating a thin layer of polyaniline (PANI) by oxidizing aniline using ammonium persulfate. Affinity sites for creatinine, a clinically relevant molecule, were created in the coated layer by adding creatinine as print molecules during the oxidation. The imprinted layer adsorbed creatinine was compared to non-imprinted surface reflecting the creation of creatinine-specific sites on the surface. The equilibrium was attained rapidly, indicating that a material of this kind is suitable for sensing applications. The adsorbed creatinine on the surface was detected using the technique of Fourier transform attenuated total internal reflection infra red spectroscopy (FT-ATR-IR). The results show that molecularly imprinted surface can enrich molecules of interest and the enriched molecules can be detected using FT-IR.
Fourier Transform Infrared Spectroscopy Part III. Applications.

ERIC Educational Resources Information Center

Perkins, W. D.

1987-01-01

Discusses the use of the FT-IR spectrometer in analyses that were previously avoided. Examines some of the applications of this spectroscopy with aqueous solutions, circular internal reflection, samples with low transmission, diffuse reflectance, infrared emission, and the infrared microscope. (TW)
The characterization of hydroxypropyl methylcellulose through the analysis of its substituents

USDA-ARS?s Scientific Manuscript database

The methyl and hydroxypropyl substituents in hydroxypropyl methylcellulose (HPMC) affect the resulting gel properties. These substituents in five HPMC gels were characterized using Fourier transform infrared spectroscopy (FT-IR), Raman spectroscopy, small-amplitude oscillatory shear measurements, a...
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
Technical note: Characterization of lipid constitution in Fourier transform infrared spectra and spectroscopic discrimination of animal-derived feedstuffs from different species.

PubMed

Gao, F; Han, L; Yang, Z; Xu, L; Liu, X

2017-06-01

The objective of the current work was to assess the capability of Fourier transform infrared (FT-IR) spectroscopy in combination with chemometric methods to discriminate animal-derived feedstuffs from different origins based on the lipid characteristics. A total of 82 lipid samples extracted from animal-derived feedstuffs, comprising porcine, poultry, bovine, ovine, and fish samples, were investigated by gas chromatography and FT-IR. The relationship between the lipid constitutions and the responding FT-IR spectral characteristics were explored. Results indicated that high correlations ( > 0.900) were found between the contents of MUFA and PUFA and FT-IR spectral data. In addition, the peak intensity at about 1,116 and 1,098 cm-1 showed a significant difference ( < 0.05) between ruminant and nonruminant animals; the change of peak ratio (1,116:1,098) was proved consistent with the degree of unsaturation of lipid from different animal species. Successful discrimination was further achieved among porcine, poultry, bovine, and ovine meat and bone meal (MBM) and fishmeal based on lipid characteristics by applying the FT-IR spectra coupled with chemometrics, for which the values of sensitivity and specificity were close to 1 and classification error were almost equal to 0.
Rapid discrimination of sea buckthorn berries from different H. rhamnoides subspecies by multi-step IR spectroscopy coupled with multivariate data analysis

NASA Astrophysics Data System (ADS)

Liu, Yue; Zhang, Ying; Zhang, Jing; Fan, Gang; Tu, Ya; Sun, Suqin; Shen, Xudong; Li, Qingzhu; Zhang, Yi

2018-03-01

As an important ethnic medicine, sea buckthorn was widely used to prevent and treat various diseases due to its nutritional and medicinal properties. According to the Chinese Pharmacopoeia, sea buckthorn was originated from H. rhamnoides, which includes five subspecies distributed in China. Confusion and misidentification usually occurred due to their similar morphology, especially in dried and powdered forms. Additionally, these five subspecies have vital differences in quality and physiological efficacy. This paper focused on the quick classification and identification method of sea buckthorn berry powders from five H. rhamnoides subspecies using multi-step IR spectroscopy coupled with multivariate data analysis. The holistic chemical compositions revealed by the FT-IR spectra demonstrated that flavonoids, fatty acids and sugars were the main chemical components. Further, the differences in FT-IR spectra regarding their peaks, positions and intensities were used to identify H. rhamnoides subspecies samples. The discrimination was achieved using principal component analysis (PCA) and partial least square-discriminant analysis (PLS-DA). The results showed that the combination of multi-step IR spectroscopy and chemometric analysis offered a simple, fast and reliable method for the classification and identification of the sea buckthorn berry powders from different H. rhamnoides subspecies.
A photochemical proposal for the preparation of ZnAl{sub 2}O{sub 4} and MgAl{sub 2}O{sub 4} thin films from β-diketonate complex precursors

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

Cabello, G., E-mail: gerardocabelloguzman@hotmail.com; Lillo, L.; Caro, C.

2016-05-15

Highlights: • ZnAl{sub 2}O{sub 4} and MgAl{sub 2}O{sub 4} thin films were prepared by photo-chemical method. • The Zn(II), Mg(II) and Al(III) β-diketonate complexes were used as precursors. • The photochemical reaction was monitored by UV–vis and FT-IR spectroscopy. • The results reveal spinel oxide formation and the generation of intermediate products. - Abstract: ZnAl{sub 2}O{sub 4} and MgAl{sub 2}O{sub 4} thin films were grown on Si(100) and quartz plate substrates using a photochemical method in the solid phase with thin films of β-diketonate complexes as the precursors. The films were deposited by spin-coating and subsequently photolyzed at room temperaturemore » using 254 nm UV light. The photolysis of these films results in the deposition of metal oxide thin films and fragmentation of the ligands from the coordination sphere of the complexes. The obtained samples were post-annealed at different temperatures (350–1100 °C) for 2 h and characterized by FT-Infrared spectroscopy, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), atomic force miscroscopy (AFM), and UV–vis spectroscopy. The results indicate the formation of spinel-type structures and other phases. These characteristics determined the quality of the films, which were obtained from the photodeposition of ternary metal oxides.« less
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.
Synthesis, characterization and application of iron (II, III) oxide (Fe3O4) magnetic nanoparticles in mimic of wound healing model

NASA Astrophysics Data System (ADS)

Konyala, Divya

The research study focused on synthesis, characterization and applications of Fe3O4 core-shelled magnetic nanomaterials. This Fe3O4 magnetic nanomaterials will be prepared by using cost effective and convenient wet-chemistry method and will encapsulated using aqueous extracts of medicinal natural products. Three natural products namely Symplocos racemosa, Picrorhiza kurroa and Butea monosperma used to encapsulate Fe3O 4 MNMs due to their scope to reduce the risk of cancer, improves health, increase energy and enhance the immunity. These three medicinal natural products are synthesize by using water as a solvents to derive its active constituents, which will further used to functionalize the magnetic nanomaterials. The magnetic nanoparticles characterization studies performed using X-ray powder diffraction, Scanning electron microscope, Transmission electron microscope, Ultraviolet-visible spectroscopy, Fourier Transform Infrared spectroscopy (FT-IR) and Magnetic property. Fe3O4 magnetic nanomaterials biological activity was tested on Gram-negative bacteria (Escherichia coli). The results pointed out that, due to the adequate coating of Fe 3O4 (Iron Oxide) core by the medicinal chemical constituents from the natural products, the absorption of Fe3O4 magnetic nanomaterials was not detected in the UV-VIS Spectroscopy. TEM images showed that Fe3O4 coated with natural product extract in core-shelled structure, and the size of the particle ranges from 6 nm to 10 nm. Fourier Transform Infrared spectroscopy (FT-IR) was performed to determine the nature of chemicals present in natural extracts and functionalized Fe3O 4 magnetic nanomaterials. The model of wound healing mimic and antibacterial activity performed on gram-negative (Escherichia coli), indicating steady increasing cell growth after adding Fe3O4 MNMs. It was also found that MNMs synthesized at high temperatures shows less wound healing activity, when compared to MNMs prepared at room temperature due to formation of clusters at high temperatures.
Thermal decomposition of ammonium perchlorate in the presence of Al(OH)(3)·Cr(OH)(3) nanoparticles.

PubMed

Zhang, WenJing; Li, Ping; Xu, HongBin; Sun, Randi; Qing, Penghui; Zhang, Yi

2014-03-15

An Al(OH)(3)·Cr(OH)(3) nanoparticle preparation procedure and its catalytic effect and mechanism on thermal decomposition of ammonium perchlorate (AP) were investigated using transmission electron microscopy (TEM), X-ray diffraction (XRD), thermogravimetric analysis and differential scanning calorimetry (TG-DSC), X-ray photoelectron spectroscopy (XPS), and thermogravimetric analysis and mass spectroscopy (TG-MS). In the preparation procedure, TEM, SAED, and FT-IR showed that the Al(OH)(3)·Cr(OH)(3) particles were amorphous particles with dimensions in the nanometer size regime containing a large amount of surface hydroxyl under the controllable preparation conditions. When the Al(OH)(3)·Cr(OH)(3) nanoparticles were used as additives for the thermal decomposition of AP, the TG-DSC results showed that the addition of Al(OH)(3)·Cr(OH)(3) nanoparticles to AP remarkably decreased the onset temperature of AP decomposition from approximately 450°C to 245°C. The FT-IR, RS and XPS results confirmed that the surface hydroxyl content of the Al(OH)(3)·Cr(OH)(3) nanoparticles decreased from 67.94% to 63.65%, and Al(OH)3·Cr(OH)3 nanoparticles were limitedly transformed from amorphous to crystalline after used as additives for the thermal decomposition of AP. Such behavior of Al(OH)(3)·Cr(OH)(3) nanoparticles promoted the oxidation of NH3 of AP to decompose to N2O first, as indicated by the TG-MS results, accelerating the AP thermal decomposition. Copyright © 2014 Elsevier B.V. All rights reserved.
Synthesis of silver nanoparticles from stem bark of Cochlospermum religiosum (L.) Alston: an important medicinal plant and evaluation of their antimicrobial efficacy

NASA Astrophysics Data System (ADS)

Sasikala, A.; Linga Rao, M.; Savithramma, N.; Prasad, T. N. V. K. V.

2015-10-01

The use of different parts of plants for the synthesis of nanoparticles is considered as a green technology as it does not involve any harmful chemicals. Herein, we report on rapid biosynthesis of silver nanoparticles (SNPs) from aqueous stem bark extract of Cochlospermum religiosum a medicinal plant. The reduced silver nanoparticles were characterized by using UV-Visible spectroscopy (UV-Vis), X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray analysis, atomic force microscopy, and Fourier transform infrared (FT-IR). The UV-Visible spectrum of the aqueous medium containing silver nanoparticles showed an absorption peak at around 445 nm, XRD showed that the particles are crystalline in nature, with a face-centered cubic structure and the SEM images showed that the spherical-shaped silver nanoparticles were observed and the size range was found to be 20-35 nm. FT-IR spectroscopy analysis revealed that carbohydrate, polyphenols, and protein molecules were involved in the synthesis and capping of silver nanoparticles. These phytosynthesized SNPs were tested for their antimicrobial activity and it analyzed by measuring the inhibitory zone. Cochlospermum religiosum aqueous stem bark extract of SNPs showed highest toxicity to Staphylococcus followed by Pseudomonas, Escherichia coli and Bacillus and lowest toxicity towards Proteus. Whereas in fungal species highest inhibition zone against Aspergillus flavus followed by Rhizopus, Fusarium, and Curvularia, and minimum inhibition zone was observed against Aspergillus niger species. The outcome of this study could be useful for the development of value added products from indigenous medicinal plants of India for nanotechnology-based biomedical applications.
Preparation and characterization of highly water-soluble magnetic Fe3O4 nanoparticles via surface double-layered self-assembly method of sodium alpha-olefin sulfonate

NASA Astrophysics Data System (ADS)

Li, Honghong; Qin, Li; Feng, Ying; Hu, Lihua; Zhou, Chunhua

2015-06-01

A kind of double-layered self-assembly sodium alpha-olefin sulfonate (AOS) capped Fe3O4 magnetic nanoparticles (Fe3O4-AOS-MN) with highly water-solubility was prepared by a wet co-precipitation method with a pH of 4.8. The resulting Fe3O4-AOS-MN could be dispersed into water to form stable magnetic fluid without other treatments. The result of X-ray diffraction (XRD) indicated that the Fe3O4-AOS-MN maintained original crystalline structure and exhibited a diameter of about 7.5 nm. The iron oxide phase of nanoparticles determined by Raman spectroscopy is Fe3O4. Transmission electron microscopy (TEM) analysis confirmed that the Fe3O4-AOS-MN with spherical morphology were uniformly dispersed in water. FT-IR spectroscopy (FT-IR) and thermo-gravimetric analysis (TGA) verified the successful preparation of Fe3O4-AOS-MN capped with double-layered self-assembled AOS. The corresponding capacities of monolayer chemical absorption and the second-layer self-assembly absorption were respectively 4.07 and 14.71 wt% of Fe3O4-MN, which were much lower than those of other surfactants. Vibrating sample magnetometer (VSM) test result showed Fe3O4-AOS-MN possessed superparamagnetic behavior with the saturation magnetization value of about 44.45 emu/g. The blocking temperature TB of Fe3O4-AOS-MN capped with double-layered AOS is 170 K.
Antimicrobial and anticancer activities of porous chitosan-alginate biosynthesized silver nanoparticles.

PubMed

Venkatesan, Jayachandran; Lee, Jin-Young; Kang, Dong Seop; Anil, Sukumaran; Kim, Se-Kwon; Shim, Min Suk; Kim, Dong Gyu

2017-05-01

The main aim of this study was to obtain porous antimicrobial composites consisting of chitosan, alginate, and biosynthesized silver nanoparticles (AgNPs). Chitosan and alginate were used owing to their pore-forming capacity, while AgNPs were used for their antimicrobial property. The developed porous composites of chitosan-alginate-AgNPs were characterized using Fourier transform infrared spectroscopy (FT-IR), ultraviolet-visible spectroscopy, X-ray diffraction (XRD) analysis, and scanning electron microscopy (SEM). The FT-IR results revealed the presence of a strong chemical interaction between chitosan and alginate due to polyelectrolyte complex; whereas, the XRD results confirmed the presence of AgNPs in the composites. The dispersion of AgNPs in the porous membrane was uniform with a pore size of 50-500μm. Antimicrobial activity of the composites was checked with Escherichia coli and Staphylococcus aureus. The developed composites resulted in the formation of a zone of inhibition of 11±1mm for the Escherichia coli, and 10±1mm for Staphylococcus aureus. The bacterial filtration efficiency of chitosan-alginate-AgNPs was 1.5-times higher than that of the chitosan-alginate composite. The breast cancer cell line MDA-MB-231 was used to test the anticancer activity of the composites. The IC 50 value of chitosan-alginate-AgNPs on MDA-MB-231 was 4.6mg. The developed chitosan-alginate-AgNPs composite showed a huge potential for its applications in antimicrobial filtration and cancer treatment. Copyright © 2017 Elsevier B.V. All rights reserved.
Synthesis, dielectric, conductivity and magnetic studies of LiNi1/3Co1/3Mn(1/3)-xAlxO2 (x = 0.0, 0.02, 0.04 and 0.06) for cathode materials of lithium-ion batteries

NASA Astrophysics Data System (ADS)

Murali, N.; Margarette, S. J.; Veeraiah, V.

Layered structure cathode materials LiNi1/3Co1/3Mn(1/3)-xAlxO2 (x = 0.0, 0.02, 0.04 and 0.06) are prepared by the sol-gel method by adding citric acid as chelating agent. The physical, electrical and magnetic properties of the synthesized materials are systematically discussed using the structural (XRD, FESEM with EDS and FT-IR), impedance (LCR) and electron spin resonance (ESR) measurements. The X-ray diffraction pattern of the synthesized samples possessed the α-NaFeO2 structure of the space group, R 3 bar m , with no evidence of any impurities. The peak intensity ratio I(104)/I(003) increased with Al concentration, which indicated the cation mixing between transition metal layer and lithium layer. The field effect scanning electron microscopy showed the particle size distribution in the range of 230-250 nm and EDS has been analysed for elemental mapping. The local structure is investigated by vibrational spectroscopy in FT-IR study. The impedance studies are characterized by complex impedance spectroscopy (CIS) in the frequency range from 42 Hz to 1 MHz at room temperature (30 °C). The dielectric properties are analyzed in the framework of complex dielectric permittivity and formalism of the complex electric modulus. For these samples, the ESR analysis of magnetic measurements, the degree of cation mixing, is estimated to be Ni2+(3b) = 2.75%.
Rapid identification of Pterocarpus santalinus and Dalbergia louvelii by FTIR and 2D correlation IR spectroscopy

NASA Astrophysics Data System (ADS)

Zhang, Fang-Da; Xu, Chang-Hua; Li, Ming-Yu; Huang, An-Min; Sun, Su-Qin

2014-07-01

Since Pterocarpus santalinus and Dalbergia louvelii, which are of precious Rosewood, are very similar in their appearance and anatomy characteristics, cheaper Hongmu D. louvelii is often illegally used to impersonate valuable P. santalinus, especially in Chinese furniture manufacture. In order to develop a rapid and effective method for easy confused wood furniture differentiation, we applied tri-step identification method, i.e., conventional infrared spectroscopy (FT-IR), second derivative infrared (SD-IR) spectroscopy and two-dimensional correlation infrared (2DCOS-IR) spectroscopy to investigate P. santalinus and D. louvelii furniture. According to FT-IR and SD-IR spectra, it has been found two unconditional stable difference at 848 cm-1 and 700 cm-1 and relative stable differences at 1735 cm-1, 1623 cm-1, 1614 cm-1, 1602 cm-1, 1509 cm-1, 1456 cm-1, 1200 cm-1, 1158 cm-1, 1055 cm-1, 1034 cm-1 and 895 cm-1 between D. louvelii and P. santalinus IR spectra. The stable discrepancy indicates that the category of extractives is different between the two species. Besides, the relative stable differences imply that the content of holocellulose in P. santalinus is more than that of D. louvelii, whereas the quantity of extractives in D. louvelii is higher. Furthermore, evident differences have been observed in their 2DCOS-IR spectra of 1550-1415 cm-1 and 1325-1030 cm-1. P. santalinus has two strong auto-peaks at 1459 cm-1 and 1467 cm-1, three mid-strong auto-peaks at 1518 cm-1, 1089 cm-1 and 1100 cm-1 and five weak auto-peaks at 1432 cm-1, 1437 cm-1, 1046 cm-1, 1056 cm-1 and 1307 cm-1 while D. louvelii has four strong auto-peaks at 1465 cm-1, 1523 cm-1, 1084 cm-1 and 1100 cm-1, four mid-strong auto-peaks at 1430 cm-1, 1499 cm-1, 1505 cm-1 and 1056 cm-1 and two auto-peaks at 1540 cm-1 and 1284 cm-1. This study has proved that FT-IR integrated with 2DCOS-IR could be applicable for precious wood furniture authentication in a direct, rapid and holistic manner.
Anionic 11-mercaptoundecanoic acid capped ZnO nanoparticles

NASA Astrophysics Data System (ADS)

Šimšíková, Michaela; Antalík, Marián; Kaňuchová, Mária; Škvarla, Jiří

2013-10-01

The anionic zinc oxide nanoparticles have been prepared at room temperature by a precipitation method using ZnCl2 and NaOH and surface modification with 11-mercaptoundecanoic acid (MUA). Atomic force microscopy (AFM) was used for definition of morphology and size of prepared nanoparticles which was proved by measurements of particle size distribution using Zetasizer. Successful coating with MUA as surfactant was acknowledged by X-ray photoelectron spectroscopy and ATR FT-IR spectroscopy. The isoelectric point (IEP) of ZnO-MUA nanoparticles was obtained by measurements of zeta potential and FT-IR dependence on pH; the obtained value was approximately 3.58. The value of exchanged protons was 2.88 which indicates a positive binding cooperativity of modified nanoparticles.
Atmospheric-Pressure Plasma Interaction with Soft Materials as Fundamental Processes in Plasma Medicine.

PubMed

Takenaka, Kosuke; Miyazaki, Atsushi; Uchida, Giichiro; Setsuhara, Yuichi

2015-03-01

Molecular-structure variation of organic materials irradiated with atmospheric pressure He plasma jet have been investigated. Optical emission spectrum in the atmospheric-pressure He plasma jet has been measured. The spectrum shows considerable emissions of He lines, and the emission of O and N radicals attributed to air. Variation in molecular structure of Polyethylene terephthalate (PET) film surface irradiated with the atmospheric-pressure He plasma jet has been observed via X-ray photoelectron spectroscopy (XPS) and Fourier transform infrared spectroscopy (FT-IR). These results via XPS and FT-IR indicate that the PET surface irradiated with the atmospheric-pressure He plasma jet was oxidized by chemical and/or physical effect due to irradiation of active species.
Multiple functionalization of multi-walled carbon nanotubes with carboxyl and amino groups

NASA Astrophysics Data System (ADS)

Zhao, Zhiyuan; Yang, Zhanhong; Hu, Youwang; Li, Jianping; Fan, Xinming

2013-07-01

In this paper, carboxyl and amino groups have been introduced onto the surface of the multi-walled carbon nanotubes (MWCNTs) by the mixed acid treatment and the diazonium reaction, respectively. The presence of multifunctionality groups on the MWCNTs has been characterized by Fourier transform infrared (FT-IR) spectroscopy, thermogravimetric (TGA) analysis, Raman spectra, scanning electron microscopy (SEM) and energy dispersive X-ray spectrum (EDS). The multifunctionalized carbon nanotubes were further utilized to react with acetyl chloride and ethylenediamine (EDA). The formation of the amide bond in the grafting reaction has been confirmed by FT-IR spectroscopy. The result indicates that the further grafting is successful. The multifunctionalized MWCNTs can be a new versatile platform for many interesting applications.
High throughput operando studies using Fourier transform infrared imaging and Raman spectroscopy.

PubMed

Li, Guosheng; Hu, Dehong; Xia, Guanguang; White, J M; Zhang, Conrad

2008-07-01

A prototype high throughput operando (HTO) reactor designed and built for catalyst screening and characterization combines Fourier transform infrared (FT-IR) imaging and Raman spectroscopy in operando conditions. Using a focal plane array detector (HgCdTe focal plane array, 128x128 pixels, and 1610 Hz frame rate) for the FT-IR imaging system, the catalyst activity and selectivity of all parallel reaction channels can be simultaneously followed. Each image data set possesses 16 384 IR spectra with a spectral range of 800-4000 cm(-1) and with an 8 cm(-1) resolution. Depending on the signal-to-noise ratio, 2-20 s are needed to generate a full image of all reaction channels for a data set. Results on reactant conversion and product selectivity are obtained from FT-IR spectral analysis. Six novel Raman probes, one for each reaction channel, were specially designed and house built at Pacific Northwest National Laboratory, to simultaneously collect Raman spectra of the catalysts and possible reaction intermediates on the catalyst surface under operando conditions. As a model system, methanol partial oxidation reaction on silica-supported molybdenum oxide (MoO3SiO2) catalysts has been studied under different reaction conditions to demonstrate the performance of the HTO reactor.

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 Â© 2016 Elsevier B.V. All rights reserved.
The use of FT-IR reflection-absorbance spectroscopy to study photochemical degradation of polymeric coatings on mirrors

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

Webb, J.D.; Chughtai, A.R.; Czanderna, A.W.

1981-10-01

A technique is presented for in situ study of degradative changes in polymeric coatings on metallic substrates. The technique uses a controlled environment chamber in conjunction with a Fourier-transform infrared (FT-IR) spectrophotometer. The chamber design permits collection of IR reflection-absorbance spectra from a sample undergoing exposure to controlled ultraviolet (UV) radiation, gas mixtures, and temperatures. Initial data presented confirm the ability of the technique to provide information regarding the bulk photochemistry of bisphenol-A polycarbonate coatings on gold and aluminum substrates. Refinements of this technique should allow a detailed kinetic study of degradative reactions at the polymer/metal interface.
Use of FT-IR reflection-absorbance spectroscopy to study photochemical degradation of polymeric coatings on mirrors

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

Webb, J D; Schissel, P; Czanderna, A W

1981-01-01

A technique is presented for in situ study of degradative changes in polymeric coatings on metallic substrates. The technique uses a controlled environment chamber in conjunction with a Fourier-transform infrared (FT-IR) spectrophotometer. The chamber design permits collection of IR reflection-absorbance spectra from a sample undergoing exposure to controlled ultraviolet (uv) radiation, gas mixtures, and temperatures. Initial data presented confirm the ability of the technique to provide information regarding the bulk photochemistry of bisphenol-A polycarbonate coatings on gold and aluminum substrates. Refinements of this technique should allow a detailed kinetic study of degradative reactions at the polymer/metal interface.
Two-dimensional correlation infrared spectroscopy applied to analyzing and identifying the extracts of Baeckea frutescens medicinal materials.

PubMed

Adib, Adiana Mohamed; Jamaludin, Fadzureena; Kiong, Ling Sui; Hashim, Nuziah; Abdullah, Zunoliza

2014-08-05

Baeckea frutescens or locally known as Cucur atap is used as antibacterial, antidysentery, antipyretic and diuretic agent. In Malaysia and Indonesia, they are used as an ingredient of the traditional medicine given to mothers during confinement. A three-steps infra-red (IR) macro-fingerprinting method combining conventional IR spectra, and the secondary derivative spectra with two dimensional infrared correlation spectroscopy (2D-IR) have been proved to be effective methods to examine a complicated mixture such as herbal medicines. This study investigated the feasibility of employing multi-steps IR spectroscopy in order to study the main constituents of B. frutescens and its different extracts (extracted by chloroform, ethyl acetate, methanol and aqueous in turn). The findings indicated that FT-IR and 2D-IR can provide many holistic variation rules of chemical constituents. The structural information of the samples indicated that B. frutescens and its extracts contain a large amount of flavonoids, since some characteristic absorption peaks of flavonoids, such as ∼1600cm(-1), ∼1500cm(-1), ∼1450cm(-1), and ∼1270cm(-1) can be observed. The macroscopical fingerprint characters of FT-IR and 2D-IR spectra can not only provide the information of main chemical constituents in medicinal materials and their different extracts, but also compare the components differences among the similar samples. In conclusion, the multi-steps IR macro-fingerprint method is rapid, effective, visual and accurate for pharmaceutical research. Copyright © 2014 Elsevier B.V. All rights reserved.
Supramolecular complexes of Co(II), Ni(II) and Zn(II) p-hydroxybenzoates with caffeine: Synthesis, spectral characterization and crystal structure

NASA Astrophysics Data System (ADS)

Taşdemir, Erdal; Özbek, Füreya Elif; Sertçelik, Mustafa; Hökelek, Tuncer; Çelik, Raziye Çatak; Necefoğlu, Hacali

2016-09-01

Three novel complexes Co(II), Ni(II) and Zn(II) containing p-hydroxybenzoates and caffeine ligands were synthesized and characterized by elemental analysis, FT-IR and UV-vis Spectroscopy, molar conductivity and single crystal X-ray diffraction methods. The thermal properties of the synthesized complexes were investigated by TGA/DTA. The general formula of the complexes is [M(HOC6H4COO)2(H2O)4]·2(C8H10N4O2)·8H2O (where: M: Co, Ni and Zn). The IR studies showed that carboxylate groups of p-hydroxybenzoate ligands have monodentate coordination mode. The M2+ ions are octahedrally coordinated by two p-hydroxybenzoate ligands, four water molecules leading to an overall MO6 coordination environment. The medium-strength hydrogen bondings involving the uncoordinated caffeine ligands and water molecules, coordinated and uncoordinated water molecules and p-hydroxybenzoate ligands lead to three-dimensional supramolecular networks in the crystal structures.
The functionalization and characterization of multi-walled carbon nanotubes (MWCNTs)

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

Abdullah, Mohd Pauzi; Center of Water Analysis and Research; Zulkepli, Siti Aminah

2015-09-25

Functionalization is the process of introducing chemical functional groups on the surface of the material. In this study, a multi-walled carbon nanotube (MWCNTs) was functionalized by oxidation treatment using concentrated nitric acid. The functionalized and pristine MWCNTs were analyzed by using Fourier Transform Infrared Spectroscopy (FT-IR) and X-Ray Diffraction (XRD). The XRD patterns exhibit the graphitic properties for all samples. Besides, the XRD results also demonstrate that the percent of crystallinity of MWCNTs increases as the duration of acid treatment increases. The percent of crystallinity increases from 66% to 80% when the pristine MWCNT treated for 12 hours with additionalmore » 12 hours reflux process with nitric acid. The IR spectrum for the 12 hours-treated MWCNTs shows the formation of carboxyl functional group. Additional 12 hours reflux process with nitric acid on the 12 hours-treated MWCNTs have shown the loss of existing carboxyl group and only hydroxyl group formed.« less
Validation of ATR FT-IR to identify polymers of plastic marine debris, including those ingested by marine organisms

USGS Publications Warehouse

Jung, Melissa R.; Horgen, F. David; Orski, Sara V.; Rodriguez, Viviana; Beers, Kathryn L.; Balazs, George H.; Jones, T. Todd; Work, Thierry M.; Brignac, Kayla C.; Royer, Sarah-Jeanne; Hyrenbach, David K.; Jensen, Brenda A.; Lynch, Jennifer M.

2018-01-01

Polymer identification of plastic marine debris can help identify its sources, degradation, and fate. We optimized and validated a fast, simple, and accessible technique, attenuated total reflectance Fourier transform infrared spectroscopy (ATR FT-IR), to identify polymers contained in plastic ingested by sea turtles. Spectra of consumer good items with known resin identification codes #1–6 and several #7 plastics were compared to standard and raw manufactured polymers. High temperature size exclusion chromatography measurements confirmed ATR FT-IR could differentiate these polymers. High-density (HDPE) and low-density polyethylene (LDPE) discrimination is challenging but a clear step-by-step guide is provided that identified 78% of ingested PE samples. The optimal cleaning methods consisted of wiping ingested pieces with water or cutting. Of 828 ingested plastics pieces from 50 Pacific sea turtles, 96% were identified by ATR FT-IR as HDPE, LDPE, unknown PE, polypropylene (PP), PE and PP mixtures, polystyrene, polyvinyl chloride, and nylon.
Biochemical Monitoring of Spinal Cord Injury by FT-IR Spectroscopy—Effects of Therapeutic Alginate Implant in Rat Models

PubMed Central

Uckermann, Ortrud; Sitoci-Ficici, Kerim H.; Later, Robert; Beiermeister, Rudolf; Doberenz, Falko; Gelinsky, Michael; Leipnitz, Elke; Schackert, Gabriele; Koch, Edmund; Sablinskas, Valdas; Steiner, Gerald; Kirsch, Matthias

2015-01-01

Spinal cord injury (SCI) induces complex biochemical changes, which result in inhibition of nervous tissue regeneration abilities. In this study, Fourier-transform infrared (FT-IR) spectroscopy was applied to assess the outcomes of implants made of a novel type of non-functionalized soft calcium alginate hydrogel in a rat model of spinal cord hemisection (n = 28). Using FT-IR spectroscopic imaging, we evaluated the stability of the implants and the effects on morphology and biochemistry of the injured tissue one and six months after injury. A semi-quantitative evaluation of the distribution of lipids and collagen showed that alginate significantly reduced injury-induced demyelination of the contralateral white matter and fibrotic scarring in the chronic state after SCI. The spectral information enabled to detect and localize the alginate hydrogel at the lesion site and proved its long-term persistence in vivo. These findings demonstrate a positive impact of alginate hydrogel on recovery after SCI and prove FT-IR spectroscopic imaging as alternative method to evaluate and optimize future SCI repair strategies. PMID:26559822
Analysis of fingerprints features of infrared spectra of various processed products of Rhizoma Coptidis and their different extracts

NASA Astrophysics Data System (ADS)

Xu, Beilei; Zhang, Guijun; Xu, Changhua; Sun, Suqin

2015-09-01

Fourier transform infrared spectroscopy (FT-IR) associated with second derivative infrared spectroscopy (SD-IR) and two-dimensional correlation infrared spectroscopy (2D-IR) are employed to analyze various processed products and different extracts of Rhizoma Coptidis. There is a shift of the peak of 1641 cm-1 of raw Rhizoma Coptidis after processed, which drifts to lower wave number. Peaks at 1508, 1387, 1363, 1332, 1274 and 1234 cm-1 barely change in most samples, except an obvious enhancement of these peaks after processed, suggesting that processed Rhizoma Coptidis may have higher content of berberine than raw material, which is corresponding to the results of correlation coefficients analysis. There are some differences in the absorption peaks in the range of 1800-1000 cm-1 in the SD-IR spectra, which have better resolution, of different processed products. 2D-IR spectra, which elevate the resolution further, can present more differences among the products in the range of 1300-800 cm-1 and 1800-1300 cm-1. Analysis of aqueous, ethanol and petroleum ether extracts of various processed products proves that there are distinctive differences of all auto-peaks in shapes and intensities in all of them. With the advantages of high resolution, high speed and convenience, FT-IR combined with 2D-IR can quickly and precisely distinguish various processed products of Rhizoma Coptidis and can be applied to predict the tendency of transformation of the complicated chemical mixture systems under heat perturbation.
Evaluation of turmeric powder adulterated with metanil yellow using FT-Raman and FT-IR spectroscopy

USDA-ARS?s Scientific Manuscript database

Turmeric powder (Curcuma longa L.) is valued both for its medicinal properties and for its popular culinary use such as being a component in curry powder. Due to its high demand in international trade, turmeric powder has been subject to economically driven, hazardous chemical adulteration. This stu...
Generation of drugs coated iron nanoparticles through high energy ball milling

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

Radhika Devi, A.; Murty, B. S.; Chelvane, J. A.

The iron nanoparticles coated with oleic acid and drugs such as folic acid/Amoxicillin were synthesized by high energy ball milling and characterized by X-ray diffraction, Transmission electron microscope, zeta potential, dynamic light scattering, Fourier Transform Infra red (FT-IR) measurements, and thermo gravimetric analysis (TGA). FT-IR and TGA measurements show good adsorption of drugs on oleic acid coated nanoparticles. Magnetic measurements indicate that saturation magnetization is larger for amoxicillin coated particles compared to folic acid coated particles. The biocompatibility of the magnetic nanoparticles prepared was evaluated by in vitro cytotoxicity assay using L929 cells as model cells.
Molecular and crystal structure of 2-{( E)-[(4-Methylphenyl)imino]methyl}-4-nitrophenol: A redetermination

NASA Astrophysics Data System (ADS)

Kaynar, Nihal Kan; Tanak, Hasan; Şahin, Songul; Dege, Necmi; Ağar, Erbil; Yavuz, Metin

2016-03-01

The crystal structure of the title compound, C14H12N2O3, was recently determined as a mixture of its neutral (OH containing) and zwitterionic (NH containing) forms, in a 0.60 (4): 0.40 (4) ratio using the X-ray determination. In this study, the title compound has been characterized by FT-IR and X-ray diffraction. The redetermination showed that the title compound has only enol (OH) form because of lack of the NH stretching vibration in FT-IR spectrum. In addition, the molecular structure and tautomerism of the title compound have been discussed.
Molecular and crystal structure of 2-((E)-[(4-Methylphenyl)imino]methyl)-4-nitrophenol: A redetermination

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

Kaynar, Nihal Kan, E-mail: nihal-kan84@windowslive.com; Tanak, Hasan; Şahin, Songul

The crystal structure of the title compound, C{sub 14}H{sub 12}N{sub 2}O{sub 3}, was recently determined as a mixture of its neutral (OH containing) and zwitterionic (NH containing) forms, in a 0.60 (4): 0.40 (4) ratio using the X-ray determination. In this study, the title compound has been characterized by FT-IR and X-ray diffraction. The redetermination showed that the title compound has only enol (OH) form because of lack of the NH stretching vibration in FT-IR spectrum. In addition, the molecular structure and tautomerism of the title compound have been discussed.
Molecular geometry and vibrational studies of 3,5-diamino-1,2,4-triazole using quantum chemical calculations and FT-IR and FT-Raman spectroscopies

NASA Astrophysics Data System (ADS)

Guennoun, L.; El jastimi, J.; Guédira, F.; Marakchi, K.; Kabbaj, O. K.; El Hajji, A.; Zaydoun, S.

2011-01-01

The 3,5-diamino-1,2,4-triazole (guanazole) was investigated by vibrational spectroscopy and quantum methods. The solid phase FT-IR and FT-Raman spectra were recorded in the region 4000-400 cm -1 and 3600-50 cm -1 respectively, and the band assignments were supported by deuteration effects. The results of energy calculations have shown that the most stable form is 1H-3,5-diamino-1,2,4-triazole under C 1 symmetry. For this form, the molecular structure, harmonic vibrational wave numbers, infrared intensities and Raman activities were calculated by the ab initio/HF and DFT/B3LYP methods using 6-31G* basis set. The calculated geometrical parameters of the guanazole molecule using B3LYP methodology are in good agreement with the previously reported X-ray data, and the scaled vibrational wave number values are in good agreement with the experimental data. The normal vibrations were characterized in terms of potential energy distribution (PEDs) using VEDA 4 program.
Acid-base properties, FT-IR, FT-Raman spectroscopy and computational study of 1-(pyrid-4-yl)piperazine.

PubMed

Mary, Y Sheena; Panicker, C Yohannan; Varghese, Hema Tresa; Van Alsenoy, Christian; Procházková, Markéta; Sevčík, Richard; Pazdera, Pavel

2014-01-01

We report the vibrational spectral analysis was carried out using FT-IR and FT-Raman spectroscopy for 1-(pyrid-4-yl)piperazine (PyPi). Single crystals of PyPi suitable for X-ray structural analysis were obtained. The acid-base properties are also reported. PyPi supported on a weak acid cation-exchanger in the single protonated form and this system can be used efficiently as the solid supported analogue of 4-N,N-dimethyl-aminopyridine. The complete vibrational assignments of wavenumbers were made on the basis of potential energy distribution. The HOMO and LUMO analysis is used to determine the charge transfer within the molecule and with the molecular electrostatic potential map was applied for the reactivity assessment of PyPi molecule toward proton, electrophiles and nucleopholes as well. The stability of the molecule arising from hyper-conjugative interaction and charge delocalization has been analyzed using NBO analysis. The calculated first hyperpolarizability of PyPi is 17.46 times that of urea. Copyright © 2013 Elsevier B.V. All rights reserved.
Characterization of sodium phenytoin co-gelled with titania for a controlled drug-release system

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

Lopez, T.; Instituto Nacional de Neurologia y Neurocirugia 'MVS', Av. Insurgentes Sur 3877. Col. La Fama. P.O. Box 14269 Mexico D. F.; Quintana, P.

2007-08-15

Sodium phenytoin, C{sub 15}H{sub 11}N{sub 2}NaO{sub 2}, in several concentrations was co-gelled with titania (TiO{sub 2}), by a sol-gel process. This technique is a promising method to encapsulate several drugs, in this case, phenytoin is an anticonvulsant used to control epileptic seizures. Samples were prepared by adding different concentrations (X = 50, 100, 200 and 250 mg per 20 g of titania matrix) of sodium phenytoin (Ph) to a solution of titanium n-butoxide. The resulting titania-Ph-X materials were characterized by transmission electron microscopy (TEM), Fourier transformed infrared (FT-IR) spectroscopy, X-ray diffraction (XRD), and Brunauer-Emmet-Teller (BET) surface areas. The porous nanomaterialsmore » showed a wide range of particle size, from 10 to 210 nm, with a mean pore diameter of 5 nm. X-ray diffraction showed an amorphous structure of the prepared samples.« less
Sulfaguanidine cocrystals: Synthesis, structural characterization and their antibacterial and hemolytic analysis.

PubMed

Abidi, Syed Sibte Asghar; Azim, Yasser; Khan, Shahper Nazeer; Khan, Asad U

2018-02-05

Sulfaguanidine (SG), belongs to the class of sulfonamide drug used as an effective antibiotic. In the present work, using crystal engineering approach two novel cocrystals of SG were synthesized (SG-TBA and SG-PT) with thiobarbutaric acid (TBA) and 1,10-phenanthroline (PT), characterized by solid state techniques viz., powder X-ray diffraction (PXRD), fourier transform infrared spectroscopy (FT-IR), differential scanning calorimetry (DSC) and the crystal structures were determined by single crystal X-ray diffraction studies. A comparative antibacterial activity and hemolytic potential was done on SG drug, coformers and their cocrystals. The tested cocrystals formulations showed almost two fold higher antibacterial activity against the tested strains of bacteria Gram-positive bacteria (S. mutans and E. faecalis) and Gram-negative bacteria (E. coli, K. pneumonia and E. clocae) over SG alone and their coformers. Cocrystal SG-TBA showed better antibacterial activity and reduced hemolysis, thereby, reduced cytotoxicity than SG-PT. Copyright © 2017 Elsevier B.V. All rights reserved.
Hirshfeld surface analyses and crystal structures of supramolecular self-assembly thiourea derivatives directed by non-covalent interactions

NASA Astrophysics Data System (ADS)

Gumus, Ilkay; Solmaz, Ummuhan; Binzet, Gun; Keskin, Ebru; Arslan, Birdal; Arslan, Hakan

2018-04-01

The novel N-(bis(3,5-dimethoxybenzyl)carbamothioyl)-4-R-benzamide (R: H, Cl, CH3 and OCH3) compounds have been synthesized and characterized by FT-IR, 1H NMR and 13C NMR spectroscopy. Their crystal structures were also determined by single-crystal X-ray diffraction studies. Hirshfeld surfaces analysis and their associated two dimensional fingerprint plots of compounds were used as theoretical approach to assess driving force for crystal structure formation via the intermolecular interactions in the crystal lattices of synthesized compounds. The study of X-ray single crystal diffraction and Hirshfeld surfaces analysis of the prepared compounds shows that hydrogen bonding and other weaker interactions such as Nsbnd H⋯S, weak Csbnd H⋯S, Csbnd H⋯O, Csbnd H⋯N and Csbnd H···π intermolecular interactions and π-π stacking, among molecules of synthesized compounds participate in a cooperative way to stabilize the supramolecular structures.
Synthesis and spectral studies on Cd(II) dithiocarbamate complexes and their use as precursors for CdS nanoparticles

NASA Astrophysics Data System (ADS)

Sathiyaraj, Ethiraj; Padmavathy, Krishnaraj; Kumar, Chandran Udhaya; Krishnan, Kannan Gokula; Ramalingan, Chennan

2017-11-01

Bis(N-cyclopropyl-N-4-chlorobenzyldithiocarbamato-S,S‧)cadmium(II) (1) and (2,2‧-bipyridine) bis(N-cyclopropyl-N-4-chlorobenzyldithiocarbamato-S,S‧)cadmium(II) (2) have been synthesized and characterized by FT-IR, 1HNMR and 13C NMR analyses. For the complex 2, single crystal X-ray diffraction analysis and computational studies (optimized geometry, HOMO-LUMO and MEP) have been executed employing DFT/B3LYP method with LANL 2DZ basic set. The optimized bond lengths and bond angles agree well with the experimental results. The complexes 1 and 2 have been used as single source precursors for the synthesis of ethyleneglycol capped CdS1 and CdS2 nanoparticles, respectively. CdS1 and CdS2 nanoparticles have been synthesized by solvothermal method. PXRD, SEM, Elemental colour mapping, EDAX, TEM and UV-Vis spectroscopy have been used to characterize the as-prepared CdS nanoparticles. The X-ray diffraction pattern confirms both their hexagonal structures.
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.

High-Throughput Metabolic Fingerprinting of Legume Silage Fermentations via Fourier Transform Infrared Spectroscopy and Chemometrics

PubMed Central

Johnson, Helen E.; Broadhurst, David; Kell, Douglas B.; Theodorou, Michael K.; Merry, Roger J.; Griffith, Gareth W.

2004-01-01

Silage quality is typically assessed by the measurement of several individual parameters, including pH, lactic acid, acetic acid, bacterial numbers, and protein content. The objective of this study was to use a holistic metabolic fingerprinting approach, combining a high-throughput microtiter plate-based fermentation system with Fourier transform infrared (FT-IR) spectroscopy, to obtain a snapshot of the sample metabolome (typically low-molecular-weight compounds) at a given time. The aim was to study the dynamics of red clover or grass silage fermentations in response to various inoculants incorporating lactic acid bacteria (LAB). The hyperspectral multivariate datasets generated by FT-IR spectroscopy are difficult to interpret visually, so chemometrics methods were used to deconvolute the data. Two-phase principal component-discriminant function analysis allowed discrimination between herbage types and different LAB inoculants and modeling of fermentation dynamics over time. Further analysis of FT-IR spectra by the use of genetic algorithms to identify the underlying biochemical differences between treatments revealed that the amide I and amide II regions (wavenumbers of 1,550 to 1,750 cm−1) of the spectra were most frequently selected (reflecting changes in proteins and free amino acids) in comparisons between control and inoculant-treated fermentations. This corresponds to the known importance of rapid fermentation for the efficient conservation of forage proteins. PMID:15006782
Speciation And Distribution Of Arsenic In Fresh Water Pond Sediments Impacted By Contaminated Ground-Water Discharge

EPA Science Inventory

The speciation and mineralogy of sediments contaminated with arsenic due to arsenic enriched groundwater discharging into the pond at the Ft. Devens Super Fund Site in Ft. Devens, MA were determined using X-ray absorption fine structure and X-ray diffraction spectroscopy. Specia...
Field Evaluation Of Arsenic Speciation In Sediments At The Ground Water/Surface Water Interface

EPA Science Inventory

The speciation and mineralogy of sediments contaminated with arsenic at the ground water/surface water interface of the Ft. Devens Super Fund Site in Ft. Devens, MA were determined using X-ray absorption fine structure and X-ray diffraction spectroscopy. Speciation and mineralog...
Synthesis, X-ray diffraction method, spectroscopic characterization (FT-IR, 1H and 13C NMR), antimicrobial activity, Hirshfeld surface analysis and DFT computations of novel sulfonamide derivatives

NASA Astrophysics Data System (ADS)

Demircioğlu, Zeynep; Özdemir, Fethi Ahmet; Dayan, Osman; Şerbetçi, Zafer; Özdemir, Namık

2018-06-01

Synthesized compounds of N-(2-aminophenyl)benzenesulfonamide 1 and (Z)-N-(2-((2-nitrobenzylidene)amino)phenyl)benzenesulfonamide 2 were characterized by antimicrobial activity, FT-IR, 1H and 13C NMR. Two new Schiff base ligands containing aromatic sulfonamide fragment of (Z)-N-(2-((3-nitrobenzylidene)amino)phenyl)benzenesulfonamide 3 and (Z)-N-(2-((4-nitrobenzylidene)amino)phenyl)benzenesulfonamide 4 were synthesized and investigated by spectroscopic techniques including 1H and 13C NMR, FT-IR, single crystal X-ray diffraction, Hirshfeld surface, theoretical method analyses and by antimicrobial activity. The molecular geometry obtained from the X-ray structure determination was optimized Density Functional Theory (DFT/B3LYP) method with the 6-311++G(d,p) basis set in ground state. From the optimized geometry of the molecules of 3 and 4, the geometric parameters, vibrational wavenumbers and chemical shifts were computed. The optimized geometry results, which were well represented the X-ray data, were shown that the chosen of DFT/B3LYP 6-311G++(d,p) was a successful choice. After a successful optimization, frontier molecular orbitals, chemical activity, non-linear optical properties (NLO), molecular electrostatic mep (MEP), Mulliken population method, natural population analysis (NPA) and natural bond orbital analysis (NBO), which cannot be obtained experimentally, were calculated and investigated.
Preparation, characterization, and optical properties of gold, silver, and gold-silver alloy nanoshells having silica cores.

PubMed

Kim, Jun-Hyun; Bryan, William W; Lee, T Randall

2008-10-07

This report describes the structural and optical properties of a series of spherical shell/core nanoparticles in which the shell is comprised of a thin layer of gold, silver, or gold-silver alloy, and the core is comprised of a monodispersed silica nanoparticle. The silica core particles were prepared using the Stöber method, functionalized with terminal amine groups, and then seeded with small gold nanoparticles (approximately 2 nm in diameter). The gold-seeded silica particles were coated with a layer of gold, silver, or gold-silver alloy via solution-phase reduction of an appropriate metal ion or mixture of metal ions. The size, morphology, and elemental composition of the composite nanoparticles were characterized by field emission scanning electron microscopy (FE-SEM), energy-dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, thermal gravimetric analysis (TGA), dynamic light scattering (DLS), and transmission electron microscopy (TEM). The optical properties of the nanoparticles were analyzed by UV-vis spectroscopy, which showed strong absorptions ranging from 400 nm into the near-IR region, where the position of the plasmon band reflected not only the thickness of the metal shell, but also the nature of the metal comprising the shell. Importantly, the results demonstrate a new strategy for tuning the position of the plasmon resonance without having to vary the core diameter or the shell thickness.
Particle design using a 4-fluid-nozzle spray-drying technique for sustained release of acetaminophen.

PubMed

Chen, Richer; Okamoto, Hirokazu; Danjo, Kazumi

2006-07-01

We prepared matrix particles of acetaminophen (Act) with chitosan (Cht) as a carrier using a newly developed 4-fluid-nozzle spray dryer. Cht dissolves in acid solutions and forms a gel, but it does not dissolve in alkaline solutions. Therefore, we tested the preparation of controlled release matrix particles using the characteristics of this carrier. Act and Cht mixtures in prescribed ratios were dissolved in an acid solution. We evaluated the matrix particles by preparing a solid dispersion using a 4-fluid-nozzle spray dryer. Observation of the particle morphology by scanning electron microscopy (SEM) revealed that the particles from the spray drying process had atomized to several microns, and that they had become spherical. We investigated the physicochemical properties of the matrix particles by powder X-ray diffraction, differential scanning calorimetry, and dissolution rate analyses with a view to clarifying the effects of crystallinity on the dissolution rate. The powder X-ray diffraction peaks and the heat of the Act fusion in the spray-dried samples decreased with the increase of the carrier content, indicating that the drug was amorphous. These results indicate that the system formed a solid dispersion. Furthermore, we investigated the interaction between the drug and carrier using FT-IR analysis. The FT-IR spectroscopy for the Act solid dispersions suggested that the Act carboxyl group and the Cht amino group formed a hydrogen bond. In addition, the measurement results of the 13C CP/MAS solid-state NMR, indicated that a hydrogen bond had been formed between the Act carbonyl group and the Cht amino group. In the Act-Cht system, the 4-fluid-nozzle spray-dried preparation with a mixing ratio of 1 : 5 obtained a sustained release preparation in all pH test solutions.
Sensing the Structural Differences in Cellulose from Apple and Bacterial Cell Wall Materials by Raman and FT-IR Spectroscopy

PubMed Central

Szymańska-Chargot, Monika; Cybulska, Justyna; Zdunek, Artur

2011-01-01

Raman and Fourier Transform Infrared (FT-IR) spectroscopy was used for assessment of structural differences of celluloses of various origins. Investigated celluloses were: bacterial celluloses cultured in presence of pectin and/or xyloglucan, as well as commercial celluloses and cellulose extracted from apple parenchyma. FT-IR spectra were used to estimate of the Iβ content, whereas Raman spectra were used to evaluate the degree of crystallinity of the cellulose. The crystallinity index (XCRAMAN%) varied from −25% for apple cellulose to 53% for microcrystalline commercial cellulose. Considering bacterial cellulose, addition of xyloglucan has an impact on the percentage content of cellulose Iβ. However, addition of only xyloglucan or only pectins to pure bacterial cellulose both resulted in a slight decrease of crystallinity. However, culturing bacterial cellulose in the presence of mixtures of xyloglucan and pectins results in an increase of crystallinity. The results confirmed that the higher degree of crystallinity, the broader the peak around 913 cm−1. Among all bacterial celluloses the bacterial cellulose cultured in presence of xyloglucan and pectin (BCPX) has the most similar structure to those observed in natural primary cell walls. PMID:22163913
Multifunctional Nanotherapeutic System for Advanced Prostate Cancer

DTIC Science & Technology

2012-10-01

aqueous part was again dialyzed against fresh deionized water two times for 12 hours. After dialysis the whole content was lyophilized using Freeze ... dryer (VirTis).The conjugate was characterized using UV visible spectroscopy, FT-IR spectroscopy and proton NMR. The results of the UV –Visible
Photochemical degradation of polymeric coatings on mirrors as studied in situ using FT-IR reflection-absorbance spectroscopy

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

Webb, J.D.; Schissel, P.; Czanderna, A.W.

1981-12-01

Reflection-absorbance spectroscopy has been used to obtain analytical information on samples of polymer/metal multilayer stacks subjected to degradative factors. The capabilities of the apparatus are summarized and representative data from initial studies are presented. (LEW)
Diffraction-limited IR Microspectroscopy with IRENI

Treesearch

J. Sedlmair; B. Illman; M. Unger; C. Hirschmugl

2012-01-01

In a unique way, IRENI (Infrared environmental Imaging), operated at the Synchrotron Radiation Center in Madison, combines IR spectroscopy and IR imaging, revealing the chemical morphology of a sample. Most storage ring based IR confocal microscopes have to overcome a trade-off between spatial resolution versus...
Effects of Low Carbohydrate High Protein (LCHP) diet on atherosclerotic plaque phenotype in ApoE/LDLR-/- mice: FT-IR and Raman imaging.

PubMed

Wrobel, T P; Marzec, K M; Chlopicki, S; Maślak, E; Jasztal, A; Franczyk-Żarów, M; Czyżyńska-Cichoń, I; Moszkowski, T; Kostogrys, R B; Baranska, M

2015-09-22

Low Carbohydrate High Protein (LCHP) diet displays pro-atherogenic effects, however, the exact mechanisms involved are still unclear. Here, with the use of vibrational imaging, such as Fourier transform infrared (FT-IR) and Raman (RS) spectroscopies, we characterize biochemical content of plaques in Brachiocephalic Arteries (BCA) from ApoE/LDLR(-/-) mice fed LCHP diet as compared to control, recomended by American Institute of Nutrition, AIN diet. FT-IR images were taken from 6-10 sections of BCA from each mice and were complemented with RS measurements with higher spatial resolution of chosen areas of plaque sections. In aortic plaques from LCHP fed ApoE/LDLR(-/-) mice, the content of cholesterol and cholesterol esters was increased, while that of proteins was decreased as evidenced by global FT-IR analysis. High resolution imaging by RS identified necrotic core/foam cells, lipids (including cholesterol crystals), calcium mineralization and fibrous cap. The decreased relative thickness of the outer fibrous cap and the presence of buried caps were prominent features of the plaques in ApoE/LDLR(-/-) mice fed LCHP diet. In conclusion, FT-IR and Raman-based imaging provided a complementary insight into the biochemical composition of the plaque suggesting that LCHP diet increased plaque cholesterol and cholesterol esters contents of atherosclerotic plaque, supporting the cholesterol-driven pathogenesis of LCHP-induced atherogenesis.
Rapid measurement of human milk macronutrients in the neonatal intensive care unit: accuracy and precision of fourier transform mid-infrared spectroscopy.

PubMed

Smilowitz, Jennifer T; Gho, Deborah S; Mirmiran, Majid; German, J Bruce; Underwood, Mark A

2014-05-01

Although it is well established that human milk varies widely in macronutrient content, it remains common for human milk fortification for premature infants to be based on historic mean values. As a result, those caring for premature infants often underestimate protein intake. Rapid precise measurement of human milk protein, fat, and lactose to allow individualized fortification has been proposed for decades but remains elusive due to technical challenges. This study aimed to evaluate the accuracy and precision of a Fourier transform (FT) mid-infrared (IR) spectroscope in the neonatal intensive care unit to measure human milk fat, total protein, lactose, and calculated energy compared with standard chemical analyses. One hundred sixteen breast milk samples across lactation stages from women who delivered at term (n = 69) and preterm (n = 5) were analyzed with the FT mid-IR spectroscope and with standard chemical methods. Ten of the samples were tested in replicate using the FT mid-IR spectroscope to determine repeatability. The agreement between the FT mid-IR spectroscope analysis and reference methods was high for protein and fat and moderate for lactose and energy. The intra-assay coefficients of variation for all outcomes were less than 3%. The FT mid-IR spectroscope demonstrated high accuracy in measurement of total protein and fat of preterm and term milk with high precision.
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
One-Pot Route towards Active TiO2 Doped Hierarchically Porous Cellulose: Highly Efficient Photocatalysts for Methylene Blue Degradation

PubMed Central

Sun, Xiaoxia; Wang, Kunpeng; Shu, Yu; Zou, Fangdong; Zhang, Boxing; Sun, Guangwu; Uyama, Hiroshi; Wang, Xinhou

2017-01-01

In this study, novel photocatalyst monolith materials were successfully fabricated by a non-solvent induced phase separation (NIPS) technique. By adding a certain amount of ethyl acetate (as non-solvent) into a cellulose/LiCl/N,N-dimethylacetamide (DMAc) solution, and successively adding titanium dioxide (TiO2) nanoparticles (NPs), cellulose/TiO2 composite monoliths with hierarchically porous structures were easily formed. The obtained composite monoliths possessed mesopores, and two kinds of macropores. Scanning Electron Microscope (SEM), Energy Dispersive Spectroscopy (EDS), Fourier Transform Infrared Spectroscopy (FT-IR), X-ray Diffraction (XRD), Brunauer-Emmett-Teller (BET), and Ultraviolet-visible Spectroscopy (UV-Vis) measurements were adopted to characterize the cellulose/TiO2 composite monolith. The cellulose/TiO2 composite monoliths showed high efficiency of photocatalytic activity in the decomposition of methylene blue dye, which was decomposed up to 99% within 60 min under UV light. Moreover, the composite monoliths could retain 90% of the photodegradation efficiency after 10 cycles. The novel NIPS technique has great potential for fabricating recyclable photocatalysts with highly efficiency. PMID:28772734
Preparation of Fe 3O 4/poly(styrene-butyl acrylate-[2-(methacryloxy)ethyl]trimethylammonium chloride) by emulsifier-free emulsion polymerization and its interaction with DNA

NASA Astrophysics Data System (ADS)

Li, Xiaolong; Liu, Guoqiang; Yan, Wei; Chu, Paul K.; Yeung, Kelvin W. K.; Wu, Shuilin; Yi, Changfeng; Xu, Zushun

2012-04-01

Cationic magnetic polymer particles Fe3O4/poly(styrene-butyl acrylate-[2-(methacryloxy)ethyl]trimethylammonium chloride), a type of potential gene carrier, were prepared by emulsifier-free emulsion polymerization with oleic acid modified magnetite Fe3O4, styrene, butyl acrylate and [2-(methacryloxy)ethyl]trimethylammonium chloride) (METAC). The morphology of the particles was characterized by transmission electron microscopy and the composites of particles were characterized by FT-IR spectroscopy, X-ray diffraction. These results showed that magnetic particles were well dispersed in polymers with the content of about 15%(wt/wt). The composites exhibited superparamagnetism and possessed a certain level of magnetic response. The interactions between the particles with calf-thymus DNA (ct DNA) were confirmed by zeta potential measurement, UV-vis spectroscopy and fluorescence spectroscopy. The DNA-binding capacity determined by the agarose gel electrophoresis showed good binding capacity of the emulsion to DNA. These results suggested the potential of the cationic magnetic polymer emulsion as gene target delivery carrier.
Application of glucose as a green capping agent and reductant to fabricate CuI micro/nanostructures

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

Tavakoli, Farnosh; Salavati-Niasari, Masoud, E-mail: salavati@kashanu.ac.ir; Ghanbari, Davood

Graphical abstract: - Highlights: • CuI nanostructures were prepared via a simple precipitation method. • Glucose as a green capping agent and reductant was applied. • The effect of glucose concentration on the morphology of CuI was investigated. • According to XRD results, pure cubic phase CuI have been formed by using glucose. - Abstract: In this work, CuI micro/nanostructures have been successfully prepared via a simple precipitation route at room temperature. By using glucose as a clean reducing agent with different concentrations, CuI micro/nanostructures with various morphologies were obtained. Besides glucose, Na{sub 2}SO{sub 3}, KBH{sub 4} and N{sub 2}H{submore » 4}·H{sub 2}O have been applied as reductant. X-ray diffraction (XRD), scanning electron microscopy (SEM), photoluminescence spectroscopy, X-ray energy dispersive spectroscopy (EDS) and Fourier transformed infrared (FT-IR) spectroscopy were used to characterize the as-produced CuI micro/nanostructures. According to the XRD results, it was found that pure cubic phase CuI have been formed by using glucose.« less
Synthesis of Fluorinated Graphene/CoAl-Layered Double Hydroxide Composites as Electrode Materials for Supercapacitors.

PubMed

Peng, Weijun; Li, Hongqiang; Song, Shaoxian

2017-02-15

CoAl-layered double hydroxide/fluorinated graphene (CoAl-LDH/FGN) composites were fabricated via a two-step hydrothermal method. The synthesized CoAl-LDH/FGN composites have been characterized by powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), field-emission scanning electron microscopy (FESEM), energy dispersive X-ray spectroscopy (EDS), and electrochemical measurements. The results indicated that the fluorinated carbon with various configuration forms were grafted onto the framework of graphene, and the C-F bond configuration and fluorine content could be tuned by the fluorination time. Most of semi-ionic C-F bonds were formed at an appropriate fluorination time and, then, converted into fluorine rich surface groups (such as CF 2 , CF 3 , etc.) which were electrochemically inactive as the fluorination time prolonged. Moreover, the CoAl-LDH/FGN composites prepared at the optimal fluorination time exhibited the highest specific capacitance (1222 F/g at 1 A/g), the best rate capability, and the most stable capacitance retention, which offered great promise as electrode materials for supercapacitors.
Preparation of Copper (II) Containing Phosphomolybdic Acid Salt as Catalyst for the Synthesis of Biodiesel by Esterification.

PubMed

Cai, Jie; Zhang, Qiu-Yun; Wei, Fang-Fang; Huang, Jin-Shu; Feng, Yun-Mei; Ma, Hai-Tao; Zhang, Yutao-

2018-04-01

Copper (II) containing phosphomolybdic acid (PMA) catalysts were synthesized by ion exchange method and characterization using various physico-chemical techniques such as X-ray diffraction (XRD), fourier transform infrared spectroscopy (FT-IR), thermogravimetric (TG) and scanning electron microscopy (SEM). The characterization results showed that the Keggin ions were retained in the catalysts and possessed well thermal stability. The catalytic esterification of lauric acid with methanol could be easily achieved about 78.7% conversion under optimum condition, the catalyst also contributed to the stability of the catalyst in which it can be reused for a certain time. This study demonstrated an alternative approach to biodiesel production with high efficiency by Cu (II) ion exchanged phosphomolybdic acid catalyst in the esterification catalytic.
Conductivity study of thermally stabilized RuO2/polythiophene nanocomposites

NASA Astrophysics Data System (ADS)

Hebbar, Vidyashree; Bhajantri, R. F.

2018-04-01

The polymer nanocomposites of Ruthenium oxide (RuO2) filled polythiophene (PT) were synthesized by polymerization using chemical method. The purity of the synthesized polymer composite is verified using X-Ray diffraction (XRD). The structural discrepancies of the RuO2 filled PT composites are studied by Fourier transform infrared (FT-IR) spectroscopy. The phase transition and thermal stability of the prepared composite is revised by thermal characterization such as differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). The DC conductivity of RuO2 filled PT composite in the form of pellets is calculated using current-voltage (I-V) characterization by two-probe method. The enhancement in conductivity with increased RuO2 content in PT matrix is examined, which is the required property for electrical and electronic applications in supercapacitors.
A facile mechanochemical approach to synthesize Zn-Al layered double hydroxide

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

Qu, Jun, E-mail: forsjun@whut.edu.cn; He, Xiaoman; Chen, Min

2017-06-15

In this study, a mechanochemical route to synthesize Zn-Al layered double hydroxide (LDH) was introduced, in which Zn basic carbonate and Al hydroxide were first dry milled into an activated state and then agitated in water to obtain the final products. The as-prepared samples were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), Thermogravimetry (TG) and Scanning electron microscopy (SEM). The products possessed a high crystallinity of Zn–Al LDH phase without any other impurities, proving a facile and effective preparation of Zn–Al LDH by using non-heating mechanochemical approach. - Highlights: • A non-heating mechanochemical route to synthesize Zn-Almore » LDH. • The products possessed high crystalline Zn-Al LDH phase. • No emission of other impurities or wastewater.« less

Syntheses, crystal structures and properties of series of 4d-4f ln(III)-Ag(I) heterometallic coordination polymers

NASA Astrophysics Data System (ADS)

Ran, Xing-Rui; Wang, Ning; Xie, Wei-Ping; Xiong, Yan-Ju; Cheng, Qian; Long, Yi; Yue, Shan-Tang; Liu, Ying-Liang

2015-05-01

By control of the experimental parameters such as ligands, pH value and reacting temperature, series of three-dimensional (3D) 4d-4f Ln(III)-Ag(I) porous coordination polymers (PCPs) with interesting chain-layer construction, namely, {[LnIIIAgI(na)(ina)(ox)]·2(H2O)}n [Ln=Sm(1), Eu(2), Gd(3), Tb(4), Dy(5), Ho(6), Y(7), Yb(8)], have been successfully synthesized under hydrothermal conditions and structurally characterized. All the complexes are characterized by elemental analyses, FT-IR spectroscopy, Powder X-ray diffraction (PXRD) and thermogravimetric analyses (TGA). Furthermore, the luminescence properties of compounds 2 and 4 and the magsnetic properties of complexes 3 and 5 were also investigated in detail.
Production and characterization of hydrophobic zinc borate by using palm oil

NASA Astrophysics Data System (ADS)

Acarali, Nil Baran; Tugrul, Nurcan; Derun, Emek Moroydor; Piskin, Sabriye

2013-11-01

Zinc borate (ZB) was synthesized using zinc oxide, boric acid synthesized from colemanite, and reference ZB as seed. The effects of reaction parameters such as reaction time, reactant ratio, and seed ratio on its yield were examined. Then, the effects of palm oil with solvents (isopropyl alcohol (IPA), ethanol, and methanol) added to the reaction on its hydrophobicity were explored. Reactions were carried out under determined reaction conditions with magnetically and mechanically stirred systems. The produced ZB was characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), and measurements of contact angle identified hydrophobicity. The results showed that hydrophobic ZB was successfully produced under determined reaction conditions. The change of process parameters influenced its yield and the usage of palm oil provided hydrophobicity.
Hydroxyapatite nanocrystals: simple preparation, characterization and formation mechanism.

PubMed

Mohandes, Fatemeh; Salavati-Niasari, Masoud; Fathi, Mohammadhossein; Fereshteh, Zeinab

2014-12-01

Crystalline hydroxyapatite (HAP) nanoparticles and nanorods have been successfully synthesized via a simple precipitation method. To control the shape and particle size of HAP nanocrystals, coordination ligands derived from 2-hydroxy-1-naphthaldehyde were first prepared, characterized by Fourier transform infrared (FT-IR) and proton nuclear magnetic resonance ((1)H-NMR) spectroscopies, and finally applied in the synthesis process of HAP. On the other hand, the HAP nanocrystals were also characterized by several techniques including powder X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). According to the FE-SEM and TEM micrographs, it was found that the morphology and crystallinity of the HAP powders depended on the coordination mode of the ligands. Copyright © 2014 Elsevier B.V. All rights reserved.
Synthesis and characterization of high-quality cobalt vanadate crystals and their applications in lithium-ion batteries

NASA Astrophysics Data System (ADS)

Bhuiyan, Md. Tofajjol Hossen; Rahman, Md. Afjalur; Rahman, Md. Atikur; Sultana, Rajia; Mostafa, Md. Rakib; Tania, Asmaul Husna; Sarker, Md. Abdur Razzaque

2016-12-01

High-quality cobalt vanadate crystals have been synthesized by solid-state reaction route. Structure and morphology of the synthesized powders were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), and Fourier transform infrared (FT-IR) spectroscopy. The XRD patterns revealed that the as prepared materials are of high crystallinity and high quality. The SEM images showed that the crystalline CoV2O6 material is very uniform and well separated, with particle (of) area 252 μm. The electronic and optical properties were investigated by impedance analyzer and UV-visible spectrophotometer. Temperature-dependent electrical resistivity was measured using four-probe technique. The crystalline CoV2O6 material is a semiconductor and its activation energy is 0.05 eV.
Polyethyleneglycol/silver functionalized reduced graphene oxide aerogel for environmental application

NASA Astrophysics Data System (ADS)

Kumari, G. Vanitha; Asha, S.; Ananth, A. Nimrodh; Rajan, M. A. Jothi; Mathavan, T.

2018-04-01

Polyethylene glycol (PEG)/Silver (Ag) functionalized reduced graphene oxide aerogel (RGOA) was synthesized. PEG/Ag decorated reduced graphene oxide aerogel was characterized using XRD, Raman spectroscopy, Fourier transform infrared spectroscopy (FT-IR). The surface morphology of PEG/Ag/RGOA was analyzed using scanning electron microscope. The non-covalent interaction between reduced graphene oxide layers and the interaction between PEG and Ag on RGOA were studied by FT-IR spectra. It was observed that the interaction between Ag and PEG could enhance the properties of RGOA. Methyl Orange (MO) dye degradation was observed from UV-Vis Spectra. The process was studied by monitoring the simultaneous decrease in the height of UV-Vis absorption peak of dye solution. The results show that PEG/RGOA and PEG/Ag/RGOA are an efficient catalyst for dye degradation.
Fast quality control of Herba Epimedii by using Fourier transform infrared spectroscopy

NASA Astrophysics Data System (ADS)

Pei, Li-Kuan; Sun, Su-Qin; Guo, Bao-Lin; Huang, Wen-Hua; Xiao, Pei-Gen

2008-07-01

Herba Epimedii is a well-known traditional Chinese medicine (TCM) having the effect of nourishing the kidney and strengthening the 'Yang'. Its primary effective constituents are considered to be the 8-prenyl flavonols, which can be assorted into 4'-methoxyl-prenylflavonols (MPFs) and 4'-hydroxyl-prenylflavonols (HPFs), according to the group (methoxyl or hydroxyl) located at 4' in their structures. The Fourier transform infrared spectroscopy (FT-IR) has been widely used in the researches of TCMs. In the present study, the FT-IR was attempted to be applied in the quality control of Herba Epimedii. We compared the IR spectra of 17 pure flavonoids, of which eight were derived from Herba Epimedii, and found a characteristic absorption peak at 1259 ± 1 cm -1, corresponding to the MPFs, the major 8-prenyl flavonols in the aerial parts of the Epimedium species. This peak could also be found in the IR spectra of both the herbal samples and their 70% ethanol extracts. Moreover, the intensity of this peak was in the direct correlation with the total content of MPFs. The correlation values, representing the semblance of two spectra, of the IR spectrum of herbal sample and icariin, in the range of 1280-1200 cm -1, had been established to be a good index for the quality control of the herbs. Accordingly, a correlation value of not less than 0.50 could be used as the essential screening criteria for the herbs. The FT-IR could be used for the fast and effective quality control of Herba Epimedii.
Antimicrobial cellulosic hydrogel from olive oil industrial residue.

PubMed

Dacrory, Sawsan; Abou-Yousef, Hussein; Abouzeid, Ragab E; Kamel, Samir; Abdel-Aziz, Mohamed S; El-Badry, Mohamed

2018-05-25

The cellulose-based antimicrobial hydrogel was prepared from seed and husk cellulosic fibers of olive industry residues by load silver nanoparticles (AgNPs) onto grafted acrylamide monomer (Am) cellulosic fibers. The grafting approach was the free radical mechanism by utilizing ceric ammonium nitrate (CAN) as initiator in aqueous medium and N,N methylene bisacrylamide (MBAm) as a cross linker. The effect of different grafting conditions on the properties of produced hydrogels has been studied by determining the grafting parameters, i.e. concentration of Am, MBAm, grafting time and temperature to optimize grafting yield (G %), grafting efficiency (GE %), and swelling %. Characterizations of the obtained hydrogels were performed through monitoring swelling behavior, FTIR spectroscopy, SEM, and EDX. AgNPs were grown into the prepared hydrogel. Hydrogel/AgNPs were characterized by FT-IR spectroscopy, X-ray diffraction (XRD) and scanning electron microscopy (SEM). The hydrogel loaded AgNPs exhibit high efficient antimicrobial activity against Staphylococcus aureus, Pseudomonas aeruginosa, and Candida albicans. Copyright © 2018. Published by Elsevier B.V.
Functionalized mesoporous silica supported copper(II) and nickel(II) catalysts for liquid phase oxidation of olefins.

PubMed

Nandi, Mahasweta; Roy, Partha; Uyama, Hiroshi; Bhaumik, Asim

2011-12-14

Highly ordered 2D-hexagonal mesoporous silica has been functionalized with 3-aminopropyltriethoxysilane (3-APTES). This is followed by its condensation with a dialdehyde, 4-methyl-2,6-diformylphenol to produce an immobilized Schiff-base ligand (I). This material is separately treated with methanolic solution of copper(II) chloride and nickel(II) chloride to obtain copper and nickel anchored mesoporous materials, designated as Cu-AMM and Ni-AMM, respectively. The materials have been characterized by Fourier transform infrared (FT-IR) and UV-vis diffuse reflectance (DRS) spectroscopy, powder X-ray diffraction (XRD), transmission electron microscopy (TEM), N(2) adsorption-desorption studies and (13)C CP MAS NMR spectroscopy. The metal-grafted mesoporous materials have been used as catalysts for the efficient and selective epoxidation of alkenes, viz. cyclohexene, trans-stilbene, styrene, α-methyl styrene, cyclooctene and norbornene to their corresponding epoxides in the presence of tert-butyl hydroperoxide (TBHP) as the oxidant under mild liquid phase conditions.
Green synthesis of silver nanoparticles using Terminalia chebula extract at room temperature and their antimicrobial studies

NASA Astrophysics Data System (ADS)

Mohan Kumar, Kesarla; Sinha, Madhulika; Mandal, Badal Kumar; Ghosh, Asit Ranjan; Siva Kumar, Koppala; Sreedhara Reddy, Pamanji

2012-06-01

A green rapid biogenic synthesis of silver nanoparticles (Ag NPs) using Terminalia chebula (T. chebula) aqueous extract was demonstrated in this present study. The formation of silver nanoparticles was confirmed by Surface Plasmon Resonance (SPR) at 452 nm using UV-visible spectrophotometer. The reduction of silver ions to silver nanoparticles by T. chebula extract was completed within 20 min which was evidenced potentiometrically. Synthesised nanoparticles were characterised using UV-vis spectroscopy, Fourier transformed infrared spectroscopy (FT-IR), powder X-ray diffraction (XRD), transmission electron microscopy (TEM) and atomic force microscopy (AFM). The hydrolysable tannins such as di/tri-galloyl-glucose present in the extract were hydrolyzed to gallic acid and glucose that served as reductant while oxidised polyphenols acted as stabilizers. In addition, it showed good antimicrobial activity towards both Gram-positive bacteria (S. aureus ATCC 25923) and Gram-negative bacteria (E. coli ATCC 25922). Industrially it may be a smart option for the preparation of silver nanoparticles.
Biogenic copper oxide nanoparticles synthesis using Tabernaemontana divaricate leaf extract and its antibacterial activity against urinary tract pathogen

NASA Astrophysics Data System (ADS)

Sivaraj, Rajeshwari; Rahman, Pattanathu K. S. M.; Rajiv, P.; Salam, Hasna Abdul; Venckatesh, R.

2014-12-01

This investigation explains the biosynthesis and characterization of copper oxide nanoparticles from an Indian medicinal plant by an eco-friendly method. The main objective of this study is to synthesize copper oxide nanoparticles from Tabernaemontana divaricate leaves through a green chemistry approach. Highly stable, spherical copper oxide nanoparticles were synthesized by using 50% concentration of Tabernaemontana leaf extract. Formation of copper oxide nanoparticles have been characterized by UV-Vis absorption spectroscopy, X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM) with energy dispersive X-ray analysis (EDX) and transmission electron microscopy (TEM) analysis. All the analyses revealed that copper oxide nanoparticles were 48 ± 4 nm in size. Functional groups and chemical composition of copper oxide were also confirmed. Antimicrobial activity of biogenic copper oxide nanoparticles were investigated and maximum zone of inhibition was found in 50 μg/ml copper oxide nanoparticles against urinary tract pathogen (Escherichia coli).
One-step Melt Synthesis of Water Soluble, Photoluminescent, Surface-Oxidized Silicon Nanoparticles for Cellular Imaging Applications

PubMed Central

Manhat, Beth A.; Brown, Anna L.; Black, Labe A.; Ross, J.B. Alexander; Fichter, Katye; Vu, Tania; Richman, Erik

2012-01-01

We have developed a versatile, one-step melt synthesis of water-soluble, highly emissive silicon nanoparticles using bi-functional, low-melting solids (such as glutaric acid) as reaction media. Characterization through transmission electron microscopy, selected area electron diffraction, X-ray photoelectron spectroscopy, and Raman spectroscopy shows that the one-step melt synthesis produces nanoscale Si cores surrounded by a silicon oxide shell. Analysis of the nanoparticle surface using FT-IR, zeta potential, and gel electrophoresis indicates that the bi-functional ligand used in the one-step synthesis is grafted onto the nanoparticle, which allows for tuning of the particle surface charge, solubility, and functionality. Photoluminescence spectra of the as-prepared glutaric acid-synthesized silicon nanoparticles show an intense blue-green emission with a short (ns) lifetime suitable for biological imaging. These nanoparticles are found to be stable in biological media and have been used to examine cellular uptake and distribution in live N2a cells. PMID:23139440
Preparation and Characterization of Self-Reinforced Antibacterial and Oil-Resistant Paper Using a NaOH/Urea/ZnO Solution.

PubMed

Jiao, Li; Ma, Jinxia; Dai, Hongqi

2015-01-01

This paper describes self-reinforced antibacterial and oil-resistant properties that were successfully prepared by surface selective dissolution of filter paper in a NaOH/Urea/ZnO (weight ratio of 8:12:0.25) aqueous solution. The effect of the processing time on the mechanical properties of this paper was evaluated at -12°C. The paper morphologies were characterized using Scanning Electron Microscopy (SEM), X-ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FT-IR) and X-ray photoelectron spectroscopy (XPS). The oil-resistance and antibacterial properties of the produced paper were also investigated. Excellent mechanical properties were observed for an optimized handling time. The tensile and burst strengths of the modified paper were in excess of 100% of the original. Meanwhile, the treated paper was completely oil-resistant within 24 h and demonstrated good antibacterial properties when exposed to Staphylococcus aureus. The traces of residual zinc oxide were found to be safe for food.
Preparation and Characterization of Self-Reinforced Antibacterial and Oil-Resistant Paper Using a NaOH/Urea/ZnO Solution

PubMed Central

Jiao, Li; Ma, Jinxia; Dai, Hongqi

2015-01-01

This paper describes self-reinforced antibacterial and oil-resistant properties that were successfully prepared by surface selective dissolution of filter paper in a NaOH/Urea/ZnO (weight ratio of 8:12:0.25) aqueous solution. The effect of the processing time on the mechanical properties of this paper was evaluated at -12°C. The paper morphologies were characterized using Scanning Electron Microscopy (SEM), X-ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FT-IR) and X-ray photoelectron spectroscopy (XPS). The oil-resistance and antibacterial properties of the produced paper were also investigated. Excellent mechanical properties were observed for an optimized handling time. The tensile and burst strengths of the modified paper were in excess of 100% of the original. Meanwhile, the treated paper was completely oil-resistant within 24 h and demonstrated good antibacterial properties when exposed to Staphylococcus aureus. The traces of residual zinc oxide were found to be safe for food. PMID:26465917
Biogenic Silver Nanoparticles by Gelidiella acerosa Extract and their Antifungal Effects

PubMed Central

Vivek, Marimuthu; Kumar, Palanisamy Senthil; Steffi, Sesurajan; Sudha, Sellappa

2011-01-01

The synthesis, characterization and application of biologically synthesized nanomaterials are an important aspect in nanotechnology. The present study deals with the synthesis of silver nanoparticles (Ag-NPs) using the aqueous extract of red seaweed Gelidiella acerosa as the reducing agent to study the antifungal activity. The formation of Ag-NPs was confirmed by UV-Visible Spectroscopy, X-Ray Diffraction (XRD) pattern, Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM). The synthesized Ag-NPs was predominately spherical in shape and polydispersed. Fourier Transform Infra-Red (FT-IR) spectroscopy analysis showed that the synthesized nano-Ag was capped with bimolecular compounds which are responsible for reduction of silver ions. The antifungal effects of these nanoparticles were studied against Humicola insolens (MTCC 4520), Fusarium dimerum (MTCC 6583), Mucor indicus (MTCC 3318) and Trichoderma reesei (MTCC 3929). The present study indicates that Ag-NPs have considerable antifungal activity in comparison with standard antifungal drug, and hence further investigation for clinical applications is necessary. PMID:23408653
Preparation and characterization of dialdehyde starch by one-step acid hydrolysis and oxidation.

PubMed

Zuo, Yingfeng; Liu, Wenjie; Xiao, Junhua; Zhao, Xing; Zhu, Ying; Wu, Yiqiang

2017-10-01

Dialdehyde starch was prepared by one-step synthesis of acid hydrolysis and oxidation, using corn starch as the raw material, sodium periodate (NaIO 4 ) as the oxidant, and hydrochloric acid (HCl) as the acid solution. The prepared dialdehyde starch was characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), and gel permeation chromatography (GPC). The results confirmed that oxidation occurred between the starch and NaIO 4 . The acid hydrolysis reaction reduced the molecular weight of starch and effectively improved the aldehyde group contents (92.7%). Scanning electron microscope (SEM) analysis indicated that the average particle size decreased after acid hydrolysis and oxidation reaction. X-ray diffraction (XRD) and thermal gravimetric analyzer (TGA) analysis demonstrated that the crystallinity of the obtained dialdehyde starch showed a downward trend and a decelerated thermal decomposition rate. The starch after acid hydrolysis and oxidation exhibited lower hot paste viscosity and higher reactivity. Copyright © 2017. Published by Elsevier B.V.
Montmorillonite/graphene oxide/chitosan composite: Synthesis, characterization and properties.

PubMed

Yadav, Mithilesh; Ahmad, Sharif

2015-08-01

The present work reports the successful preparation, thermal and mechanical characterization of high performance films of Na(+) montmorillonite (MMT)/graphene oxide (GO)/chitosan (CS) composite using simple solution mixing evaporation method. The formations of films were verified by Fourier transform infrared (FT-IR) spectroscopy, scanning electron microscopy (SEM), X-ray diffraction (XRD) and Raman spectroscopy. The thermal stability and mechanical properties of these films were investigated by thermogravimetric analysis (TGA) and mechanical testing (Instron 8871). The results obtained from these studies revealed that the composites of chitosan, MMT, and graphene oxide were homogeneous in nature. A synergistic effect of MMT and GO reinforcing on chitosan matrix was observed for the first time, in case of 5 wt.% MMT and 1 wt.% GO. The tensile strength of (5 wt.%) MMT/(1 wt.%) GO/CS composite was formed 9±0.23% and 27±0.25% higher than that of the (1 wt.%) GO/CS composite and chitosan, respectively. Copyright © 2015 Elsevier B.V. All rights reserved.
One-step synthesis of solid state luminescent carbon-based silica nanohybrids for imaging of latent fingerprints

NASA Astrophysics Data System (ADS)

Li, Feng; Li, Hongren; Cui, Tianfang

2017-11-01

Fluorescent carbon-based nanomaterials(CNs) with tunable visible emission are biocompatible, environment friendly and most suitable for various biomedical applications. Despite the successes in preparing strongly fluorescent CNs, preserving the luminescence in solid materials is still challenging because of the serious emission quenching of CNs in solid state materials. In this work, fluorescent carbon and silica nanohybrids (SiCNHs) were synthesized via a simple one-step hydrothermal approach by carbonizing sodium citrate and (3-aminopropyl)triethoxysilane(APTES), and hydrolysis of tetraethyl orthosilicate(TEOS). The resultant SiCNs were characterized through X-ray diffraction (XRD), transmission electron microscopy (TEM), FT-IR, X-ray photoelectron spectroscopy (XPS), and photoluminescence (PL) spectroscopy. The SiCNs exhibited strong fluorescence in both aqueous and solid states. The luminescent solid state SiCNs power were successfully used as a fluorescent labeling material for enhanced imaging of latent fingerprints(LFPs) on single background colour and multi-coloured surfaces substrates in forensic science for individual identification.
Rapid discrimination of Panax notogeinseng of different grades by FT-IR and 2DCOS-IR

NASA Astrophysics Data System (ADS)

Ma, Fang; Chen, Jian-bo; Wu, Xian-xue; Zhou, Qun; Sun, Su-qin

2016-11-01

The herbal material of Notoginseng (the root of Panax notoginseng) is sold by "Tou" (the number of Notoginseng in every 500 g) to distinguish the grade. Normally the better quality, the few number of the "Tou" and the size of Notoginseng is bigger. In this study, three grades of Notoginseng harvested from Yunnan province were discriminated and identified by Fourier transform infrared spectroscopy (FT-IR) and two-dimensional correlation infrared spectroscopy (2DCOS-IR)). The correlation coefficient of IR spectra between the three grades of Notoginseng and starch are greater than 0.95 in the range of 1300-800 cm-1, means the main compositions of Notoginseng are starch polysaccharide. Also, when the size of Notoginseng is bigger, it may contain more polysaccharide. There is no difference in range of 815-1000 cm-1 of the 2DCOS-IR synchronous spectra of the three grades means polysaccharides possess good thermal stability. In the range of 1200-1300 cm-1 shows the inverse ration between the thermal sensitivity of C-O and the number of "Tou". Combination with the 2DCOS-IR asynchronous spectra, the response speed of amino acid (1640 cm-1) on the thermal perturbation is the fastest, followed by nitrate (1384 cm-1); the response speed of polysaccharides (1079 cm-1) is the slowest. The result proved that the 2DCOS-IR could discriminate different grades of Notoginseng.
Investigation of the Cross-Section Stratifications of Icons Using Micro-Raman and Micro-Fourier Transform Infrared (FT-IR) Spectroscopy.

PubMed

Lazidou, Dimitra; Lampakis, Dimitrios; Karapanagiotis, Ioannis; Panayiotou, Costas

2018-01-01

The cross-section stratifications of samples, which were removed from six icons, are studied using optical microscopy, micro-Raman spectroscopy, and micro-Fourier transform infrared (FT-IR) spectroscopy. The icons, dated from the 14th to 19th centuries, are prominent examples of Byzantine painting art and are attributed to different artistic workshops of northern Greece. The following materials are identified in the cross-sections of the icon samples using micro-Raman spectroscopy: anhydrite; calcite; carbon black; chrome yellow; cinnabar; gypsum; lead white; minium; orpiment; Prussian blue; red ochre; yellow ochre; and a paint of organic origin which can be either indigo ( Indigofera tinctoria L. and others) or woad ( Isatis tinctoria L.). The same samples are investigated using micro-FT-IR which leads to the following identifications: calcite; calcium oxalates; chrome yellow; gypsum; kaolinite; lead carboxylates; lead sulfate (or quartz); lead white; oil; protein; Prussian blue; saponified oil; shellac; silica; and tree resin. The study of the cross-sections of the icon samples reveals the combinations of the aforementioned inorganic and organic materials. Although the icons span over a long period of six centuries, the same stratification comprising gypsum ground layer, paint layers prepared by modified "egg tempera" techniques (proteinaceous materials mixed with oil and resins), and varnish layer is revealed in the investigated samples. Moreover, the presence of three layers of varnishes, one at the top and other two as intermediate layers, in the cross-section analysis of a sample from Virgin and Child provide evidence of later interventions.
Photocatalytic degradation of metronidazole and methylene blue by PVA-assisted Bi2WO6-CdS nanocomposite film under visible light irradiation

NASA Astrophysics Data System (ADS)

Rajendran, Ranjith; Varadharajan, Krishnakumar; Jayaraman, Venkatesan; Singaram, Boobas; Jeyaram, Jayaprakash

2018-02-01

The enhanced photocatalytic performance of nanocomposite is synthesized via the hydrothermal method and characterized using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), field emission scanning electron microscopy (FESEM), Fourier transform infrared spectroscopy (FT-IR), UV-visible diffuse reflectance spectroscopy (UV-Vis DRS) and photoluminescence spectroscopy (PL). Under visible light irradiation, PVA assisted Bi2WO6-CdS nanocomposite film displayed enhanced photocatalytic efficiency and inhibition of photocorrosion as compared with pure CdS, pure Bi2WO6 and Bi2WO6-CdS composite. The PVA assisted Bi2WO6-CdS composite film catalyst showed stable catalytic performance until seven successive runs with 92% of methylene blue(MB) degradation, and easy to recover after degradation of organic pollutant. PVA assisted Bi2WO6-CdS nanocomposite film has optimal band edge position for superior photocatalytic degradation. Furthermore, the trapping experiment was carried out using different scavenger for active species. Among the active species, OH· are the most responsive species which play a vital role in the degradation of metronidazole and MB.

Fabrication of chloroform sensor based on hydrothermally prepared low-dimensional β-Fe 2O 3 nanoparticles

NASA Astrophysics Data System (ADS)

Rahman, Mohammed M.; Jamal, A.; Khan, Sher Bahadar; Faisal, M.

2011-10-01

Hydrothermally prepared as-grown low-dimensional nano-particles (NPs) have been characterized using UV-vis spectroscopy, Fourier transform infrared (FT-IR) spectroscopy, powder X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), Raman spectroscopy, and electron dispersion spectroscopy (EDS). The uniformity of the nano-material was executed by the scanning electron microscopy, where the single phase of the nano-crystalline β-Fe 2O 3 was characterized using XRD techniques. β-Fe 2O 3 nanoparticles fabricated glassy carbon electrode (GCE) have improved chloroform-sensing performances in terms of electrical response ( I- V technique) for detecting analyte in liquid phase. The analytical performances were investigated, which showed that the better sensitivity, stability, and reproducibility of the sensor improved significantly by using Fe 2O 3 NPs thin-film on GCE. The calibration plot was linear ( R = 0.9785) over the large range of 12.0 μM to 12.0 mM. The sensitivity was calculated as 2.1792 μA cm -2 mM -1 with a detection limit of 4.4 ± 0.10 μM in short response time (10.0 s).
Progress of reduction of graphene oxide by ascorbic acid

NASA Astrophysics Data System (ADS)

De Silva, K. Kanishka H.; Huang, Hsin-Hui; Yoshimura, Masamichi

2018-07-01

Graphene oxide (GO) and reduced graphene oxide (RGO) are in greater demand in many research fields. As a result, the synthesis of these materials on a large scale in a costeffective manner is more concerned for numerous applications. In the present work, GO was synthesized by oxidizing natural graphite and reduced by ascorbic acid (AA), which is a green reductant. The reduced products obtained at different time periods were in detail characterized by UV-Visible spectroscopy, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), attenuated total reflectance Fourier transform infrared (ATR-FT-IR) spectroscopy, Raman spectroscopy, thermogravimetric analysis (TGA), atomic force microscopy (AFM) and scanning electron microscopy (SEM). Results showed that the oxidation of graphite has given highly oxidized GO with a 9.30 Å interlayer space and about 33% of oxygen atomic percentage. Until 50 min of the reduction, both GO and RGO coexist. The reduction rate is fast within the first 30 min. In addition, the suitability of natural graphite over synthetic graphite for the synthesis of GO is shown. The findings of this work pave the way to select GO and RGO for applications of interest in a cheap, green and efficient manner.
Speciation And Distribution Of Arsenic In Fresh Water Pond Sediments Impacted By Contaminated Ground-Water Discharge (Presentation)

EPA Science Inventory

The speciation and mineralogy of sediments contaminated with arsenic due to arsenic enriched groundwater discharging into the pond at the Ft. Devens Super Fund Site in Ft. Devens, MA were determined using X-ray absorption fine structure and X-ray diffraction spectroscopy. Speci...
Conformational, IR spectroscopic and electronic properties of conium alkaloids and their adducts with C60 fullerene

NASA Astrophysics Data System (ADS)

Zabolotnyi, M. A.; Prylutskyy, Yu I.; Poluyan, N. A.; Evstigneev, M. P.; Dovbeshko, G. I.

2016-08-01

Conformational, IR spectroscopic and electronic properties of the components of Conium alkaloids (Conium maculatum) in aqueous environment were determined by model calculations and experiment. With the help of FT-IR spectroscopy the possibility of formation of an adduct between γ-coniceine alkaloid and C60 fullerene was demonstrated, which is important for further application of conium analogues in biomedical purposes.
Formulation and characterization of hydrophilic drug diclofenac sodium-loaded solid lipid nanoparticles based on phospholipid complexes technology.

PubMed

Liu, Dongfei; Chen, Li; Jiang, Sunmin; Zhu, Shuning; Qian, Yong; Wang, Fengzhen; Li, Rui; Xu, Qunwei

2014-03-01

To successfully prepare the diclofenac sodium (DS)-loaded solid lipid nanoparticles (SLNs), phospholipid complexes (PCs) technology was applied here to improve the liposolubility of DS. Solid lipid nanoparticles (SLNs) loaded with phospholipid complexes (PCs) were prepared by the modified emulsion/solvent evaporation method. DS could be solubilized effectively in the organic solvents with the existence of phospholipid and apparent partition coefficient of DS in PCs increased significantly. X-ray diffraction analysis suggested that DS in PCs was either molecularly dispersed or in an amorphous form. However, no significant difference was observed between the Fourier transform infrared spectroscopy (FT-IR) spectra of physical mixture and that of PCs. Particles with small sizes, narrow polydispersity indexes and high entrapment efficiencies could be obtained with the addition of PCs. Furthermore, according to the transmission electron microscopy, a core-shell structure was likely to be formed. The presence of PCs caused the change of zeta potential and retarded the drug release of SLNs, which indicated that phospholipid formed multilayers around the solid lipid core of SLNs. Both FT-IR and differential scanning calorimetry analysis also illustrated that some weak interactions between DS and lipid materials might take place during the preparation of SLNs. In conclusion, the model hydrophilic drug-DS can be formulated into the SLNs with the help of PCs.
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.
Green synthesis of gold nanoparticles using a cheap Sphaeranthus indicus extract: Impact on plant cells and the aquatic crustacean Artemia nauplii.

PubMed

Balalakshmi, Chinnasamy; Gopinath, Kasi; Govindarajan, Marimuthu; Lokesh, Ravi; Arumugam, Ayyakannu; Alharbi, Naiyf S; Kadaikunnan, Shine; Khaled, Jamal M; Benelli, Giovanni

2017-08-01

The impact of green-fabricated gold nanoparticles on plant cells and non-target aquatic species is scarcely studied. In this research, we reported an environment friendly technique for the synthesis of gold nanoparticles (Au NPs) using the Sphaeranthus indicus leaf extract. The formation of the metal NPs was characterized by UV-Visible and FT-IR spectroscopy, XRD, SEM and TEM analyses. The UV-Visible spectra of Au NPs showed a surface plasmon resonance peak at 531nm. FT-IR analysis indicated functional bio-molecules associated with Au NPs formation. The crystalline nature of Au nanoparticles was confirmed by their XRD diffraction pattern. TEM revealed the spherical shape with a mean particle size of 25nm. Au NPs was tested at 0, 1, 3, 5, 7 and 10% doses in mitotic cell division assays, pollen germination experiments, and in vivo toxicity trials against the aquatic crustacean Artemia nauplii. Au NPs did not show any toxic effects on plant cells and aquatic invertebrates. Notably, Au NPs promoted mitotic cell division in Allium cepa root tip cells and germination of Gloriosa superba pollen grains. Au NPs showed no mortality on A. nauplii, all the tested animals showed 100% survivability. Therefore, these Au NPs have potential applications in the development of pollen germination media and plant tissue culture. Copyright © 2017 Elsevier B.V. All rights reserved.
Biocompatibility assessment of SiO2-TiO2 composite powder on MG63 osteoblast cell lines for orthopaedic applications.

PubMed

Chellappa, Maniickam; Thejaswini, Bezawada; Vijayalakshmi, Uthirapathy

2017-02-01

The objective of this study is to evaluate the biocompatibility of composite powder consisting of silica and titania (SiO 2 -TiO 2 ) for biomedical applications. The advancement of nanoscience and nanotechnology encourages researchers to actively participate in reinvention of existing materials with improved physical, chemical and biological properties. Hence, a composite/hybrid material has given birth of new materials with intriguing properties. In the present investigation, SiO 2 -TiO 2 composite powder was synthesised by sol-gel method and the prepared nanocomposite was characterised for its phase purity, functional groups, surface topography by powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR) and scanning electron microscopy. Furthermore, to understand the adverse effects of composite, biocompatibility test was analysed by cell culture method using MG63 osteoblast cell lines as a basic screening method. From the results, it was observed that typical Si-O-Ti peaks in FT-IR confirms the formation of composite and the crystallinity of the composite powder was analysed by XRD analysis. Further in vitro biocompatibility and acridine orange results have indicated better biocompatibility at different concentrations on osteoblast cell lines. On the basis of these observations, we envision that the prepared silica-titania nanocomposite is an intriguing biomaterial for better biomedical applications.
Biocompatible interpolymer complex matrix tablets - an oral sustained release class-III antidiabetic drug

NASA Astrophysics Data System (ADS)

Ershadul Haque, S. K.; Sheela, A.

2017-11-01

Development of sustained release formulations of Metformin hydrochloride (Met) having low bioavailability and short half-life is one of the frontier areas of research towards achieving novel drug delivery systems. Towards the same, we have prepared interpolymer complexes (IPCs) of chitosan (CH) and two different viscosity grades of hydroxypropyl methylcellulose - HPMC (K4M and K100M) in various ratios, say, 4:6, 2:8, 1:9, respectively. The IPCs are characterized by Fourier transform infrared spectroscopy (FT-IR) and Thermo gravimetric analysis (TGA) techniques. Drug compatibility study is carried out by FT-IR and powder X-ray diffraction (XRD) techniques. The physical properties and drug content of formulated tablets are evaluated and found to be optimum. In addition, in vitro drug release kinetics is carried out at two different pH, say, 1.2 and 6.8. The release pattern from different polymeric matrices is shown in figure below: a) Chitosan, HPMC K4M and HPMC K100M b) IPCs of CH/HPMC K4M in [2:3, 1:4 and 1:9 ratios] c) IPCs of CH/HPMC K100M in [2:3, 1:4 and 1:9 ratios]. From the study, it has been observed that the drug release is sustained for a period of 12h in 1:9 ratio of CH: K100M IPC due to the formation of complex network matrix.
In vitro and in vivo studies on a novel solid dispersion of repaglinide using polyvinylpyrrolidone as the carrier.

PubMed

Yin, Li-Fang; Huang, Shi-Jing; Zhu, Chun-Li; Zhang, Shu-Hui; Zhang, Qiang; Chen, Xi-Jing; Liu, Qing-Wang

2012-11-01

In order to improve the dissolution and absorption of the water insoluble drug repaglinide, a solid dispersion was developed by solvent method using polyvinylpyrrolidone K30 (PVP K30) as the hydrophilic carrier for the first time. Studies indicated that both solubility and the dissolution rate of repaglinide were significantly increased in the solid dispersion system compared with that of repaglinide raw material or physical mixtures. The repaglinide solid dispersions with PVP K30 solid state was characterized by polarizing microscopy, differential scanning calorimetry (DSC), X-ray diffraction (XRD), and Fourier transform infrared spectroscopy (FT-IR). DSC and XRD studies indicated that repaglinide existed in an amorphous form in the solid dispersion. FT-IR analysis demonstrated the presence of intermolecular hydrogen bonding between repaglinide and PVP K30 in the solid dispersion. In the in situ gastrointestinal perfusion experiment, solid dispersion was shown to remarkably enhance the absorption of repaglinide in stomach and all segments of intestine. In vivo pharmacokinetic study in rats showed that immediate and complete release of repaglinide from the solid dispersion resulted in rapid absorption that significantly increased the bioavailability and the maximum plasma concentration over repaglinide raw material. These results demonstrated PVP K30 was an appropriate carrier for solid dispersion of repaglinide, with increased dissolution and oral absorption.
Immobilization of pectinase onto Fe3O4@SiO2-NH2 and its activity and stability.

PubMed

Fang, Gang; Chen, Honggao; Zhang, Yunpeng; Chen, Anqing

2016-07-01

Fe3O4 magnetic nanometer particles (MNPS) with a diameter of 30-40nm and coated by ammoniated silicon dioxides were developed by sol-gel method. The X-ray diffraction (XRD) pattern indicates that the Fe3O4 is wrapped in the amorphous SiO2, and the Fourier-transform infrared spectroscopy (FT-IR) analysis confirmed the NH2 group had been successfully introduced onto the surface of Fe3O4@SiO2 nanoparticles. The main factors related to the immobilization process of pectinase onto the magnetic support were optimized by multi-factor orthogonal experiments, and the recommended combination is that 3% glutaraldehyde (coupling agent), pH=8.0, 50°C, and cross-linking time 8h. Scanning electron microscope (SEM) and FT-IR analyses confirmed that the pectinase had been immobilized onto the surface of the amino modified nanoparticles. The storage stability and reusability of the pectinase were enhanced by the immobilization that 64.4% of the total starting activity was retrieved after 7 recycling batches and only about 21.1% of the total activity was lost after 30-day storage. For the application of the immobilized pectinase, the optimal pH and temperature were 8.5 and 55°C, respectively. Copyright © 2016 Elsevier B.V. All rights reserved.
Attenuated Total Reflection Fourier Transform Infrared (ATR FT-IR) Spectroscopy as a Forensic Method to Determine the Composition of Inks Used to Print the United States One-cent Blue Benjamin Franklin Postage Stamps of the 19th Century.

PubMed

Brittain, Harry G

2016-01-01

Through the combined use of infrared (IR) absorption spectroscopy and attenuated total reflectance (ATR) sampling, the composition of inks used to print the many different types of one-cent Benjamin Franklin stamps of the 19th century has been established. This information permits a historical evaluation of the formulations used at various times, and also facilitates the differentiation of the various stamps from each other. In two instances, the ink composition permits the unambiguous identification of stamps whose appearance is identical, and which (until now) have only been differentiated through estimates of the degree of hardness or softness of the stamp paper, or through the presence or absence of a watermark in the paper. In these instances, the use of ATR Fourier transform infrared spectroscopy (FT-IR) spectroscopy effectively renders irrelevant two 100-year-old practices of stamp identification. Furthermore, since the use of ATR sampling makes it possible to obtain the spectrum of a stamp still attached to its cover, it is no longer necessary to identify these blue Franklin stamps using their cancellation dates. © The Author(s) 2015.
Synthesis, photoluminescence and Magnetic properties of iron oxide (α-Fe2O3) nanoparticles through precipitation or hydrothermal methods

NASA Astrophysics Data System (ADS)

Lassoued, Abdelmajid; Lassoued, Mohamed Saber; Dkhil, Brahim; Ammar, Salah; Gadri, Abdellatif

2018-07-01

In this work the iron oxide (α-Fe2O3) nanoparticles are synthesized using two different methods: precipitation and hydrothermal. Size, structural, optical and magnetic properties were determined and compared using X-ray diffraction (XRD), Transmission Electron Microscopy (TEM), Scanning Electron Microscopy (SEM), Fourier Transform Infra-Red (FT-IR), Raman spectroscopy, Differential Thermal Analysis (DTA), Thermogravimetric Analysis (TGA), Ultraviolet-Visible (UV-Vis) analysis, Superconducting QUantum Interference Device (SQUID) magnetometer and Photoluminescence (PL). XRD data further revealed a rhombohedral (hexagonal) structure with the space group (R-3c) and showed an average size of 21 nm for hydrothermal samples and 33 nm for precipitation samples which concorded with TEM and SEM images. FT-IR confirms the phase purity of the nanoparticles synthesized. The Raman spectroscopy was used not only to prove that we have synthesized pure α-Fe2O3 but also to identify their phonon modes. The TGA showed three mass losses, whereas DTA resulted in three endothermic peaks. The decrease in the particle size of hematite of 33 nm for precipitation samples to 21 nm for hydrothermal samples is responsible for increasing the optical band gap of 1.94-2.10 eV where, the relation between them is inverse relationship. The products exhibited the attractive magnetic properties with good saturation magnetization, which were examined by a SQUID magnetometer. Photoluminescence measurements showed a strong emission band at 450 nm. Pure hematite prepared by hydrothermal method has smallest size, best crystallinity, highest band gap and best value of saturation magnetization compared to the hematite elaborated by the precipitation method.
Improving antiproliferative effect of the anticancer drug cytarabine on human promyelocytic leukemia cells by coating on Fe3O4@SiO2 nanoparticles.

PubMed

Shahabadi, Nahid; Falsafi, Monireh; Mansouri, Kamran

2016-05-01

In this study, Fe3O4@SiO2-cytarabine magnetic nanoparticles (MNPs) were prepared via chemical coprecipitation reaction and coating silica on the surface of Fe3O4 MNPs by Stöber method via sol-gel process. The surface of Fe3O4@SiO2 MNPs was modified by an anticancer drug, cytarabine. The structural properties of the samples were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), Zetasizer analyzer, and transmission electron microscopy (TEM). The results indicated that the crystalline phase of iron oxide NPs was magnetite (Fe3O4) and the average sizes of Fe3O4@SiO2-cytarabine MNPs were about 23 nm. Also, the surface characterization of Fe3O4@SiO2-cytarabine MNPs by FT-IR showed that successful coating of Fe3O4 NPs with SiO2 and binding of cytarabine drug onto the surface of Fe3O4@SiO2 MNPs were through the hydroxyl groups of the drug. The in vitro cytotoxic activity of Fe3O4@SiO2-cytarabine MNPs was investigated against cancer cell line (HL60) in comparison with cytarabine using MTT colorimetric assay. The obtained results showed that the effect of Fe3O4@SiO2-cytarabine magnetic nanoparticles on the cell lines were about two orders of magnitude higher than that of cytarabine. Furthermore, in vitro DNA binding studies were investigated by UV-vis, circular dichroism, and fluorescence spectroscopy. The results for DNA binding illustrated that DNA aggregated on Fe3O4@SiO2-cytarabine MNPs via groove binding. Copyright © 2016 Elsevier B.V. All rights reserved.
Crystal structures, Hirshfeld surface analysis, thermal behavior and dielectric properties of a new organic-inorganic hybrid [C6H10(NH3)2]Cu2Cl8

NASA Astrophysics Data System (ADS)

Salah, Najet; Hamdi, Besma; Bouzidia, Nabaa; Salah, Abdelhamid Ben

2017-12-01

A novel organic-inorganic hybrid sample [C6H10(NH3)2]Cu2Cl8 has been prepared under mild hydrothermal conditions and characterized by single crystal X-ray diffraction, Hirshfeld surface analysis, FT-IR,NMR and UV-Vis spectroscopies, differential scanning calorimetric and dielectric measurement. It is crystallized in the monoclinic system with P21/c space group. The cohesion and stabilization of the structure are provided by the hydrogen bond interactions, (Nsbnd H⋯Cl and Csbnd H⋯Cl), between [C6H10(NH3)2]2+ cation and [Cu2Cl8]2- anion. The Hirschfeld surface analysis has been performed to explore the behavior of these weak interactions. The presence of different functional groups and the nature of their vibrations were identified by FT-IR and Solid state NMR. The thermal study revealed that this compound undergoes two structural phase transitions around 353 and 376 K. Electrical measurements of our compounds have been investigated using complex impedance spectroscopy (CIS) in the frequency and temperature range 331-399 K and 200 Hz-5 MHz, respectively. The AC conductivity is explained using the correlated barrier hopping model (CBH) conduction mechanism. The nature of DC conductivity variation suggests Arrhenius type of electrical conductivity. A relationship between crystal structure and ionic conductivity was established and discussed. Finally, the real and imaginary parts of the permittivity constant are analyzed with the Cole-Cole formalism and the optical spectra indicate that the compound has a direct band gap (3.14 eV) due to direct transition. The wide band gap is due to low defect concentration in the grown crystal, which is more useful for the laser/optical applications.
Synthesis, crystal structure, vibrational spectroscopy, optical properties and theoretical studies of a new organic-inorganic hybrid material: [((CH3)2NH2)(+)]6·[(BiBr6)(3-)]2.

PubMed

Ben Ahmed, A; Feki, H; Abid, Y

2014-12-10

A new organic-inorganic hybrid material, [((CH3)2NH2)(+)]6·[(BiBr6)(3-)]2, has been synthesized and characterized by X-ray diffraction, FT-IR, Raman spectroscopy and UV-Visible absorption. The studied compound crystallizes in the triclinic system, space group P1¯ with the following parameters: a=8.4749(6)(Å), b=17.1392(12)(Å), c=17.1392(12)(Å), α=117.339(0)°, β=99.487(0)°, γ=99.487(0)° and Z=2. The crystal lattice is composed of a two discrete (BiBr6)(3-) anions surrounded by six ((CH3)2NH2)(+) cations. Complex hydrogen bonding interactions between (BiBr6)(3-) and organic cations from a three-dimensional network. Theoretical calculations were performed using density functional theory (DFT) for studying the molecular structure, vibrational spectra and optical properties of the investigated molecule in the ground state. The full geometry optimization of designed system is performed using DFT method at B3LYP/LanL2DZ level of theory using the Gaussian03. The optimized geometrical parameters obtained by DFT calculations are in good agreement with single crystal XRD data. The vibrational spectral data obtained from FT-IR and Raman spectra are assigned based on the results of the theoretical calculations. The energy and oscillator strength calculated by Time-Dependent Density Functional Theory (TD-DFT) results complements with the experimental findings. The simulated spectra satisfactorily coincide with the experimental UV-Visible spectrum. The results show good consistent with the experiment and confirm the contribution of metal orbital to the HOMO-LUMO boundary. Copyright © 2014 Elsevier B.V. All rights reserved.
Production of polyimide ceria nanocomposites by development of molecular hook technology in nano-sonochemistry.

PubMed

Hatami, Mehdi

2018-06-01

Poly(amic acid), the precursor of polyimide (PI), was used for the preparation of PI/CeO 2 nanocomposites (NC)s by ultrasonic assisted technique via insertion of the surface modified CeO 2 nanoparticles (NP)s into PI matrix. In the preparation stages, in the first, the modifications of CeO 2 NPs by using hexadecyltrimethoxysilane (HDTMS) as a binder were targeted using ultrasonic waves. In the second step, newly designed PI structure was formed from the sonochemical imidization process as a molecular hook. In this step two different reactions were occurred. The acetic acid elimination reaction in the main chain of macromolecule, and the acetylation reaction in the side chains of poly(amic acid) were accomplished. By acetylation process the hook structure was created for trapping of the modified nanoparticles. In the final step the preparation of PI NCs were achieved by sonochemical process. The structural and thermal properties of pure PI and PI/CeO 2 NCs were studied by several techniques such as fourier transform infrared spectroscopy (FT-IR), nuclear magnetic resonance spectroscopy (NMR), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), atomic force microscopy (AFM), X-ray diffraction (XRD), and thermal analyses. FT-IR and 1 H NMR spectra confirmed the success in preparation of PI matrix. The FE-SEM, TEM, and AFM analyses showed the uniform distribution of CeO 2 NPs in PI matrix. The XRD patterns of NCs show the presence of crystalline CeO 2 NPs in amorphous PI matrix. The thermal analysis results reveal that, with increases in the content of CeO 2 NPs in PI matrix, the thermally stability factors of samples were improved. Copyright © 2018 Elsevier B.V. All rights reserved.
Photocatalytic activity of undoped and Ag-doped TiO{sub 2}-supported zeolite for humic acid degradation and mineralization

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

Lazau, C.; Ratiu, C.; National Institute for Research and Development in Microtechnologies, Erou Iancu Nicolae Street, 077190 Bucharest

2011-11-15

Highlights: {yields} Hybrid materials based on natural zeolite and TiO{sub 2} obtained by solid-state reaction. {yields} XRD proved the presence of anatase form of undoped and Ag-doped TiO{sub 2} onto zeolite. {yields} FT-IR spectra evidenced the presence on TiO{sub 2} bounded at the zeolite network. {yields} Ag-doped TiO{sub 2} onto zeolitic matrix exhibited an enhanced photocatalytic activity. -- Abstract: The hybrid materials based on natural zeolite and undoped and Ag-doped TiO{sub 2}, i.e., Z-Na-TiO{sub 2} and Z-Na-TiO{sub 2}-Ag, were successfully synthesized by solid-state reaction in microwave-assisted hydrothermal conditions. Undoped TiO{sub 2} and Ag-doped TiO{sub 2} nanocrystals were previously synthesized bymore » sol-gel method. The surface characterization of undoped TiO{sub 2}/Ag-doped TiO{sub 2} and natural zeolite hybrid materials has been investigated by X-ray diffraction, DRUV-VIS spectroscopy, FT-IR spectroscopy, BET analysis, SEM microscopy and EDX analysis. The results indicated that anatase TiO{sub 2} is the dominant crystalline type as spherical form onto zeolitic matrix. The presence of Ag into Z-Na-TiO{sub 2}-Ag was confirmed by EDX analysis. The DRUV-VIS spectra showed that Z-Na-TiO{sub 2}-Ag exhibited absorption within the range of 400-500 nm in comparison with Z-Na-TiO{sub 2} catalyst. The enhanced photocatalytic activity of Z-Na-TiO{sub 2}-Ag catalyst is proved through the degradation and mineralization of humic acid under ultraviolet and visible irradiation.« less
The role of extracellular DNA in uranium precipitation and biomineralisation.

PubMed

Hufton, Joseph; Harding, John H; Romero-González, Maria E

2016-10-26

Bacterial extra polymeric substances (EPS) have been associated with the extracellular precipitation of uranium. Here we report findings on the biomineralisation of uranium, with extracellular DNA (eDNA) used as a model biomolecule representative of EPS. The complexation and precipitation of eDNA with uranium were investigated as a function of pH, ionic strength and varying concentrations of reactants. The role of phosphate moieties in the biomineralisation mechanism was studied by enzymatically releasing phosphate (ePO 4 ) from eDNA compared to abiotic phosphate (aPO 4 ). The eDNA-uranium precipitates and uranium minerals obtained were characterised by Attenuated Total Reflectance-Fourier Transform Infrared (ATR-FT-IR) spectroscopy, Scanning Electron Microscopy-Energy Dispersive X-Ray analysis (SEM-EDX), X-Ray Powder Diffraction (XRD) and X-Ray Photoelectron Spectroscopy (XPS). ATR-FT-IR showed that at pH 5, the eDNA-uranium precipitation mechanism was predominantly mediated by interactions with phosphate moieties from eDNA. At pH 2, the uranium interactions with eDNA occur mainly through phosphate. The solubility equilibrium was dependent on pH with the formation of precipitate reduced as the pH increased. The XRD data confirmed the formation of a uranium phosphate precipitate when synthesised using ePO 4 . XPS and SEM-EDX studies showed the incorporation of carbon and nitrogen groups from the enzymatic orthophosphate hydrolysis on the obtained precipitated. These results suggested that the removal of uranium from solution occurs via two mechanisms: complexation by eDNA molecules and precipitation of a uranium phosphate mineral of the type (UO 2 HPO 4 )·xH 2 O by enzymatic orthophosphate hydrolysis. This demonstrated that eDNA from bacterial EPS is a key contributor to uranium biomineralisation.
Synthesis, structural characterization and luminescence properties of 1-carboxymethyl-3-ethylimidazolium chloride

DOE PAGES

Prodius, Denis; Wilk-Kozubek, Magdalena; Mudring, Anja -Verena

2018-05-08

A microcrystalline carboxyl-functionalized imidazolium chloride, namely 1-carboxymethyl-3-ethylimidazolium chloride, C 7H 11N 2O 2 +·Cl –, has been synthesized and characterized by elemental analysis, attenuated total reflectance Fourier transform IR spectroscopy (ATR-FT-IR), single-crystal X-ray diffraction, thermal analysis (TGA/DSC), and photoluminescence spectroscopy. In the crystal structure, cations and anions are linked by C—H...Cl and C—H...O hydrogen bonds to create a helix along the [010] direction. Adjacent helical chains are further interconnected through O—H...Cl and C—H...O hydrogen bonds to form a (101¯) layer. Finally, neighboring layers are joined together via C—H...Cl contacts to generate a three-dimensional supramolecular architecture. Thermal analyses reveal that themore » compound melts at 449.7 K and is stable up to 560.0 K under a dynamic air atmosphere. Photoluminescence measurements show that the compound exhibits a blue fluorescence and a green phosphorescence associated with spin-allowed ( 1π← 1π*) and spin-forbidden ( 1π← 3π*) transitions, respectively. As a result, the average luminescence lifetime was determined to be 1.40 ns for the short-lived ( 1π← 1π*) transition and 105 ms for the long-lived ( 1π← 3π*) transition.« less

Synthesis, structural characterization and luminescence properties of 1-carboxymethyl-3-ethylimidazolium chloride

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

Prodius, Denis; Wilk-Kozubek, Magdalena; Mudring, Anja -Verena

A microcrystalline carboxyl-functionalized imidazolium chloride, namely 1-carboxymethyl-3-ethylimidazolium chloride, C 7H 11N 2O 2 +·Cl –, has been synthesized and characterized by elemental analysis, attenuated total reflectance Fourier transform IR spectroscopy (ATR-FT-IR), single-crystal X-ray diffraction, thermal analysis (TGA/DSC), and photoluminescence spectroscopy. In the crystal structure, cations and anions are linked by C—H...Cl and C—H...O hydrogen bonds to create a helix along the [010] direction. Adjacent helical chains are further interconnected through O—H...Cl and C—H...O hydrogen bonds to form a (101¯) layer. Finally, neighboring layers are joined together via C—H...Cl contacts to generate a three-dimensional supramolecular architecture. Thermal analyses reveal that themore » compound melts at 449.7 K and is stable up to 560.0 K under a dynamic air atmosphere. Photoluminescence measurements show that the compound exhibits a blue fluorescence and a green phosphorescence associated with spin-allowed ( 1π← 1π*) and spin-forbidden ( 1π← 3π*) transitions, respectively. As a result, the average luminescence lifetime was determined to be 1.40 ns for the short-lived ( 1π← 1π*) transition and 105 ms for the long-lived ( 1π← 3π*) transition.« less
FT-IR, FT-Raman spectra and DFT calculations of melaminium perchlorate monohydrate

NASA Astrophysics Data System (ADS)

Kanagathara, N.; Marchewka, M. K.; Drozd, M.; Renganathan, N. G.; Gunasekaran, S.; Anbalagan, G.

2013-08-01

Melaminium perchlorate monohydrate (MPM), an organic material has been synthesized by slow solvent evaporation method at room temperature. Powder X-ray diffraction analysis confirms that MPM crystal belongs to triclinic system with space group P-1. FTIR and FT Raman spectra are recorded at room temperature. Functional group assignment has been made for the melaminium cations and perchlorate anions. Vibrational spectra have also been discussed on the basis of quantum chemical density functional theory (DFT) calculations using Firefly (PC GAMESS) version 7.1 G. Vibrational frequencies are calculated and scaled values are compared with experimental values. The assignment of the bands has been made on the basis of the calculated PED. The Mulliken charges, HOMO-LUMO orbital energies are analyzed directly from Firefly program log files and graphically illustrated. HOMO-LUMO energy gap and other related molecular properties are also calculated. The theoretically constructed FT-IR and FT-Raman spectra of MPM coincide with the experimental one. The chemical structure of the compound has been established by 1H and 13C NMR spectra. No detectable signal was observed during powder test for second harmonic generation.
A comprehensive physicochemical, thermal, and spectroscopic characterization of zinc (II) chloride using X-ray diffraction, particle size distribution, differential scanning calorimetry, thermogravimetric analysis/differential thermogravimetric analysis, ultraviolet-visible, and Fourier transform-infrared spectroscopy

PubMed Central

Trivedi, Mahendra Kumar; Sethi, Kalyan Kumar; Panda, Parthasarathi; Jana, Snehasis

2017-01-01

Objective: Zinc chloride is an important inorganic compound used as a source of zinc and has other numerous industrial applications. Unfortunately, it lacks reliable and accurate physicochemical, thermal, and spectral characterization information altogether. Hence, the authors tried to explore in-depth characterization of zinc chloride using the modern analytical technique. Materials and Methods: The analysis of zinc chloride was performed using powder X-ray diffraction (PXRD), particle size distribution, differential scanning calorimetry (DSC), thermogravimetric analysis/differential thermogravimetric analysis (TGA/DTG), ultraviolet-visible spectroscopy (UV-vis), and Fourier transform-infrared (FT-IR) analytical techniques. Results: The PXRD patterns showed well-defined, narrow, sharp, and the significant peaks. The crystallite size was found in the range of 14.70–55.40 nm and showed average crystallite size of 41.34 nm. The average particle size was found to be of 1.123 (d10), 3.025 (d50), and 6.712 (d90) μm and average surface area of 2.71 m2/g. The span and relative span values were 5.849 μm and 1.93, respectively. The DSC thermogram showed a small endothermic inflation at 308.10°C with the latent heat (ΔH) of fusion 28.52 J/g. An exothermic reaction was observed at 449.32°C with the ΔH of decomposition 66.10 J/g. The TGA revealed two steps of the thermal degradation and lost 8.207 and 89.72% of weight in the first and second step of degradation, respectively. Similarly, the DTG analysis disclosed Tmax at 508.21°C. The UV-vis spectrum showed absorbance maxima at 197.60 nm (λmax), and FT-IR spectrum showed a peak at 511/cm might be due to the Zn–Cl stretching. Conclusions: These in-depth, comprehensive data would be very much useful in all stages of nutraceuticals/pharmaceuticals formulation research and development and other industrial applications. PMID:28405577
A comprehensive physicochemical, thermal, and spectroscopic characterization of zinc (II) chloride using X-ray diffraction, particle size distribution, differential scanning calorimetry, thermogravimetric analysis/differential thermogravimetric analysis, ultraviolet-visible, and Fourier transform-infrared spectroscopy.

PubMed

Trivedi, Mahendra Kumar; Sethi, Kalyan Kumar; Panda, Parthasarathi; Jana, Snehasis

2017-01-01

Zinc chloride is an important inorganic compound used as a source of zinc and has other numerous industrial applications. Unfortunately, it lacks reliable and accurate physicochemical, thermal, and spectral characterization information altogether. Hence, the authors tried to explore in-depth characterization of zinc chloride using the modern analytical technique. The analysis of zinc chloride was performed using powder X-ray diffraction (PXRD), particle size distribution, differential scanning calorimetry (DSC), thermogravimetric analysis/differential thermogravimetric analysis (TGA/DTG), ultraviolet-visible spectroscopy (UV-vis), and Fourier transform-infrared (FT-IR) analytical techniques. The PXRD patterns showed well-defined, narrow, sharp, and the significant peaks. The crystallite size was found in the range of 14.70-55.40 nm and showed average crystallite size of 41.34 nm. The average particle size was found to be of 1.123 ( d 10 ), 3.025 ( d 50 ), and 6.712 ( d 90 ) μm and average surface area of 2.71 m 2 /g. The span and relative span values were 5.849 μm and 1.93, respectively. The DSC thermogram showed a small endothermic inflation at 308.10°C with the latent heat (ΔH) of fusion 28.52 J/g. An exothermic reaction was observed at 449.32°C with the ΔH of decomposition 66.10 J/g. The TGA revealed two steps of the thermal degradation and lost 8.207 and 89.72% of weight in the first and second step of degradation, respectively. Similarly, the DTG analysis disclosed T max at 508.21°C. The UV-vis spectrum showed absorbance maxima at 197.60 nm (λ max ), and FT-IR spectrum showed a peak at 511/cm might be due to the Zn-Cl stretching. These in-depth, comprehensive data would be very much useful in all stages of nutraceuticals/pharmaceuticals formulation research and development and other industrial applications.
Single-source-precursor synthesis of dense SiC/HfC(x)N(1-x)-based ultrahigh-temperature ceramic nanocomposites.

PubMed

Wen, Qingbo; Xu, Yeping; Xu, Binbin; Fasel, Claudia; Guillon, Olivier; Buntkowsky, Gerd; Yu, Zhaoju; Riedel, Ralf; Ionescu, Emanuel

2014-11-21

A novel single-source precursor was synthesized by the reaction of an allyl hydrido polycarbosilane (SMP10) and tetrakis(dimethylamido)hafnium(iv) (TDMAH) for the purpose of preparing dense monolithic SiC/HfC(x)N(1-x)-based ultrahigh temperature ceramic nanocomposites. The materials obtained at different stages of the synthesis process were characterized via Fourier transform infrared (FT-IR) as well as nuclear magnetic resonance (NMR) spectroscopy. The polymer-to-ceramic transformation was investigated by means of MAS NMR and FT-IR spectroscopy as well as thermogravimetric analysis (TGA) coupled with in situ mass spectrometry. Moreover, the microstructural evolution of the synthesized SiHfCN-based ceramics annealed at different temperatures ranging from 1300 °C to 1800 °C was characterized by elemental analysis, X-ray diffraction, Raman spectroscopy and transmission electron microscopy (TEM). Based on its high temperature behavior, the amorphous SiHfCN-based ceramic powder was used to prepare monolithic SiC/HfC(x)N(1-x)-based nanocomposites using the spark plasma sintering (SPS) technique. The results showed that dense monolithic SiC/HfC(x)N(1-x)-based nanocomposites with low open porosity (0.74 vol%) can be prepared successfully from single-source precursors. The average grain size of both HfC0.83N0.17 and SiC phases was found to be less than 100 nm after SPS processing owing to a unique microstructure: HfC0.83N0.17 grains were embedded homogeneously in a β-SiC matrix and encapsulated by in situ formed carbon layers which acted as a diffusion barrier to suppress grain growth. The segregated Hf-carbonitride grains significantly influenced the electrical conductivity of the SPS processed monolithic samples. While Hf-free polymer-derived SiC showed an electrical conductivity of ca. 1.8 S cm(-1), the electrical conductivity of the Hf-containing material was analyzed to be ca. 136.2 S cm(-1).
Nitrogen-doped carbon dots originating from unripe peach for fluorescent bioimaging and electrocatalytic oxygen reduction reaction.

PubMed

Atchudan, Raji; Edison, Thomas Nesakumar Jebakumar Immanuel; Lee, Yong Rok

2016-11-15

This paper reports the robust hydrothermal synthesis of nitrogen doped carbon dots (N-CDs) using the unripe fruit of Prunus persica (peach) as the carbon precursor and aqueous ammonia as the nitrogen source. The optical properties of synthesized N-CDs were characterized by ultraviolet visible (UV-Vis) and fluorescence spectroscopy techniques. The synthesized N-CDs were emitted blue light when excitated with a portable UV lamp. The materials with the optical properties were characterized further by high resolution transmission electron microscope (HRTEM), X-ray diffraction (XRD), Raman, Fourier transform infrared (FT-IR) and X-ray photoelectron spectroscopy (XPS). The mean size of the N-CDs was approximately 8nm, as calculated from the HRTEM image. The d-spacing of N-CDs, calculated using Bragg law, was approximately 0.21nm, which was consistent with the interlayer distance calculated from the HRTEM image. FT-IR spectroscopy and XPS revealed the presence of the phytoconstituents functionalities of peach fruit over the N-CDs surface and a high level of nitrogen doping on carbon dots (CDs) was confirmed by XPS studies. These results suggest that the unripe fruit extract of peach is an ideal candidate for the preparation of N-CDs. The resulting N-CDs showed excellent optical properties in water. The synthesized N-CDs exhibited a high fluorescence quantum yield and low cytotoxicity, and can be used as fluorescence imaging probes. In addition, the N-CDs were catalytically activite towards the oxygen reduction reaction (ORR). The N-CDs exhibited good catalytic activity in an alkaline medium (0.1M KOH) with a remarkable ORR of approximately 0.72V vs reversible hydrogen electrode (RHE), and O2 reduction follows mainly a 2 electron pathway by being reduced to hydrogen peroxide. The 2-electron reduction pathway is used in industry for H2O2 production. Copyright © 2016 Elsevier Inc. All rights reserved.
Hybride ZnCdCrO embedded aminated polyethersulfone nanocomposites for the development of Hg2+ ionic sensor

NASA Astrophysics Data System (ADS)

Rahman, Mohammed M.; Alenazi, Noof A.; Hussein, Mahmoud A.; Alam, M. M.; Alamry, Khalid A.; Asiri, Abdullah M.

2018-06-01

In this current study, ‑NH2 functions are introduced on Polyethersulfone (PES) by a nitration reaction then a reduction reaction to fabricate PES-NH2 materials with a better hydrophilicity property. The structure of PES-NH2 was first confirmed using proton nuclear magnetic resonance spectroscopy (1H-NMR) and Fourier transform infrared (FT-IR) spectroscopy. Then, the resultant polymer was doped with different concentrations of ZnCdCrO nanocomposites. The polymeric nanocomposites materials were characterized using FT-IR, x-ray powder diffraction (XRD), thermal analysis (TA), and energy dispersive x-ray (EDX) spectroscopy while the morphology was investigated using scanning electron microscopy (SEM). The performance PES-NH2-ZnCdCrO nanocomposites was investigated by sensor-probe towards the selective detection of Hg2+. The results showed the excellent thermal properties of PES-NH2-ZnCdCrO nanocomposites in comparison with non-doped polymer (PES-NH2). Here, Hg2+ ionic sensor was prepared using a flat glassy carbon electrode (GCE) coated with a thin-layer of PES-NH2-ZnCdCrO nanocomposites (20%) with nafion conducting nafion binder (5%). To evaluate the analytical performances of Hg2+ ion sensor, a calibration curve was drawn by plotting the current versus concentration. The sensitivity (0.6566 μAμM-1 cm‑2) and detection limit (14.46 ± 0.72 pM) are calculated using the slope of the calibration curve. It was determined the linearity (r2 = 0.9941) over the large linear dynamic range (LDR) (0.1 nM to 0.1 mM). Thus, this research approach might be an important route to the selective detection of environmental toxin (Hg2+ cation) from the aqueous system in broad scales for the safety of health care, environmental, and aquatic fields.
Selective Iron(III) ion uptake using CuO-TiO2 nanostructure by inductively coupled plasma-optical emission spectrometry

PubMed Central

2012-01-01

Background CuO-TiO2 nanosheets (NSs), a kind of nanomaterials is one of the most attracting class of transition doped semiconductor materials due to its interesting and important optical, electrical, and structural properties and has many technical applications, such as in metal ions detection, photocatalysis, Chemi-sensors, bio-sensors, solar cells and so on. In this paper the synthesis of CuO-TiO2 nanosheets by the wet-chemically technique is reported. Methods CuO-TiO2 NSs were prepared by a wet-chemical process using reducing agents in alkaline medium and characterized by UV/vis., FT-IR spectroscopy, X-ray photoelectron spectroscopy (XPS), powder X-ray diffraction (XRD), and field-emission scanning electron microscopy (FE-SEM) etc. Results The structural and optical evaluation of synthesized NSs were measured by XRD pattern, Fourier transform infrared (FT-IR) and UV–vis spectroscopy, respectively which confirmed that the obtained NSs are well-crystalline CuO-TiO2 and possessing good optical properties. The morphological analysis of CuO-TiO2 NSs was executed by FE-SEM, which confirmed that the doped products were sheet-shaped and growth in large quantity. Here, the analytical efficiency of the NSs was applied for a selective adsorption of iron(III) ion prior to detection by inductively coupled plasma-optical emission spectrometry (ICP-OES). The selectivity of NSs towards various metal ions, including Au(III), Cd(II), Co(II), Cr(III), Fe(III), Pd(II), and Zn(II) was analyzed. Conclusions Based on the selectivity study, it was confirmed that the selectivity of doped NSs phase was the most towards Fe(III) ion. The static adsorption capacity for Fe(III) was calculated to be 110.06 mgg−1. Results from adsorption isotherm also verified that the adsorption process was mainly monolayer-adsorption onto a surface containing a finite number of CuO-TiO2 NSs adsorption sites. PMID:23244218
Rapid discrimination of three Uighur medicine of Eremurus by FT-IR combined with 2DCOS-IR

NASA Astrophysics Data System (ADS)

Zhu, Yun; Xu, Chang-hua; Huang, Jian; Li, Guo-yu; Zhou, Qun; Liu, Xin-Hu; Sun, Su-qin; Wang, Jin-hui

2014-07-01

As complicated mixture systems, traditional Chinese medicines (TCMs) are difficult to be identified and discriminated, especially for the drug samples originated from the same source. In this study, a tri-step infrared spectroscopy method, i.e., conventional infrared spectroscopy (FT-IR) combined with second derivatives spectra and two-dimensional correlation infrared spectroscopy (2DCOS-IR), was employed to study and identify three Uighur drugs of Eremurus in Xinjiang, i.e. Eremurus altaicus (Pall.) Stev (AET), E. inderiensis (M.Bieb.)Regel(CB), E. anisopterus (Kar.et Kir.) Regel(YC). It was founded that the conventional IR spectra of the three species Eremurus were very similar based on the peak positions and shapes, indicating that the three had similar chemical profiles. On the basis of the different IR spectra of reference compounds and microscopic identification, the roots of YC, CB and AET all have comparable amount of calcium oxalate. The second derivative spectra of Eremurus enhanced the spectral resolution and amplified the small differences, especially at about 1468 cm-1, 1454 cm-1, and 1164 cm-1, and subsequently provided some dissimilarity in their calcium oxalate content. AET has relatively higher content of calcium oxalate but the lower content of anthraquinones. Moreover, the 2D-IR spectra revealed tiny differences among the three species by providing dynamic structural information of their chemical components in a more direct and visual way. The differences embodied mainly on the intensity of the auto-peaks at 971 cm-1, 1008 cm-1, 1468 cm-1 and 1578 cm-1. As a result, it was demonstrated that the macroscopic IR fingerprint method could discriminate the three similar Uighur drugs, YC, CB and AET.
Analysis of Trans Fat in Edible Oils with Cooking Process

PubMed Central

Song, Juhee; Park, Joohyeok; Jung, Jinyeong; Lee, Chankyu; Gim, Seo Yeoung; Ka, HyeJung; Yi, BoRa; Kim, Mi-Ja; Kim, Cho-il

2015-01-01

Trans fat is a unsaturated fatty acid with trans configuration and separated double bonds. Analytical methods have been introduced to analyze trans fat content in foods including infrared (IR) spectroscopy, gas chromatography (GC), Fourier transform-infrared (FT-IR) spectroscopy, reverses-phase silver ion high performance liquid chromatography, and silver nitrate thin layer chromatography. Currently, FT-IR spectroscopy and GC are mostly used methods. Trans fat content in 6 vegetable oils were analyzed and processing effects including baking, stir-frying, pan-frying, and frying on the formation of trans fat in corn oil was evaluated by GC. Among tested vegetable oils, corn oil has 0.25 g trans fat/100 g, whereas other oils including rapeseed, soybean, olive, perilla, and sesame oils did not have detectable amount of trans fat content. Among cooking methods, stir-frying increased trans fat in corn oil whereas baking, pan-frying, and frying procedures did not make changes in trans fat content compared to untreated corn oils. However, the trans fat content was so low and food label can be declared as ‘0’ trans based on the regulation of Ministry of Food ad Drug Safety (MFDS) (< 2 g/100 g edible oil). PMID:26483890
A novel green synthesis of Fe3O4-Ag core shell recyclable nanoparticles using Vitis vinifera stem extract and its enhanced antibacterial performance

NASA Astrophysics Data System (ADS)

Venkateswarlu, Sada; Natesh Kumar, B.; Prathima, B.; Anitha, K.; Jyothi, N. V. V.

2015-01-01

We described a novel and eco-friendly method for preparing Fe3O4-Ag core shell nanoparticles (CSNPs) with high magnetism and potent antibacterial activity. The Fe3O4-Ag CSNPs were obtained using waste material of Vitis vinifera (grape) stem extract as the green solvent, reducing and capping agent. The result recorded from X-ray powder diffraction (XRD), UV-vis spectrum, energy dispersive spectroscopy (EDS), Fourier transform infrared spectroscopy (FT-IR) supports the biosynthesis and characterization of Fe3O4-Ag CSNPs. From transmission electron microscopy (TEM) the size of the Fe3O4-Ag nanoparticles was measured below 50 nm; high-resolution TEM (HRTEM) indicates the core shell structure; and selected area electron diffraction (SAED) has revealed polycrystalline nature. Vibrating sample magnetometer (VSM) shows the ferromagnetic nature of Fe3O4-Ag CSNPs at room temperature with saturation magnetization of 15.74 emu/g. Further, these biogenic nanoparticles were highly hazardous to microorganisms. The antibacterial activity of biogenic Fe3O4-Ag CSNPs showed potent inhibitory activity against both Gram-positive and Gram-negative pathogens. These nanoparticles may also be reusable because of its excellent ferromagnetic property.
FT-IR spectroscopy as a tool for rapid identification and intra-species characterization of airborne filamentous fungi.

PubMed

Fischer, Guido; Braun, Silvia; Thissen, Ralf; Dott, Wolfgang

2006-01-01

Identification of microfungi is time-consuming due to cultivation and microscopic examination and can be influenced by the interpretation of the macro- and micro-morphological characters observed. Fungal conidia contain mycotoxins that may be present in bioaerosols and thus the capacity for production of mycotoxins (and allergens) needs to be investigated to create a basis for reliable risk assessment in environmental and occupational hygiene. The present investigation aimed to create a simple but sophisticated method for the preparation of samples and the identification of airborne fungi by FT-IR spectroscopy. The method was suited to reproducibly differentiate Aspergillus and Penicillium species on the generic, the species, and the strain level. There are strong indications that strains of one taxon differing in metabolite production can be reliably distinguished by FT-IR spectroscopy (e.g. Aspergillus parasiticus). On the other hand, species from different taxa being similar in secondary metabolite production showed comparably higher similarities. The results obtained here can serve as a basis for the development of a database for species identification and strain characterization of microfungi. The method presented here will improve and facilitate the risk assessment in case of bioaerosol exposure, as strains with different physiological properties (e.g. toxic, non-toxic) could be differentiated. Moreover, it has the potential to significantly improve the identification of microfungi in various fields of applied microbiological research, e.g. high throughput screening in view of specific physiological properties, biodiversity studies, inventories in environmental microbiology, and quality control measures.
Advanced sampling techniques for hand-held FT-IR instrumentation

NASA Astrophysics Data System (ADS)

Arnó, Josep; Frunzi, Michael; Weber, Chris; Levy, Dustin

2013-05-01

FT-IR spectroscopy is the technology of choice to identify solid and liquid phase unknown samples. The challenging ConOps in emergency response and military field applications require a significant redesign of the stationary FT-IR bench-top instruments typically used in laboratories. Specifically, field portable units require high levels of resistance against mechanical shock and chemical attack, ease of use in restrictive gear, extreme reliability, quick and easy interpretation of results, and reduced size. In the last 20 years, FT-IR instruments have been re-engineered to fit in small suitcases for field portable use and recently further miniaturized for handheld operation. This article introduces the HazMatID™ Elite, a FT-IR instrument designed to balance the portability advantages of a handheld device with the performance challenges associated with miniaturization. In this paper, special focus will be given to the HazMatID Elite's sampling interfaces optimized to collect and interrogate different types of samples: accumulated material using the on-board ATR press, dispersed powders using the ClearSampler™ tool, and the touch-to-sample sensor for direct liquid sampling. The application of the novel sample swipe accessory (ClearSampler) to collect material from surfaces will be discussed in some detail. The accessory was tested and evaluated for the detection of explosive residues before and after detonation. Experimental results derived from these investigations will be described in an effort to outline the advantages of this technology over existing sampling methods.
Secondary cell wall development in cotton fibers as examined with attenuated total reflection Fourier transform infrared spectroscopy

USDA-ARS?s Scientific Manuscript database

Cotton fibers harvested at 18, 20, 24, 28, 32, 36 and 40 days after flowering were examined using attenuated total reflection Fourier transform-infrared (ATR FT-IR) spectroscopy. The selected harvesting points coincide with secondary cell wall (SCW) development in the fibers. Progressive but moderat...
Discrimination between Bacillus and Alicyclobacillus isolates in apple juice by Fourier transform infrared spectroscopy and multivariate analysis.

PubMed

Al-Holy, Murad A; Lin, Mengshi; Alhaj, Omar A; Abu-Goush, Mahmoud H

2015-02-01

Alicyclobacillus is a causative agent of spoilage in pasteurized and heat-treated apple juice products. Differentiating between this genus and the closely related Bacillus is crucially important. In this study, Fourier transform infrared spectroscopy (FT-IR) was used to identify and discriminate between 4 Alicyclobacillus strains and 4 Bacillus isolates inoculated individually into apple juice. Loading plots over the range of 1350 and 1700 cm(-1) reflected the most distinctive biochemical features of Bacillus and Alicyclobacillus. Multivariate statistical methods (for example, principal component analysis and soft independent modeling of class analogy) were used to analyze the spectral data. Distinctive separation of spectral samples was observed. This study demonstrates that FT-IR spectroscopy in combination with multivariate analysis could serve as a rapid and effective tool for fruit juice industry to differentiate between Bacillus and Alicyclobacillus and to distinguish between species belonging to these 2 genera. © 2015 Institute of Food Technologists®
Analysis of a Brazilian baroque sculpture using Raman spectroscopy and FT-IR

NASA Astrophysics Data System (ADS)

Freitas, Renato P.; Ribeiro, Iohanna M.; Calza, Cristiane; Oliveira, Ana L.; Felix, Valter S.; Ferreira, Douglas S.; Pimenta, André R.; Pereira, Ronaldo V.; Pereira, Marcelo O.; Lopes, Ricardo T.

2016-02-01

In this study, samples were taken from the sculpture of Our Lady of Sorrows and analyzed by Raman spectroscopy and FT-IR. This sculpture has been dated to the early eighteenth century. Samples were also examined using optical microscopy and Energy Dispersive Spectroscopy (EDS). Based on chemical analysis, the pigments vermilion [HgS], massicot [PbO] and azurite [Cu3(CO3)2(OH)2] were found in the sculpture polychrome. The results indicate that the green polychrome of the sculpture's mantle comes from the blending of massicot and azurite. Because the literature reports that the mantle of the Our Lady of Sorrows sculpture is blue, the mixing of these pigments results from a production error. The results also indicate the presence of Au in the sculpture, which indicates the originality of the piece. The results from this study helped restorers to choose the appropriate procedures for intervening in the sculpture and contributed to the knowledge about the manufacturing process of Brazilian baroque sculptures.
Determination of Structural and Vibrational Properties of 5-QUINOLINECARBOXALDEHYDE Using Experimental Ft-Ir Ft-Raman Techniques and Theoretical HF and DFT Methods

NASA Astrophysics Data System (ADS)

Kumru, Mustafa; Kocademir, Mustafa; Bardakci, Tayyibe

2013-06-01

Quinoline derivatives have been used in several pharmaceuticals. They have vital roles in regulating the functions of DNA and cancerous cells. It's necessary to determine the structures and spectroscopic properties of quinoline derivates. In this study, the FT-IR (including mid and far regions) and FT-Raman spectra of 5-quinolinecarboxaldehyde have been investigated. Hartree-Fock (HF) and density functional B3LYP calculations have also been employed with the 6-311++G(d,p) basis set for investigating the structural and spectroscopic properties of the cis and trans conformers of 5-quinolinecarboxaldehyde. Experimental and theoretical results have been compared and the results are in good agreement with each other. Keywords: 5-quinolinecarboxaldehyde; Vibrational Spectroscopy; FT-IR spectra; FT-Raman spectra; Vibrational Modes; HF; DFT [1] V. Kucuk, A. Altun, M. Kumru, Spectrochim. Acta Part A 85(2012)92-98 [2] M. Kumru, V. Kucuk, T. Bardakci, Spectrochim. Acta Part A 90(2012)28-34 [3] M. Kumru, V. Kucuk, M. Kocademir, Spectrochim. Acta Part A, 96 (2012) 242-251 We thank the Turkish Scientific and Technical Research Council (TUBITAK) for their financial support through National Postdoctoral Research Scholarship Programme and Scientific Research Fund of Fatih University under the project number P50011001 G (1457).
Experimental (FT-IR, FT-Raman, 1H, 13C NMR) and theoretical study of alkali metal 2-aminobenzoates

NASA Astrophysics Data System (ADS)

Samsonowicz, M.; Świsłocka, R.; Regulska, E.; Lewandowski, W.

2008-09-01

The influence of lithium, sodium, potassium, rubidium and cesium on the electronic system of the 2-aminobenzoic acid was studied by the methods of molecular spectroscopy. The vibrational (FT-IR, FT-Raman) and NMR ( 1H and 13C) spectra for 2-aminobenzoic acid and its alkali metal salts were recorded. The assignment of vibrational spectra was done on the basis of literature data, theoretical calculations and our previous experience. Characteristic shifts of bands and changes in intensities of bands along the metal series were observed. The changes of chemical shifts of protons ( 1H NMR) and carbons ( 13C NMR) in the series of studied alkali metal 2-aminobenzoates were observed too. Optimized geometrical structures of studied compounds were calculated by B3LYP method using 6-311++G ∗∗ basis set. Geometric aromaticity indices, dipole moments and energies were also calculated. The theoretical wavenumbers and intensities of IR and Raman spectra were obtained. The calculated parameters were compared to experimental characteristic of studied compounds.
Vibrational and theoretical study of selected diacetylenes.

PubMed

Roman, Maciej; Baranska, Malgorzata

2013-11-01

Six commonly used disubstituted diacetylenes with short side-chains (RCCCCR, where R=CH2OH, CH2OPh, C(CH3)2OH, C(CH3)3, Si(CH3)3, and Ph) were analyzed using vibrational spectroscopy and quantum-chemical calculations to shed new light on structural and spectroscopic properties of these compounds. Prior to that the conformational analysis of diacetylenes was performed to search the Potential Energy Surface for low-energy minima. Theoretical investigations were followed by the potential energy distribution (PED) analysis to gain deeper insight into FT-Raman and FT-IR spectra that, in some cases, were recorded for the first time for the studied compounds. The analysis was focused mainly on spectral features of the diacetylene system sensitive to the substitution. Shifts of the characteristic bands and changes in bond lengths were observed when changing the substituent. Furthermore, Fermi resonance was observed in the vibrational spectra of some diacetylenes. FT-IR spectra were measured by using two methods, i.e. transmission (with KBr substrate) and Attenuated Total Reflection (ATR), showing the latter adequate and fast tool for IR measurements of diacetylenes. Additionally, Surface Enhanced Raman Spectroscopy (SERS) was applied for phenyl derivative for the first time to study its interaction with metallic nanoparticles that seems to be perpendicular. Copyright © 2013 Elsevier B.V. All rights reserved.
Utilization of visible to NIR light energy by Yb+3, Er+3 and Tm+3 doped BiVO4 for the photocatalytic degradation of methylene blue

NASA Astrophysics Data System (ADS)

Regmi, Chhabilal; Kshetri, Yuwaraj K.; Ray, Schindra Kumar; Pandey, Ramesh Prasad; Lee, Soo Wohn

2017-01-01

Lanthanide-doped BiVO4 semiconductors with efficient photocatalytic activities over a broad range of the solar light spectrum have been synthesized by the microwave hydrothermal method using ethylenediaminetetraacetic acid (EDTA). The structural, morphological, and optical properties of the as-synthesized samples were evaluated by Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), X-ray powder diffraction (XRD), Raman spectroscopy, FT-IR spectroscopy, UV-vis diffuse reflectance spectroscopy (DRS), and photoluminescence spectroscopy (PL). The chemical compositions were analyzed by X-ray photoelectron spectroscopy (XPS). The toxicity of the samples was measured using Mus musculus skin melanoma cells (B16-F10 (ATCC® CRL-6475™)) and were found to be nontoxic for human cells. The photocatalytic efficiency of the prepared samples was evaluated by methylene blue (MB) degradation. The best photocatalytic activity was shown by BiVO4 with 6:3:3 mol percentage of Yb+3:Er+3:Tm+3 in all solar light spectrum. The synthesized samples possess low band gap energy and a hollow structure suitable for the better photocatalytic activity. The observed NIR photoactivity supports that the upconversion mechanism is involved in the overall photocatalytic process. Therefore, this approach provides a better alternative upconversion material for integral solar light absorption.

Molecular structure and vibrational analysis of Trifluoperazine by FT-IR, FT-Raman and UV-Vis spectroscopies combined with DFT calculations.

PubMed

Rajesh, P; Gunasekaran, S; Gnanasambandan, T; Seshadri, S

2015-02-25

The complete vibrational assignment and analysis of the fundamental vibrational modes of Trifluoperazine (TFZ) was carried out using the experimental FT-IR, FT-Raman and UV-Vis data and quantum chemical studies. The observed vibrational data were compared with the wavenumbers derived theoretically for the optimized geometry of the compound from the DFT-B3LYP gradient calculations employing 6-31G (d,p) basis set. Thermodynamic properties like entropy, heat capacity and enthalpy have been calculated for the molecule. The HOMO-LUMO energy gap has been calculated. The intramolecular contacts have been interpreted using natural bond orbital (NBO) and natural localized molecular orbital (NLMO) analysis. Important non-linear properties such as first hyperpolarizability of TFZ have been computed using B3LYP quantum chemical calculation. Copyright © 2014 Elsevier B.V. All rights reserved.
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.
Differentiation of Leishmania species by FT-IR spectroscopy

NASA Astrophysics Data System (ADS)

Aguiar, Josafá C.; Mittmann, Josane; Ferreira, Isabelle; Ferreira-Strixino, Juliana; Raniero, Leandro

2015-05-01

Leishmaniasis is a parasitic infectious disease caused by protozoa that belong to the genus Leishmania. It is transmitted by the bite of an infected female Sand fly. The disease is endemic in 88 countries Desjeux (2001) [1] (16 developed countries and 72 developing countries) on four continents. In Brazil, epidemiological data show the disease is present in all Brazilian regions, with the highest incidences in the North and Northeast. There are several methods used to diagnose leishmaniasis, but these procedures have many limitations, are time consuming, have low sensitivity, and are expensive. In this context, Fourier Transform Infrared Spectroscopy (FT-IR) analysis has the potential to provide rapid results and may be adapted for a clinical test with high sensitivity and specificity. In this work, FT-IR was used as a tool to investigate the promastigotes of Leishmaniaamazonensis, Leishmaniachagasi, and Leishmaniamajor species. The spectra were analyzed by cluster analysis and deconvolution procedure base on spectra second derivatives. Results: cluster analysis found four specific regions that are able to identify the Leishmania species. The dendrogram representation clearly indicates the heterogeneity among Leishmania species. The band deconvolution done by the curve fitting in these regions quantitatively differentiated the polysaccharides, amide III, phospholipids, proteins, and nucleic acids. L. chagasi and L. major showed a greater biochemistry similarity and have three bands that were not registered in L. amazonensis. The L. amazonensis presented three specific bands that were not recorded in the other two species. It is evident that the FT-IR method is an indispensable tool to discriminate these parasites. The high sensitivity and specificity of this technique opens up the possibilities for further studies about characterization of other microorganisms.
Analysis of tissue specific progenitor cell differentiation using FT-IR

NASA Astrophysics Data System (ADS)

Ishii, Katsunori; Kimura, Akinori; Kushibiki, Toshihiro; Awazu, Kunio

2007-07-01

Tissue specific progenitor cells and its differentiations have got a lot of attentions in regenerative medicine. The process of differentiations, the formation of tissues, has become better understood by the study using a lot of cell types progressively. These studies of cells and tissue dynamics at molecular levels are carried out through various approaches like histochemical methods, application of molecular biology and immunology. However, in case of using regenerative sources (cells, tissues and biomaterials etc.) clinically, they are measured and quality-controlled by non-contact and non-destructive methods from the view point of safety. Or the analysis with small quantities of materials could be possible if the quantities of materials are acceptable. A non-contact and non-destructive quality control method has been required. Recently, the use of Fourier Transform Infrared spectroscopy (FT-IR) has been used to monitor biochemical changes in cells, and has gained considerable importance. The changes in the cells and tissues, which are subtle and often not obvious in the histpathological studies, are shown to be well resolved using FT-IR. Moreover, although most techniques designed to detect one or a few changes, FT-IR is possible to identify the changes in the levels of various cellular biochemicals simultaneously under in vivo and in vitro conditions. The objective of this study is to establish the infrared spectroscopy of tissue specific progenitor cell differentiations as a quality control of cell sources for regenerative medicine. In the present study, as a basic study, we examine the adipose differentiation kinetics of preadipose cells (3T3-L1) and the osteoblast differentiation kinetics of mesenchymal stem cells (Kusa-A1) to analyze the infrared absorption spectra.
Magnetic cellulose/Ag as a novel eco-friendly nanobiocomposite to catalyze synthesis of chromene-linked nicotinonitriles.

PubMed

Maleki, Ali; Movahed, Hamed; Ravaghi, Parisa

2017-01-20

In this work, design, preparation and performance of magnetic cellulose/Ag nanobiocomposite as a recyclable and highly efficient heterogeneous nanocatalyst is described. Fourier transform infrared (FT-IR) spectroscopy, X-ray diffraction (XRD) pattern, vibrating sample magnetometer (VSM) curve, field-emission scanning electron microscopy (FE-SEM) image, energy dispersive X-ray (EDX) analysis and thermogravimetric analysis/differential thermal analysis (TGA/DTA) were used for the characterization. Then, its activity was investigated in the synthesis of 2-amino-6-(2-oxo-2H-chromen-3-yl)-4-phenylnicotinonitrile derivatives. The main advantages of the reaction are high yields and short reaction times. The remarkable magnetic property of the nanobiocomposite catalyst provides easy separation from the reaction mixture by an external magnet without considerable loss of its catalytic activity. Copyright © 2016 Elsevier Ltd. All rights reserved.
Rationally Designed 2D Covalent Organic Framework with a Brick-Wall Topology

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

Cai, Song-Liang; Zhang, Kai; Tan, Jing-Bo

In this paper, we report the design and synthesis of an imine-based two-dimensional covalent organic framework (2D COF) with a novel brick-wall topology by judiciously choosing a tritopic T-shaped building block and a ditopic linear linker. Unlike the main body of COF frameworks reported to-date, which consists of higher-symmetry 2D topologies, the unconventional layered brick-wall topology have only been proposed but never been realized experimentally. The brick-wall structure was characterized by powder X-ray diffraction analysis, FT-IR, solid state 13C NMR spectroscopy, nitrogen, and carbon oxide adsorption-desorption measurements as well as theoretical simulations. Lastly, our present work opens the door tomore » the design of novel 2D COFs and will broaden the scope of emerging COF materials.« less
Synthesis and characterization of nanocomposite polymer blend electrolyte thin films by spin-coating method

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

Chapi, Sharanappa; Niranjana, M.; Devendrappa, H., E-mail: dehu2010@gmail.com

2016-05-23

Solid Polymer blend electrolytes based on Polyethylene oxide (PEO) and poly vinyl pyrrolidone (PVP) complexed with zinc oxide nanoparticles (ZnO NPs; Synthesized by Co-precipitation method) thin films have prepared at a different weight percent using the spin-coating method. The complexation of the NPs with the polymer blend was confirmed by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR). The variation in film morphology was examined by polarized optical micrographs (POMs). The thermal behavior of blends was investigated under non-isothermal conditions by differential thermal analyses (DTA). A single glass transition temperature for each blend was observed, which supports the existence ofmore » compatibility of such system. The obtained results represent that the ternary based thin films are prominent materials for battery and optoelectronic device applications.« less
Carbonic anhydrase inhibition of Schiff base derivative of imino-methyl-naphthalen-2-ol: Synthesis, structure elucidation, molecular docking, dynamic simulation and density functional theory calculations

NASA Astrophysics Data System (ADS)

Abbas, Saghir; Nasir, Hafiza Huma; Zaib, Sumera; Ali, Saqib; Mahmood, Tariq; Ayub, Khurshid; Tahir, Muhammad Nawaz; Iqbal, Jamshed

2018-03-01

In the present study, we have designed and synthesized a Schiff base derivative 3 and characterized by FT-IR, 1H and 13C NMR spectroscopy. Single crystal X-ray diffraction and NMR studies were also performed. The synthetic compound was screened for its inhibitory potential against carbonic anhydrase II. The experimental results were validated by molecular docking and dynamic simulations of compound 3 in the active pocket of enzyme. Important binding interactions with the key residues in the active site of the carbonic anhydrase enzyme were revealed. Moreover, supramolecular assembly of the title compound was analyzed by density functional theory (DFT) calculations. These studies rendered a more clear understanding for the demonstration of novel molecular mechanism involved in CA II inhibition by the synthesized compound.
A common 'aggregation-prone' interface possibly participates in the self-assembly of human zona pellucida proteins.

PubMed

Louros, Nikolaos N; Chrysina, Evangelia D; Baltatzis, Georgios E; Patsouris, Efstratios S; Hamodrakas, Stavros J; Iconomidou, Vassiliki A

2016-03-01

Human zona pellucida (ZP) is composed of four glycoproteins, namely ZP1, ZP2, ZP3 and ZP4. ZP proteins form heterodimers, which are incorporated into filaments through a common bipartite polymerizing component, designated as the ZP domain. The latter is composed of two individually folded subdomains, named ZP-N and ZP-C. Here, we have synthesized six 'aggregation-prone' peptides, corresponding to a common interface of human ZP2, ZP3 and ZP4. Experimental results utilizing electron microscopy, X-ray diffraction, ATR FT-IR spectroscopy and polarizing microscopy indicate that these peptides self-assemble forming fibrils with distinct amyloid-like features. Finally, by performing detailed modeling and docking, we attempt to shed some light in the self-assembly mechanism of human ZP proteins. © 2016 Federation of European Biochemical Societies.
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.
Hybrid magnetic materials formed by ferritin intercalated into a layered double hydroxide

NASA Astrophysics Data System (ADS)

Clemente-León, Miguel; Coronado, Eugenio; Primo, Vicent; Ribera, Antonio; Soriano-Portillo, Alejandra

2008-12-01

A hybrid magnetic material formed by ferritin intercalated into a layered double hydroxide (LDH) of Mg and Al (Mg/Al molar ratio 2) is prepared and characterized through powder X-ray diffraction (XRD), thermogravimetric analysis (TGA), Fourier transform infrared (FT-IR) spectroscopy, electron probe microanalysis (EPMA) and high resolution transmission electron microscopy (HRTEM). One observes an enhancement in the thermal stability of the ferritin molecules when they are inserted in the layered material. Magnetic measurements of the hybrid material exhibit the typical superparamagnetic behaviour of the ferritin molecule. On the other hand, the intercalation of ferritin into the LDH guarantees a homogeneous dispersion of the ferritin molecules, which do not aggregate even after calcination of the sample. This feature allows obtaining well-dispersed magnetic metal oxide nanoparticles upon calcination of the hybrid material.
Elaboration of the hydroxyapatite with different precursors and application for the retention of the lead.

PubMed

Meski, S; Ziani, S; Khireddine, H; Yataghane, F; Ferguene, N

2011-01-01

Carbonate hydroxyapatite (CHAP) was synthesized from different precursors; synthetic (CaCO3 and Ca(OH)2) and natural (egg shell before and after calcinations at 900 degrees C) under different conditions and characterized by using TG/DTG analysis, X-ray powder diffraction (XRD) method and Fourier transform infrared (FT-IR) spectroscopy techniques. The results of these analyses indicate that the four powders present the same structure of hydroxyapatite. Furthermore the four powders obtained were used for the retention of lead. The results obtained indicated that all powders present high adsorption capacity for lead, but from environmental and economic views, the hydroxyapatite synthesized from eggshell no calcined (HA2) is most advantageous. The influence of different sorption parameters, such as: initial metal concentration, equilibration time, solution pH and sorbent dosage was studied and discussed.
Synthesis, characterization, biocompatibility of hydroxyapatite-natural polymers nanocomposites for dentistry applications.

PubMed

Chung, Jin-Hwan; Kim, Young Kyung; Kim, Kyo-Han; Kwon, Tae-Yub; Vaezmomeni, Seyede Ziba; Samiei, Mohammad; Aghazadeh, Marzyeh; Davaran, Soodabeh; Mahkam, Mehrdad; Asadi, Ghale; Akbarzadeh, Abolfazl

2016-01-01

Hydroxyapatite (HA), the main mineral component of bones and teeth, was synthesized by using the reaction between calcium nitrate tetrahydrate Ca(NO3)2∙4H2O and diammonium hydrogen phosphate (NH4)2HPO4 (DAHP) with a chemical precipitation method. The objective of this study is to utilize novel inorganic-organic nanocomposites for biomedical applications. HA is an inorganic component (75% w) and chitosan, alginate and albumin (Egg white) are organic components of nanocomposites (25% w). Nanocomposites were prepared in deionized water solutions, at room temperature, using a mechanical and magnetic stirrer for 48 h. The microstructure and morphology of sintered n-HAP were tested at different preheating temperature and laser sintering speed with scanning electron microscopy (SEM), X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FT-IR).
Rationally Designed 2D Covalent Organic Framework with a Brick-Wall Topology

DOE PAGES

Cai, Song-Liang; Zhang, Kai; Tan, Jing-Bo; ...

2016-11-23

In this paper, we report the design and synthesis of an imine-based two-dimensional covalent organic framework (2D COF) with a novel brick-wall topology by judiciously choosing a tritopic T-shaped building block and a ditopic linear linker. Unlike the main body of COF frameworks reported to-date, which consists of higher-symmetry 2D topologies, the unconventional layered brick-wall topology have only been proposed but never been realized experimentally. The brick-wall structure was characterized by powder X-ray diffraction analysis, FT-IR, solid state 13C NMR spectroscopy, nitrogen, and carbon oxide adsorption-desorption measurements as well as theoretical simulations. Lastly, our present work opens the door tomore » the design of novel 2D COFs and will broaden the scope of emerging COF materials.« less
Dye sensitized solar cell based on environmental friendly eosin Y dye and Al doped titanium dioxide nano particles

NASA Astrophysics Data System (ADS)

Kulkarni, Swati S.; Bodkhe, Gajanan A.; Shirsat, Sumedh M.; Hussaini, S. S.; Shejwal, N. N.; Shirsat, Mahendra D.

2018-03-01

Present communication deals with the development of cost effective dye sensitized solar cell (DSSC) with eco-friendly materials. Eco-friendly Eosin Y dye was used to sensitize photo anode which was fabricated using undoped and Aluminium doped titanium dioxide (TiO2) nanoparticles. Undoped and Aluminium doped TiO2 nanoparticles were synthesized by simple and cost effective sol-gel method. Aluminium doped and undoped TiO2 nanoparticles were characterized using UV-visible, FT-IR spectroscopy, x-ray Diffraction, and Scanning Electron Micrograph with EDX. The photo-voltaic activity of the cell was studied under light irradiation of 100 milliwatt cm-2. Aluminium doped TiO2 nanoparticle photo electrode exhibits more than 60% increase in cell efficiency as compared to the undoped TiO2 nanoparticle photo electrode.
Magnetic graphene oxide for adsorption of organic dyes from aqueous solution

NASA Astrophysics Data System (ADS)

Drashya, Lal, Shyam; Hooda, Sunita

2018-05-01

Graphene oxide (GO), a 2-D carbon nanomaterial, large surface area, oxygen-containing groups (like: hydroxyl, epoxy and carboxyl) and excellent water dispersibility due to it is good adsorbent dye removal from pollutant water1. But it's difficult to separate GO from water after adsorption. Therefore, Iron oxide was introduced in Graphene oxide by decorating method to make separation more efficient2. We present herein a one step process to prepare Magnetic Graphene oxide (MGO). The Fourier transform infrared spectrometer (FT-IR), X-ray diffraction (XRD) and Raman Spectroscopy characterized the chemical structure of the MGO composite. The adsorption of dyes onto MGO was studied in relation to initial concentration of Dyes, contact time, adsorbent dose, temperature and pH value of solution. We have studied adsorption capacity of different dyes (Methylene blue and crystal violet) by MGO.
Chemical Functionalization of Germanium with Dextran Brushes for Immobilization of Proteins Revealed by Attenuated Total Reflection Fourier Transform Infrared Difference Spectroscopy.

PubMed

Schartner, Jonas; Hoeck, Nina; Güldenhaupt, Jörn; Mavarani, Laven; Nabers, Andreas; Gerwert, Klaus; Kötting, Carsten

2015-07-21

Protein immobilization studied by attenuated total reflection Fourier transform infrared (ATR-FT-IR) difference spectroscopy is an emerging field enabling the study of proteins at atomic detail. Gold or glass surfaces are frequently used for protein immobilization. Here, we present an alternative method for protein immobilization on germanium. Because of its high refractive index and broad spectral window germanium is the best material for ATR-FT-IR spectroscopy of thin layers. So far, this technique was mainly used for protein monolayers, which lead to a limited signal-to-noise ratio. Further, undesired protein-protein interactions can occur in a dense layer. Here, the germanium surface was functionalized with thiols and stepwise a dextran brush was generated. Each step was monitored by ATR-FT-IR spectroscopy. We compared a 70 kDa dextran with a 500 kDa dextran regarding the binding properties. All surfaces were characterized by atomic force microscopy, revealing thicknesses between 40 and 110 nm. To analyze the capability of our system we utilized N-Ras on mono-NTA (nitrilotriacetic acid) functionalized dextran, and the amount of immobilized Ras corresponded to several monolayers. The protein stability and loading capacity was further improved by means of tris-NTA for immobilization. Small-molecule-induced changes were revealed with an over 3 times higher signal-to-noise ratio compared to monolayers. This improvement may allow the observation of very small and so far hidden changes in proteins upon stimulus. Furthermore, we immobilized green fluorescent protein (GFP) and mCherry simultaneously enabling an analysis of the surface by fluorescence microscopy. The absence of a Förster resonance energy transfer (FRET) signal demonstrated a large protein-protein distance, indicating an even distribution of the protein within the dextran.
Nb2O5 nanowires in-situ grown on carbon fiber: A high-efficiency material for the photocatalytic reduction of Cr(VI).

PubMed

Du, Yucheng; Zhang, Shihao; Wang, Jinshu; Wu, Junshu; Dai, Hongxing

2018-04-01

Niobium oxide nanowire-deposited carbon fiber (CF) samples were prepared using a hydrothermal method with amorphous Nb 2 O 5 ·nH 2 O as precursor. The physical properties of the samples were characterized by means of numerous techniques, including X-ray diffraction (XRD), energy-dispersive spectroscopy (EDS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected-area electron diffraction (SAED), UV-visible spectroscopy (UV-vis), N 2 adsorption-desorption, Fourier transform infrared spectroscopy (FT-IR), and X-ray photoelectron spectroscopy. The efficiency for the removal of Cr(VI) was determined. Parameters such as pH value and initial Cr(VI) concentration could influence the Cr(VI) removal efficiency or adsorption capacity of the Nb 2 O 5 /carbon fiber sample obtained after hydrothermal treatment at 160°C for 14hr. The maximal Cr(VI) adsorption capacity of the Nb 2 O 5 nanowire/CF sample was 115mg/g. This Nb 2 O 5 /CF sample also showed excellent photocatalytic activity and stability for the reduction of Cr(VI) under UV-light irradiation: the Cr(VI) removal efficiency reached 99.9% after UV-light irradiation for 1hr and there was no significant decrease in photocatalytic performance after the use of the sample for 10 repeated cycles. Such excellent Cr(VI) adsorption capacity and photocatalytic performance was related to its high surface area, abundant surface hydroxyl groups, and good UV-light absorption ability. Copyright © 2017. Published by Elsevier B.V.
Miniature high-performance infrared spectrometer for space applications

NASA Astrophysics Data System (ADS)

Kruzelecky, Roman V.; Haddad, Emile; Wong, Brian; Lafrance, Denis; Jamroz, Wes; Ghosh, Asoke K.; Zheng, Wanping; Phong, Linh

2004-06-01

Infrared spectroscopy probes the characteristic vibrational and rotational modes of chemical bonds in molecules to provide information about both the chemical composition and the bonding configuration of a sample. The significant advantage of the Infrared spectral technique is that it can be used with minimal consumables to simultaneously detect a large variety of chemical and biochemical species with high chemical specificity. To date, relatively large Fourier Transform (FT-IR) spectrometers employing variations of the Michelson interferometer have been successfully employed in space for various IR spectroscopy applications. However, FT-IR systems are mechanically complex, bulky (> 15 kg), and require considerable processing. This paper discusses the use of advanced integrated optics and smart optical coding techniques to significantly extend the performance of miniature IR spectrometers by several orders of magnitude in sensitivity. This can provide the next-generation of compact, high-performance IR spectrometers with monolithically integrated optical systems for robust optical alignment. The entire module can weigh under 3 kg to minimize the mass penalty for space applications. Miniaturized IR spectrometers are versatile and very convenient for small and micro satellite based missions. They can be dedicated to the monitoring of the CO2 in an Earth Observation mission, to Mars exobiology exploration, as well as to vital life support in manned space system; such as the cabin air quality and the quality of the recycled water supply.
Miniature high-performance infrared spectrometer for space applications

NASA Astrophysics Data System (ADS)

Kruzelecky, Roman V.; Haddad, Emile; Wong, Brian; Lafrance, Denis; Jamroz, Wes; Ghosh, Asoke K.; Zheng, Wanping; Phong, Linh

2017-11-01

Infrared spectroscopy probes the characteristic vibrational and rotational modes of chemical bonds in molecules to provide information about both the chemical composition and the bonding configuration of a sample. The significant advantage of the Infrared spectral technique is that it can be used with minimal consumables to simultaneously detect a large variety of chemical and biochemical species with high chemical specificity. To date, relatively large Fourier Transform (FT-IR) spectrometers employing variations of the Michelson interferometer have been successfully employed in space for various IR spectroscopy applications. However, FT-IR systems are mechanically complex, bulky (> 15 kg), and require considerable processing. This paper discusses the use of advanced integrated optics and smart optical coding techniques to significantly extend the performance of miniature IR spectrometers by several orders of magnitude in sensitivity. This can provide the next generation of compact, high-performance IR spectrometers with monolithically integrated optical systems for robust optical alignment. The entire module can weigh under 3 kg to minimize the mass penalty for space applications. Miniaturized IR spectrometers are versatile and very convenient for small and micro satellite based missions. They can be dedicated to the monitoring of the CO2 in an Earth Observation mission, to Mars exobiology exploration, as well as to vital life support in manned space system; such as the cabin air quality and the quality of the recycled water supply.

Rapid identification and classification of Listeria spp. and serotype assignment of Listeria monocytogenes using fourier transform-infrared spectroscopy and artificial neural network analysis

USDA-ARS?s Scientific Manuscript database

The use of Fourier Transform-Infrared Spectroscopy (FT-IR) in conjunction with Artificial Neural Network software, NeuroDeveloper™ was examined for the rapid identification and classification of Listeria species and serotyping of Listeria monocytogenes. A spectral library was created for 245 strains...
Hydrothermal synthesis, crystal structures, and enantioselective adsorption property of bis(L-histidinato)nickel(II) monohydrate

NASA Astrophysics Data System (ADS)

Ramos, Christian Paul L.; Conato, Marlon T.

2018-05-01

Despite the numerous researches in metal-organic frameworks (MOFs), there are only few reports on biologically important amino acids, histidine in particular, on its use as bridging ligand in the construction of open-framework architectures. In this work, hydrothermal synthesis was used to prepare a compound based on Ni2+ and histidine. The coordination assembly of imidazole side chain of histidine with divalent nickel ions in aqueous condition yielded purple prismatic solids. Single crystal X-ray diffraction (XRD) analysis of the product revealed structure for Ni(C6H8N3O2)2 • H2O that has a monoclinic (C2) structure with lattice parameters, a = 29.41, b = 8.27, c = 6.31 Å, β = 90.01 ˚. Circular dichroism - optical rotatory dispersion (CD-ORD), Powder X-ray diffraction (PXRD) and Fourier transform - infrared spectroscopy (FT-IR) analyses are conducted to further characterize the crystals. Enantioselective adsorption analysis using racemic mixture of 2-butanol confirmed bis(L-histidinato)nickel(II) monohydrate MOF crystal's enantioselective property preferentially favoring the adsorption of (S)-2-butanol isomer.
Frequency dependent dielectric properties of combustion synthesized Dy2Ti2O7 pyrochlore oxide

NASA Astrophysics Data System (ADS)

Jeyasingh, T.; Saji, S. K.; Kavitha, V. T.; Wariar, P. R. S.

2018-05-01

Nanocrystalline pyrochlore material Dysprosium Titanate (Dy2Ti2O7) has been synthesized through a single step optimized combustion route. The phase purity and phase formation of the combustion product has been characterized using X-Ray diffraction analysis (XRD) and Fourier Transform Infrared Spectroscopy (FT-IR) analysis. X-Ray diffraction analysis (XRD) reveal that Dy2Ti2O7 is highly crystalline in nature with cubic structure in the Fd3m space group. The microstructures and average particle size of the prepared nanopowder were examined by High Resolution Transmission Electron Microscopy (HR-TEM). The optical band gap of the Dy2Ti2O7 nanoparticles is determined from the absorption spectrum, was attributed to direct allowed transitions through optical band gap of 3.98 eV. The frequency dependent dielectric measurements have been carried out on the sintered pellet in the frequency range 1 Hz-10 MHz. The measured value of dielectric constant (ℇ') was ˜ 43 and loss tangent (tan δ) was 4×10-3 at 1 MHz, at room temperature.
Characterization and differentiation of high energy cyclic organic peroxides by GC/FT-IR, GC-MS, FT-IR, and Raman microscopy

NASA Astrophysics Data System (ADS)

Pena, Alvaro J.; Pacheco-Londono, Leonardo; Figueroa, Javier; Rivera-Montalvo, Luis A.; Roman-Velazquez, Felix R.; Hernandez-Rivera, Samuel P.

2005-05-01

The characterization of Tetracetone Tetraperoxide (TRATRP), Triacetone Triperoxide (TATP), Diacetone Diperoxide (DADP), Tricyclohexylidene Triperoxide and Dibenzo Diperoxide using GC-MS, GC-FTIR, FTIR, FT-NMR and Raman Spectroscopy is reported. These compounds were synthesized, purified and characterized in the laboratory in order to develop methodologies for their trace detection. During this study, TATP has been synthesized by different methods obtaining high purity and good yields, even using common household products. DADP synthetic routes reported in the literature were verified. The methods described, including those that produce mixtures with TATP and other peroxides forms were also tested. This study will also focused in the preparation of other cyclic peroxides, including Hexamethelene Triperoxide Diamine (HMTD) and different forms of cyclic peroxides from ketones. This issue of thermodynamic versus kinetic control of secondary products of all syntheses and the effect of temperature in the distribution sub products of the syntheses was also addressed. A vibrational differentiation study of was carried out. Differences were found computationally in the υ(O-O), υ(C-O), δ(CH3-C) and δ(C-O) for Raman and IR bands and retention time and fragment patron for GC-MS and GC-FT-IR.
AFM-IR: Technology and Applications in Nanoscale Infrared Spectroscopy and Chemical Imaging.

PubMed

Dazzi, Alexandre; Prater, Craig B

2016-12-13

Atomic force microscopy-based infrared spectroscopy (AFM-IR) is a rapidly emerging technique that provides chemical analysis and compositional mapping with spatial resolution far below conventional optical diffraction limits. AFM-IR works by using the tip of an AFM probe to locally detect thermal expansion in a sample resulting from absorption of infrared radiation. AFM-IR thus can provide the spatial resolution of AFM in combination with the chemical analysis and compositional imaging capabilities of infrared spectroscopy. This article briefly reviews the development and underlying technology of AFM-IR, including recent advances, and then surveys a wide range of applications and investigations using AFM-IR. AFM-IR applications that will be discussed include those in polymers, life sciences, photonics, solar cells, semiconductors, pharmaceuticals, and cultural heritage. In the Supporting Information , the authors provide a theoretical section that reviews the physics underlying the AFM-IR measurement and detection mechanisms.
Fast Infrared Chemical Imaging with a Quantum Cascade Laser

PubMed Central

2015-01-01

Infrared (IR) spectroscopic imaging systems are a powerful tool for visualizing molecular microstructure of a sample without the need for dyes or stains. Table-top Fourier transform infrared (FT-IR) imaging spectrometers, the current established technology, can record broadband spectral data efficiently but requires scanning the entire spectrum with a low throughput source. The advent of high-intensity, broadly tunable quantum cascade lasers (QCL) has now accelerated IR imaging but results in a fundamentally different type of instrument and approach, namely, discrete frequency IR (DF-IR) spectral imaging. While the higher intensity of the source provides a higher signal per channel, the absence of spectral multiplexing also provides new opportunities and challenges. Here, we couple a rapidly tunable QCL with a high performance microscope equipped with a cooled focal plane array (FPA) detector. Our optical system is conceptualized to provide optimal performance based on recent theory and design rules for high-definition (HD) IR imaging. Multiple QCL units are multiplexed together to provide spectral coverage across the fingerprint region (776.9 to 1904.4 cm–1) in our DF-IR microscope capable of broad spectral coverage, wide-field detection, and diffraction-limited spectral imaging. We demonstrate that the spectral and spatial fidelity of this system is at least as good as the best FT-IR imaging systems. Our configuration provides a speedup for equivalent spectral signal-to-noise ratio (SNR) compared to the best spectral quality from a high-performance linear array system that has 10-fold larger pixels. Compared to the fastest available HD FT-IR imaging system, we demonstrate scanning of large tissue microarrays (TMA) in 3-orders of magnitude smaller time per essential spectral frequency. These advances offer new opportunities for high throughput IR chemical imaging, especially for the measurement of cells and tissues. PMID:25474546
Fast infrared chemical imaging with a quantum cascade laser.

PubMed

Yeh, Kevin; Kenkel, Seth; Liu, Jui-Nung; Bhargava, Rohit

2015-01-06

Infrared (IR) spectroscopic imaging systems are a powerful tool for visualizing molecular microstructure of a sample without the need for dyes or stains. Table-top Fourier transform infrared (FT-IR) imaging spectrometers, the current established technology, can record broadband spectral data efficiently but requires scanning the entire spectrum with a low throughput source. The advent of high-intensity, broadly tunable quantum cascade lasers (QCL) has now accelerated IR imaging but results in a fundamentally different type of instrument and approach, namely, discrete frequency IR (DF-IR) spectral imaging. While the higher intensity of the source provides a higher signal per channel, the absence of spectral multiplexing also provides new opportunities and challenges. Here, we couple a rapidly tunable QCL with a high performance microscope equipped with a cooled focal plane array (FPA) detector. Our optical system is conceptualized to provide optimal performance based on recent theory and design rules for high-definition (HD) IR imaging. Multiple QCL units are multiplexed together to provide spectral coverage across the fingerprint region (776.9 to 1904.4 cm(-1)) in our DF-IR microscope capable of broad spectral coverage, wide-field detection, and diffraction-limited spectral imaging. We demonstrate that the spectral and spatial fidelity of this system is at least as good as the best FT-IR imaging systems. Our configuration provides a speedup for equivalent spectral signal-to-noise ratio (SNR) compared to the best spectral quality from a high-performance linear array system that has 10-fold larger pixels. Compared to the fastest available HD FT-IR imaging system, we demonstrate scanning of large tissue microarrays (TMA) in 3-orders of magnitude smaller time per essential spectral frequency. These advances offer new opportunities for high throughput IR chemical imaging, especially for the measurement of cells and tissues.
Rapid Identification and Classification of Listeria spp. and Serotype Assignment of Listeria monocytogenes Using Fourier Transform-Infrared Spectroscopy and Artificial Neural Network Analysis

PubMed Central

Romanolo, K. F.; Gorski, L.; Wang, S.; Lauzon, C. R.

2015-01-01

The use of Fourier Transform-Infrared Spectroscopy (FT-IR) in conjunction with Artificial Neural Network software NeuroDeveloper™ was examined for the rapid identification and classification of Listeria species and serotyping of Listeria monocytogenes. A spectral library was created for 245 strains of Listeria spp. to give a biochemical fingerprint from which identification of unknown samples were made. This technology was able to accurately distinguish the Listeria species with 99.03% accuracy. Eleven serotypes of Listeria monocytogenes including 1/2a, 1/2b, and 4b were identified with 96.58% accuracy. In addition, motile and non-motile forms of Listeria were used to create a more robust model for identification. FT-IR coupled with NeuroDeveloper™ appear to be a more accurate and economic choice for rapid identification of pathogenic Listeria spp. than current methods. PMID:26600423
Covalent enzyme immobilization onto carbon nanotubes using a membrane reactor

NASA Astrophysics Data System (ADS)

Voicu, Stefan Ioan; Nechifor, Aurelia Cristina; Gales, Ovidiu; Nechifor, Gheorghe

2011-05-01

Composite porous polysulfone-carbon nanotubes membranes were prepared by dispersing carbon nanotubes into a polysulfone solution followed by the membrane formation by phase inversion-immersion precipitation technique. The carbon nanotubes with amino groups on surface were functionalized with different enzymes (carbonic anhydrase, invertase, diastase) using cyanuric chloride as linker between enzyme and carbon nanotube. The composite membrane was used as a membrane reactor for a better dispersion of carbon nanotubes and access to reaction centers. The membrane also facilitates the transport of enzymes to active carbon nanotubes centers for functionalization (amino groups). The functionalized carbon nanotubes are isolated by dissolving the membranes after the end of reaction. Carbon nanotubes with covalent immobilized enzymes are used for biosensors fabrications. The obtained membranes were characterized by Scanning Electron Microscopy, Thermal analysis, FT-IR Spectroscopy, Nuclear Magnetic Resonance, and functionalized carbon nanotubes were characterized by FT-IR spectroscopy.
Physicochemical properties of chars at different treatment temperatures.

PubMed

Kim, Sung Su; Kang, Youn Suk; Lee, Hyun Dong; Kim, Jae Kwan; Hong, Sung Chang

2012-02-01

In this study, the physicochemical properties of the char of Indonesian SM coal following heat treatment at various temperatures were evaluated using X-ray photoelectron spectroscopy (XPS), Fourier-transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), and morphological and specific surface area analysis. Based on these analyses, heat treatment of coal was determined to be the most effective in increasing the coal rank. In the XPS analysis, the C-O and C-O-C groups and quaternary-N species were found to be of a lower grade coal when the pretreatment temperature decreased, meanwhile the C-C group and pyridinic species increased. In the FT-IR analysis, the collapse of the C-O and C-O-C group was observed due to the collapse of the ether group. In SEM and Brunauer-Emmett-Teller (BET) analysis, a decrease in the ether group was shown to be accompanied with the formation of micropores.
Synthesis, spectroscopic and thermal studies of the copper(II) aspartame chloride complex

NASA Astrophysics Data System (ADS)

Çakır, S.; Coşkun, E.; Naumov, P.; Biçer, E.; Bulut, İ.; İçbudak, H.; Çakır, O.

2002-08-01

Aspartame adduct of copper(II) chloride Cu(Asp) 2Cl 2·2H 2O (Asp=aspartame) is synthesized and characterized by elemental analysis, FT IR, UV/vis, ESR spectroscopies, TG, DTG, DTA measurements and molecular mechanics calculations. Aqueous solution of the green solid absorbs strongly at 774 and 367 nm. According to the FT IR spectra, the aspartame moiety coordinates to the copper(II) ion via its carboxylate ends, whereas the ammonium terminal groups give rise to hydrogen bonding network with the water, the chloride ions or neighboring carboxylate groups. The results suggest tetragonally distorted octahedral environment of the copper ions.
A Controlled-Environment Chamber for Atmospheric Chemistry Studies Using FT-IR Spectroscopy

DTIC Science & Technology

1990-06-01

necessary and identify by block number) FELD GROUP SUB-GROUP i >Chamber, controlled environment; long-path cell ; 07 04 FT-IR; Hydrazine decay...modification doubles the useable path length of the original multipass cell described by White (Reference 8). The pattern of images formed on the nesting...system is shown in Figure 13. 24 z C C02, Ibm, El4 944 C3 ta) caC E-4- 252 14 $4 41) 41) 0. 0 04 04 4 41) ~0 to 0.0 V-4 (A q14 0~ 1% 4-r4 $4 0 u P416 4 4
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.
FT-IR Spectroscopic Analysis of Normal and Malignant Human Oral Tissues

NASA Astrophysics Data System (ADS)

Krishnakumar, N.; Madhavan, R. Nirmal; Sumesh, P.; Palaniappan, Pl. Rm.; Venkatachalam, P.; Ramachandran, C. R.

2008-11-01

FT-IR spectroscopy has been used to explore the changes in the vibrational bands of normal and oral squamous cell carcinoma (OSCC) tissues in the region 4000-400 cm-1. Significant changes in the spectral features were observed. The spectral changes were the results of characteristics structural alterations at the molecular level in the malignant tissues. These alterations include structural changes of proteins and possible increase of its content, an increase in the nucleic-to-cytoplasm ratio, an increase in the relative amount of DNA, an increase in the rate of phosphorylation process induced by carcinogenesis, a loss of hydrogen bonding of the C-OH groups in the amino acid residues of proteins, a decrease in the relative amount of lipids compared to normal epithelial oral tissues. The results of the present study demonstrate that the FT-IR technique has the feasibility of discriminating malignant from normal tissues and other pathological states in a short period of time and may detect malignant transformation earlier than the standard histological examination stage.
Structural modification of poly(methyl methacrylate) by proton irradiation

NASA Astrophysics Data System (ADS)

Choi, H. W.; Woo, H. J.; Hong, W.; Kim, J. K.; Lee, S. K.; Eum, C. H.

2001-01-01

A general survey is presented on the structural modification of poly(methyl methacrylate) (PMMA) by proton implantation. The implanted PMMA films were characterized by FT-IR attenuated total reflection (FT-IR ATR), Raman, Rutherford backscattering spectroscopy (RBS), gel permeation chromatography (GPC) and surface profiling. The ion fluence of 350 keV protons ranged from 2×10 14 to 1×10 15 ions/cm 2. The IR and Raman spectra showed the reduction of peaks from the pendant group of PMMA. The change of absorption and composition was observed by UV-VIS and RBS, respectively. These results showed that the pendant group is readily decomposed and eliminated by proton irradiation. The change of molecular weight distribution was also measured by GPC and G-value of scission was estimated to be 0.67.
Advances in handheld FT-IR instrumentation

NASA Astrophysics Data System (ADS)

Arnó, Josep; Cardillo, Len; Judge, Kevin; Frayer, Maxim; Frunzi, Michael; Hetherington, Paul; Levy, Dustin; Oberndorfer, Kyle; Perec, Walter; Sauer, Terry; Stein, John; Zuidema, Eric

2012-06-01

FT-IR spectroscopy is the technology of choice to identify solid and liquid phase unknown samples. The challenges of ConOps (Concepts of Operation) in emergency response and military field applications require a significant redesign of the stationary FT-IR bench-top instruments typically used in laboratories. Specifically, field portable units require high levels of resistance against mechanical shock and chemical attack, ease of use in restrictive gear, quick and easy interpretation of results, and reduced size. In the last 20 years, FT-IR instruments have been re-engineered to fit in small suitcases for field portable use and recently further miniaturized for handheld operation. This article introduces the advances resulting from a project designed to overcome the challenges associated with miniaturizing FT-IR instruments. The project team developed a disturbance-corrected permanently aligned cube corner interferometer for improved robustness and optimized opto-mechanical design to maximize optical throughput and signal-to-noise ratios. Thermal management and heat flow were thoroughly modeled and studied to isolate sensitive components from heat sources and provide the widest temperature operation range. Similarly, extensive research on mechanical designs and compensation techniques to protect against shock and vibration will be discussed. A user interface was carefully created for military and emergency response applications to provide actionable information in a visual, intuitive format. Similar to the HazMatID family of products, state-of-the-art algorithms were used to quickly identify the chemical composition of complex samples based on the spectral information. This article includes an overview of the design considerations, tests results, and performance validation of the mechanical ruggedness, spectral, and thermal performance.
A portable synthesis of water-soluble carbon dots for highly sensitive and selective detection of chlorogenic acid based on inner filter effect

NASA Astrophysics Data System (ADS)

Yang, Huan; Yang, Liu; Yuan, Yusheng; Pan, Shuang; Yang, Jidong; Yan, Jingjing; Zhang, Hui; Sun, Qianqian; Hu, Xiaoli

2018-01-01

In this work, a simple and facile hydrothermal method for synthesis of water-soluble carbon dots (CDs) with malic acid and urea, and were then employed as a high-performance fluorescent probe for selective and sensitive determination of chlorogenic acid (CGA) based on inner filter effect. The as-synthesized CDs was systematically characterized by Transmission electron microscopy (TEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), Energy disperse spectroscopy (EDS), UV-vis absorption spectroscopy, spectrofluorophotometry, and the results indicated that the sizes of CDs were mainly distributed in the range of 1.0 nm-3.0 nm with an average diameter of 2.1 nm. More significantly, the as-prepared CDs possessed remarkable selectivity and sensitivity towards CGA with the linear range of 0.15 μmol L- 1-60 μmol L- 1 and the detection limit for CGA was 45 nmol L- 1 (3σ/k). The practical applications of CDs for detection of CGA have already been successfully demonstrated in Honeysuckle. This sensitive, selective method has a great application prospect in the pharmaceutical and biological analysis field owing to its simplicity and rapidity for the detection of CGA.
Ultrasonic-assisted synthesis of ZrO2 nanoparticles and their application to improve the chemical stability of Nafion membrane in proton exchange membrane (PEM) fuel cells.

PubMed

Taghizadeh, Mohammad Taghi; Vatanparast, Morteza

2016-12-01

Zirconium dioxide (ZrO2) nanoparticles were fabricated successfully via ultrasonic-assisted method using ZrO(NO3)2·H2O, ethylenediamine and hydrazine as precursors in aqueous solution. Morphology, structure and composition of the obtained products were characterized by means of X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX), dynamic light scattering (DLS), Fourier transform infrared spectroscopy (FT-IR) and diffuse reflectance spectroscopy (DRS). Then, the synthesized nanoparticles were used to prepare Nafion/ZrO2 nanocomposite membranes. The properties of the membranes were studied by ion exchange capacity (IEC) proton conductivity (σ), thermal stability and water uptake measurements. The ex-situ Fenton's test was used to investigate the chemical stability of the membranes. From our results, compared with Nafion membrane, the nanocomposite membrane exhibited lower fluoride release and weight loss. Therefore, it can concluded that Nafion/ZrO2 nanocomposite exhibit more chemical stability than the pure Nafion membrane. ATR-FTIR spectra and SEM surface images of membranes also confirm these results. Copyright © 2016 Elsevier Inc. All rights reserved.
Investigations on surface chemical analysis using X-ray photoelectron spectroscopy and optical properties of Dy3+-doped LiNa3P2O7 phosphor

NASA Astrophysics Data System (ADS)

Munirathnam, K.; Dillip, G. R.; Chaurasia, Shivanand; Joo, S. W.; Deva Prasad Raju, B.; John Sushma, N.

2016-08-01

Near white-light emitting LiNa3P2O7:Dy3+ phosphors were prepared by a conventional solid-state reaction method. The orthorhombic crystal structure of the phosphors was confirmed using X-ray diffraction (XRD), and the valence states of the surface elements were determined from the binding energies of Li 1s, O 1s, Na 1s, P 2p, and Dy 3d by X-ray photoelectron spectroscopy (XPS). Attenuated total reflectance (ATR) - Fourier transform infrared (FT-IR) spectroscopy was employed to identify the pyrophosphate groups in the phosphors. Diffuse reflectance spectra (DRS) show the absorption bands of the Dy3+ ions in the host material. Intense blue (481 nm) and yellow (575 nm) emissions were obtained at an excitation wavelength of 351 nm and are attributed to the 4F9/2 → 6H15/2 and 4F9/2 → 6H13/2 transitions of Dy3+ ions, respectively. The combination of these two intense bands generates light emission in the near-white region of the chromaticity diagram.
Formulation and in vitro characterization of novel sildenafil citrate-loaded polyvinyl alcohol-polyethylene glycol graft copolymer-based orally dissolving films.

PubMed

Xu, Li-Li; Shi, Li-Li; Cao, Qing-Ri; Xu, Wei-Juan; Cao, Yue; Zhu, Xiao-Yin; Cui, Jing-Hao

2014-10-01

This work was aimed to develop novel sildenafil citrate (SC)-loaded polyvinyl alcohol (PVA)-polyethylene glycol (PEG) graft copolymer (Kollicoat(®) IR)-based orally dissolving films (ODFs) using a solvent casting method. Formulation factors such as plasticizers and disintegrants were optimized on the basis of characteristics of blank ODFs. The SC-loaded ODF with a loading capacity up to 6.25mg in an area of 6 cm(2) was prepared and evaluated in terms of mechanical properties, disintegration time and dissolution rate. The physicochemical properties of drug-loaded ODF were also investigated using the scanning electron microscope (SEM), X-ray diffraction (XRD), differential scanning calorimetry (DSC) and Fourier transform infrared spectroscopy (FT-IR). The blank ODF composed of Kollicoat(®) IR, sodium alginate (ALG-Na) and glycerol (10:2:1.5, w/w) had a remarkably short disintegration time of about 20s. The SC-loaded ODF showed a delayed disintegration time (about 25s), but exhibited improved mechanical properties when compared to the blank ODF. SC was homogeneously dispersed throughout the ODF and the crystalline form of drug had been partly changed, existing strong hydrogen bonding between the drug and carriers. The Kollicoat(®) IR/ALG-Na based ODFs containing SC might be an alternative to conventional tablet for the treatment of male erectile dysfunction. Copyright © 2014 Elsevier B.V. All rights reserved.

FT-IR, FT-Raman spectra and DFT calculations of melaminium perchlorate monohydrate.

PubMed

Kanagathara, N; Marchewka, M K; Drozd, M; Renganathan, N G; Gunasekaran, S; Anbalagan, G

2013-08-01

Melaminium perchlorate monohydrate (MPM), an organic material has been synthesized by slow solvent evaporation method at room temperature. Powder X-ray diffraction analysis confirms that MPM crystal belongs to triclinic system with space group P-1. FTIR and FT Raman spectra are recorded at room temperature. Functional group assignment has been made for the melaminium cations and perchlorate anions. Vibrational spectra have also been discussed on the basis of quantum chemical density functional theory (DFT) calculations using Firefly (PC GAMESS) version 7.1 G. Vibrational frequencies are calculated and scaled values are compared with experimental values. The assignment of the bands has been made on the basis of the calculated PED. The Mulliken charges, HOMO-LUMO orbital energies are analyzed directly from Firefly program log files and graphically illustrated. HOMO-LUMO energy gap and other related molecular properties are also calculated. The theoretically constructed FT-IR and FT-Raman spectra of MPM coincide with the experimental one. The chemical structure of the compound has been established by (1)H and (13)C NMR spectra. No detectable signal was observed during powder test for second harmonic generation. Copyright © 2013 Elsevier B.V. All rights reserved.
Thermal behaviour of procaine and benzocaine Part II: compatibility study with some pharmaceutical excipients used in solid dosage forms

PubMed Central

2013-01-01

Background The compatibility study of active substances with excipients finds an important role in the domain of pharmaceutical research, being known the fact that final formulation is the one administered to the patient. In order to evaluate the compatibility between active substance and excipients, different analytical techniques can be used, based on their accuracy, reproducibility and fastness. Results Compatibility study of two well-known active substances, procaine and benzocaine, with four commonly used excipients, was carried out employing thermal analysis (TG/DTG/HF) and Fourier Transform Infrared Spectroscopy (UATR-FT-IR). The selected excipients were microcrystalline cellulose, lactose monohydrate, magnesium stearate and talc. Equal proportion of active substance and excipients (w/w) was utilized in the interaction study. The absolute value of the difference between the melting point peak of active substances and the one corresponding for the active substances in the analysed mixture, as well the absolute value of the difference between the enthalpy of the pure active ingredient melting peak and that of its melting peak in the different analysed mixtures were chosen as indexes of the drug-excipient interaction degree. All the results obtained through thermal analysis were also sustained by FT-IR spectroscopy. Conclusions The corroboration of data obtained by thermal analysis with the ones from FT-IR spectroscopy indicated that no interaction occurs between procaine and benzocaine, with microcrystalline cellulose and talc, as well for the benzocaine-lactose mixture. Interactions were confirmed between procaine and benzocaine respectively and magnesium stearate, and for procaine and lactose. PMID:23962059
Application of second derivative spectroscopy for increasing molecular specificity of Fourier transform infrared spectroscopic imaging of articular cartilage.

PubMed

Rieppo, L; Saarakkala, S; Närhi, T; Helminen, H J; Jurvelin, J S; Rieppo, J

2012-05-01

Fourier transform infrared (FT-IR) spectroscopic imaging is a promising method that enables the analysis of spatial distribution of biochemical components within histological sections. However, analysis of FT-IR spectroscopic data is complicated since absorption peaks often overlap with each other. Second derivative spectroscopy is a technique which enhances the separation of overlapping peaks. The objective of this study was to evaluate the specificity of the second derivative peaks for the main tissue components of articular cartilage (AC), i.e., collagen and proteoglycans (PGs). Histological bovine AC sections were measured before and after enzymatic removal of PGs. Both formalin-fixed sections (n = 10) and cryosections (n = 6) were investigated. Relative changes in the second derivative peak heights caused by the removal of PGs were calculated for both sample groups. The results showed that numerous peaks, e.g., peaks located at 1202 cm(-1) and 1336 cm(-1), altered less than 5% in the experiment. These peaks were assumed to be specific for collagen. In contrast, two peaks located at 1064 cm(-1) and 1376 cm(-1) were seen to alter notably, approximately 50% or more. These peaks were regarded to be specific for PGs. The changes were greater in cryosections than formalin-fixed sections. The results of this study suggest that the second derivative spectroscopy offers a practical and more specific method than routinely used absorption spectrum analysis methods to obtain compositional information on AC with FT-IR spectroscopic imaging. Copyright © 2012 Osteoarthritis Research Society International. Published by Elsevier Ltd. All rights reserved.
Identification of authentic and adulterated Aquilariae Lignum Resinatum by Fourier transform infrared (FT-IR) spectroscopy and two-dimensional correlation analysis

NASA Astrophysics Data System (ADS)

Qu, Lei; Chen, Jian-bo; Zhou, Qun; Zhang, Gui-jun; Sun, Su-qin; Guo, Yi-zhen

2016-11-01

As a kind of expensive perfume and valuable herb, the commercial Aquilariae Lignum Resinatum (ALR) is often adulterated for economic motivations. In this research, Fourier transform infrared (FT-IR) spectroscopy and two-dimensional (2D) correlation analysis are employed to establish a simple and quick identification method for the authentic and adulterated ALR. In the conventional infrared spectra, the standard ALR has a strong peak at 1658 cm-1 referring to the conjugated carbonyl of resin, while this peak is absent in the adulterated samples. The position, intensity, and shape of the auto-peaks and cross-peaks of the authentic and adulterated ALR are much different in the synchronous 2D correlation spectra with thermal perturbation. In the range of 1700-1500 cm-1, the standard ALR has four obvious auto-peaks, while the strongest one is at 1659 cm-1. The adulterated sample w-1 has three obvious auto-peaks and the strongest one is at 1647 cm-1. The adulterated sample w-2 has three obvious auto-peaks and the strongest one is at 1519 cm-1. The adulterated sample w-3 has four obvious auto-peaks and the strongest one is at 1690 cm-1. The above auto-peaks confirm that the standard ALR contains a certain content of resin compounds, while the three counterfeits contain little or different resins. The results show the potential of FT-IR spectroscopy and 2D correlation analysis in the simple and quick identification of authentic and adulterated ALR.
Study of structural and optical properties of YAG and Nd:YAG single crystals

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

Kostić, S.; Lazarević, Z.Ž., E-mail: lzorica@yahoo.com; Radojević, V.

2015-03-15

Highlights: • Transparent YAG and pale pink Nd:YAG single crystals were produced by the Czochralski technique. • Growth mechanisms and shape of the liquid/solid interface and incorporation of Nd{sup 3+} were studied. • The structure of the crystals was investigated by X-ray diffraction, Raman and IR spectroscopy. • The 15 Raman and 17 IR modes were observed. • The obtained YAG and Nd:YAG single crystals were without core and of good optical quality. - Abstract: Yttrium aluminum garnet (YAG, Y{sub 3}Al{sub 5}O{sub 12}) and yttrium aluminum garnet doped with neodymium (Nd:YAG) single crystals were grown by the Czochralski technique. Themore » critical diameter and the critical rate of rotation were calculated. Suitable polishing and etching solutions were determined. As a result of our experiments, the transparent YAG and pale pink Nd:YAG single crystals were produced. The obtained crystals were studied by X-ray diffraction, Raman and IR spectroscopy. The crystal structure was confirmed by XRD. The 15 Raman and 17 IR modes were observed. The Raman and IR spectroscopy results are in accordance with X-ray diffraction analysis. The obtained YAG and Nd:YAG single crystals were without core and of good optical quality. The absence of a core was confirmed by viewing polished crystal slices. Also, it is important to emphasize that the obtained Nd:YAG single crystal has a concentration of 0.8 wt.% Nd{sup 3+} that is characteristic for laser materials.« less
FT-Raman, FT-IR spectra and total energy distribution of 3-pentyl-2,6-diphenylpiperidin-4-one: DFT method.

PubMed

Subashchandrabose, S; Saleem, H; Erdogdu, Y; Rajarajan, G; Thanikachalam, V

2011-11-01

FT-Raman and FT-IR spectra were recorded for 3-pentyl-2,6-diphenylpiperidin-4-one (PDPO) sample in solid state. The equilibrium geometries, harmonic vibrational frequencies, infrared and the Raman scattering intensities were computed using DFT/6-31G(d,p) level. Results obtained at this level of theory were used for a detailed interpretation of the infrared and Raman spectra, based on the total energy distribution (TED) of the normal modes. Molecular parameters such as bond lengths, bond angles and dihedral angles were calculated and compared with X-ray diffraction data. This comparison was good agreement. The intra-molecular charge transfer was calculated by means of natural bond orbital analysis (NBO). Hyperconjugative interaction energy was more during the π-π* transition. Energy gap of the molecule was found using HOMO and LUMO calculation, hence the less band gap, which seems to be more stable. Atomic charges of the carbon, nitrogen and oxygen were calculated using same level of calculation. Copyright © 2011 Elsevier B.V. All rights reserved.
Spectroscopic characterization of natural calcite minerals.

PubMed

Gunasekaran, S; Anbalagan, G

2007-11-01

The FT-IR, FT-Raman, NMR spectral data of ten different limestone samples have been compared. FT-IR and FT-Raman spectral data show that calcium carbonate in limestone, principally in the form of calcite, as identified by its main absorption bands at 1426, 1092, 876 and 712 cm(-1). The sharp diffractions at the d-spacings, 3.0348, 1.9166 and 1.8796 confirm the presence of calcite structure and the calculated lattice parameters are: a=4.9781 A, c=17.1188 A. The range of 13C chemical shifts for different limestone samples is very small, varying from 198.38 to 198.42 ppm. The observed chemical shifts are consistent with the identical C-O bonding in different limestone samples. 27Al MAS NMR spectra of the samples exhibit a central line at 1 ppm and another line at 60 ppm corresponding to octahedral and tetrahedral Al ions, respectively. The five component resonances were observed in 29Si MAS NMR spectrum of limestone and these resonances were assigned to Si (4 Al), Si (3 Al), Si (2 Al), Si (1 Al) and Si (0 Al) from low field to high field.
FT-IR, FT-Raman and UV-visible spectra of potassium 3-furoyltrifluoroborate salt

NASA Astrophysics Data System (ADS)

Iramain, Maximiliano A.; Davies, Lilian; Brandán, Silvia Antonia

2018-04-01

The potassium 3-furoyltrifluoroborate salt has been experimentally characterized by means of FT-IR, FT-Raman and UV-Visible spectroscopies. Here, the predicted FT-IR, FT-Raman and UV-visible spectra by using theoretical B3LYP/6-31G* and 6-311++G** calculations show very good correlations with the corresponding experimental ones. The solvation energies were predicted by using both levels of calculations. The NBO analyses reveal the high stability of the salt by using the B3LYP/6-31G* level of theory while the AIM studies evidence the ionic characteristics of the salt in both media. The strong blue colour observed on the K atom by using the molecular electrostatic potential mapped suggests that this region act as typical electrophilic site. The gap values have revealed that the salt in gas phase is more reactive than in solution, as was reported in the literature while, the F13⋯H6 interaction together with the Ksbnd O bond observed by the studies of their charges could probably modulate the reactivities of this salt in aqueous solution. The force fields were computed with the SQMFF methodology and the Molvib program to perform the complete vibrational analysis. Then, the 39 vibration normal modes classified as 26 A'+ 13 A″ were completely assigned and their force constants are also reported.
Synchrotron FTIR Imaging For The Identification Of Cell Types Within Human Tissues

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

Walsh, Michael J.; Pounder, F. Nell; Nasse, Michael J.

2010-02-03

The use of synchrotron Fourier Transform Infrared spectroscopy (S-FTIR) has been shown to be a very promising tool for biomedical research. S-FTIR spectroscopy allows for the fast acquisition of infrared (IR) spectra at a spatial resolution approaching the IR diffraction limit. The development of the Infrared Environmental Imaging (IRENI) beamline at the Synchrotron Radiation Center (SRC) at the University of Wisconsin-Madison has allowed for diffraction limited imaging measurements of cells in human prostate and breast tissues. This has allowed for the identification of cell types within tissues that would otherwise not have been resolvable using conventional FTIR sources.
Novel synergistic transparent k-Carrageenan/Xanthan gum/Gellan gum hydrogel film: Mechanical, thermal and water barrier properties.

PubMed

Balasubramanian, R; Kim, Sam Soo; Lee, Jaewoong

2018-06-24

The aim is to develop novel synergistic transparent k-Carrageenan/Xanthan gum/Gellan gum (k-C/X/G) hydrogel films with different weight ratio composition and to study the effect of these compositions on the physical properties of the films. The structure and morphological properties of the films were investigated by Fourier-transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), X-ray diffraction (XRD) and differential scanning calorimeter (DSC). Results for FT-IR, DSC and SEM analysis showed a clear interaction between k-C, X, and G to form a new material. The mechanical, thermal and water barrier properties such as water vapor permeability (WVP), water contact angle (WCA) and moisture content were determined. The temperature at 5% weight loss (T 5% ) are in the range of 64.2-121.9 °C. The WVP exhibits are in the range of 1.8-2.4, contact angle are in the range of 32-65.8° and moisture content 16.5-21.51. The hydrogel film had good tensile strength of 19.1-31.0 MPa and elongation at break of 13-19% and tensile modulus of 1.6-2.4 GPa. The UV results indicate that the films were very transparent. The range of properties of the ternary k-C/X/G hydrogel films suggest that the presence molecular interaction and cross linking within the blends. Copyright © 2018. Published by Elsevier B.V.
Evaluation of SLS: APG mixed surfactant systems as carrier for solid dispersion.

PubMed

Patel, Ashok R; Joshi, Vishal Y

2008-01-01

The present investigation aims at studying the effect of mixed surfactant system of sodium lauryl sulphate (SLS) and alkyl polyglucosides (C(10)APG, C(12)APG and C(12/14)APG) on dissolution rate enhancement of poorly water soluble drug. Aceclofenac--a non-steroidal anti-inflammatory agent was used as a model drug as it has limited water solubility. The influence of the surfactant concentration in various blends on dissolution rate of Solid Dispersion (SD), prepared using solution method with ethanol as the solvent was studied and the advantage of mixed surfactant systems over the individual surfactants was illustrated by differences in the in-vitro dissolution profiles of SD. Physico chemical evaluation (critical micellar concentration, zeta potential and beta-parameter calculations) was carried out to study the mixed surfactant systems. Solid mixtures were characterized by Infrared spectroscopy (FT-IR); X-ray diffraction studies (XRD) and scanning electron microscopy (SEM). It was seen that the dissolution rate of aceclofenac from SD increased with the increase in the APG proportion relative to SLS with the optimum ratio of 0.2 SLS:0.8 APG showing the best effect in all cases. Results obtained from physico-chemical evaluation (the decrease in the value of critical micelle concentration and higher negative value of beta-parameters) suggested the existence of synergism between surfactants blends. The observed results in the dissolution rate enhancement could be attributed to the drug--surfactant interactions as evident from FT-IR, SEM and XRD results.
Structural and electrical characterization of annealed Si1-xCx/SiC thin film prepared by magnetron sputtering

NASA Astrophysics Data System (ADS)

Huang, Shi-Hua; Liu, Jian

2014-05-01

Si-rich Si1—xCx /SiC multilayer thin films are prepared using magnetron sputtering, subsequently followed by thermal annealing in the range of 800-1200 °C. The influences of annealing temperature (Ta) on the formation of Si and/or SiC nanocrystals (NCs) and on the electrical characteristics of the multilayer film are investigated by using a variety of analytical techniques, including X-ray diffraction (XRD), Raman spectroscopy and Fourier transform infrared spectrometry (FT-IR), current—voltage (I—V) technique, and capacitance-voltage (C—V) technique. XRD and Raman analyses indicate that Si NCs begin to form in samples for Ta >= 800 °C. At annealing temperatures of 1000 °C or higher, the formation of Si NCs is accompanied by the formation of SiC NCs. With the increase in the annealing temperature, the shift of FT-IR Si—C bond absorption spectra toward a higher wave number along with the change of band shape can be explained by a Si—C transitional phase between the loss of substitutional carbon and the formation of SiC precipitates and a precursor for the growth of SiC crystalline. The C—V and I—V results indicate that the interface quality of Si1—xCx/SiC multilayer film is improved significantly and the leakage current is reduced rapidly for Ta >= 1000 °C, which can be ascribed to the formation of Si and SiC NCs.
Preparation and characterization of chitosan-natural nano hydroxyapatite-fucoidan nanocomposites for bone tissue engineering.

PubMed

Lowe, Baboucarr; Venkatesan, Jayachandran; Anil, Sukumaran; Shim, Min Suk; Kim, Se-Kwon

2016-12-01

Solid three dimensional (3D) composite scaffolds for bone tissue engineering were prepared using the freeze-drying method. The scaffolds were composed of chitosan, natural nano-hydroxyapatite (nHA) and fucoidan in the following combinations: chitosan, chitosan-fucoidan, chitosan-nHA, and chitosan-nHA-fucoidan. Fourier transform infrared spectroscopy (FT-IR), thermal gravimetric analysis (TGA), X-ray diffraction analysis (XRD), scanning electron microscopy (SEM), and optical microscopy (OM) were used to determine the physiochemical constituents and the morphology of the scaffolds. The addition of nHA into the chitosan-fucoidan composite scaffold reduced the water uptake and water retention. FT-IR analysis confirmed the presence of a phosphate group in the chitosan-nHA-fucoidan scaffold. This group is present because of the presence of nHA (isolated via alkaline hydrolysis from salmon fish bones). Microscopic results indicated that the dispersion of nHA and fucoidan in the chitosan matrix was uniform with a pore size of 10-400μm. The composite demonstrated a suitable micro architecture for cell growth and nutrient supplementation. This compatibility was further elucidated in vitro using periosteum-derived mesenchymal stem cells (PMSCs). The cells demonstrated high biocompatibility and excellent mineralization for the chitosan-nHA-fucoidan scaffold. We believe that a chitosan-nHA-fucoidan composite is a promising biomaterial for the scaffold that can be used for bone tissue regeneration. Copyright © 2016 Elsevier B.V. All rights reserved.
Characterization of rice starch-ι-carrageenan biodegradable edible film. Effect of stearic acid on the film properties.

PubMed

Thakur, Rahul; Saberi, Bahareh; Pristijono, Penta; Golding, John; Stathopoulos, Costas; Scarlett, Christopher; Bowyer, Michael; Vuong, Quan

2016-12-01

The main aim of this study was to develop rice starch (RS), ι-carrageenan (ι-car) based film. Different formulations of RS (1-4%, w/w), ι-car (0.5-2%, w/w) was blended with stearic acid (SA; 0.3-0.9%, w/w) and glycerol (1%, w/w) as a plasticizer. The effect of film ingredients on the thickness, water vapour permeability (WVP), film solubility (FS), moisture content (MC), colour, film opacity (FO), tensile strength (TS), elongation-at-break (EAB) of film was examined. Interactions and miscibility of partaking components was studied by using Fourier transform infrared spectroscopy (FT-IR) and X-ray diffraction (XRD). Hydrocolloid suspension solution of mix polysaccharides imparted a significant impact (p<0.05) on the important attributes of resulting edible film. TS and EAB of film were improved significantly (p<0.05) when ι-car was increased in the film matrix. Formulation F1 comprising 2% ι-car, 2% RS, 0.3% SA, Gly 30% w/w and 0.2% surfactant (tween ® 20) provided film with good physical, mechanical and barrier properties. FT-IR and XRD results reveal that molecular interactions between RS-ι-car have a great impact on the film properties confining the compatibility and miscibility of mixed polysaccharide. Results of the study offers new biodegradable formulation for application on fruit and vegetables. Copyright © 2016 Elsevier B.V. All rights reserved.
Sustained release effects of berberine-loaded chitosan microspheres on in vitro chondrocyte culture.

PubMed

Zhou, Yan; Liu, Shiqing; Ming, Jianghua; Li, Yaming; Deng, Ming; He, Bin

2017-10-01

The low bioavailability and short biological half-life of berberine chloride (BBR) negatively affect the protective role of this compound against osteoarthritis (OA). The present study was performed to evaluate the effectiveness of sustained BBR release system. Novel BBR-loaded chitosan microspheres (BBR-loaded CMs) were successfully synthesized using an ionic cross-linking method for sustained release. The basic characteristics of the prepared microspheres were subsequently evaluated by scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD) techniques, encapsulation efficiency (EE), and in vitro release experiments. BBR-loaded CMs displayed spherical forms to encapsulate a considerable quantity of BBR (100.8 ± 2.7 mg/g); these microspheres also exhibited an ideal releasing profile. The FT-IR spectra and XRD results revealed that BBR-loaded CMs were successfully synthesized via electrostatic interaction. In vitro experiments further showed that BBR-loaded CMs significantly inhibited sodium nitroprusside (SNP)-stimulated chondrocyte apoptosis as well as cytoskeletal remodeling, and led to increasing mitochondrial membrane potential and maintaining the nuclear morphology. BBR-loaded CMs exerted markedly higher anti-apoptotic activity in the treatment of OA, and markedly inhibited the protein expression levels of caspase-3, a disintegrin, and metalloproteinase with thrombospondin motifs (ADAMTS)-5 and matrix metalloproteinase (MMP)-13 induced by SNP in rat articular chondrocytes, compared with free BBR at equivalent concentration. Therefore, novel BBR-loaded CMs may offer potential for application in the treatment of OA.
Preparation and characterization of azithromycin--Aerosil 200 solid dispersions with enhanced physical stability.

PubMed

Li, Xuechao; Peng, Huanhuan; Tian, Bin; Gou, Jingxin; Yao, Qing; Tao, Xiaoguang; He, Haibing; Zhang, Yu; Tang, Xing; Cai, Cuifang

2015-01-01

The main purpose of this study was to investigate the feasibility of azithromycin (AZI)--Aerosil 200 solid dispersions specifically with high stability under accelerated condition (40 °C/75% RH). Ball milling (BM) and hot-melt extrusion (HME) were used to prepare AZI solid dispersions. The physical properties of solid dispersions were evaluated by differential scanning calorimetry (DSC), scanning electron microscopy (SEM), powder X-ray diffraction (PXRD), Fourier transform infrared spectroscopy (FT-IR) and thermogravimetric analysis (TGA). For solid dispersions prepared with both methods, no crystalline of AZI was detected (except for AZI: Aerosil 200=75:25) by DSC or PXRD, indicating the amorphous state of AZI in solid dispersions. The FT-IR results demonstrated the loss of crystallization water and the formation of hydrogen bonds between Aerosil 200 and AZI during the preparation of solid dispersions. After 4 weeks storage under accelerated condition, the degree of crystallinity of AZI increased in solid dispersions prepared by BM, whereas for solid dispersions containing AZI, Aerosil 200 and glyceryl behenate (GB) prepared by HME, no crystalline of AZI was identified. This high stability can be attributed to the hydrophobic properties of GB and the presence of hydrogen bonds. Based on the above results, it is inferred the protection of hydrogen bonds between AZI and Aerosil 200 formed during preparation process effectively inhibited the recrystallization of AZI and improved the physical stability of amorphous AZI in the presence of Aerosil 200. Copyright © 2015 Elsevier B.V. All rights reserved.
Synthesis and structure analysis of ferrocene-containing pseudopeptides.

PubMed

Angelici, Gaetano; Górecki, Marcin; Pescitelli, Gennaro; Zanna, Nicola; Monari, Magda; Tomasini, Claudia

2017-10-23

Ferrocene with its aromaticity and facile redox properties is an attractive moiety to be incorporated into functional moieties. Medicinal applications of ferrocene are well known and ferrocene itself shows cytotoxic and antianemic properties. In this article, we will describe the synthesis and the structure analysis of two pseudopeptides containing a ferrocene moiety as N-terminal group. After purification, Fc-l-Phe-d-Oxd-OBn [l-Phel-phenylalanine; d-Oxd(4R,5S)-4-Methyl-5-carboxy-oxazolidin-2-one] appears as bright brown solid that spontaneously forms brown needles. The X-ray diffraction of the crystals shows the presence of strong π interactions between the ferrocenyl moiety and the phenyl rings, while no NH•••OC hydrogen bonds are formed. This result is confirmed by FT-IR and 1 H NMR analysis. In contrast, both FT-IR and 1 H NMR analysis suggest that Fc-(l-Phe-d-Oxd) 2 -OBn forms a turn conformation stabilized by intramolecular NH•••OC hydrogen bonds in solution. Chiroptical spectroscopies (ECD and VCD) substantially confirmed the absence of a well-defined folded structure. The presence of the Fc moiety is responsible for specific ECD signals, one of which displayed pronounced temperature dependence and is directly related with the helicity assumed by the Fc core. Solid-state ECD spectra were recorded and rationalized on the basis of the X-ray geometry and quantum-mechanical calculations. © 2017 Wiley Periodicals, Inc.
Characterization of process-induced damage in Cu/low-k interconnect structure by microscopic infrared spectroscopy with polarized infrared light

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

Seki, Hirofumi, E-mail: Hirofumi-Seki@trc.toray.co.jp; Hashimoto, Hideki; Ozaki, Yukihiro

Microscopic Fourier-transform infrared (FT-IR) spectra are measured for a Cu/low-k interconnect structure using polarized IR light for different widths of low-k spaces and Cu lines, and for different heights of Cu lines, on Si substrates. Although the widths of the Cu line and the low-k space are 70 nm each, considerably smaller than the wavelength of the IR light, the FT-IR spectra of the low-k film were obtained for the Cu/low-k interconnect structure. A suitable method was established for measuring the process-induced damage in a low-k film that was not detected by the TEM-EELS (Transmission Electron Microscope-Electron Energy-Loss Spectroscopy) using microscopicmore » IR polarized light. Based on the IR results, it was presumed that the FT-IR spectra mainly reflect the structural changes in the sidewalls of the low-k films for Cu/low-k interconnect structures, and the mechanism of generating process-induced damage involves the generation of Si-OH groups in the low-k film when the Si-CH{sub 3} bonds break during the fabrication processes. The Si-OH groups attract moisture and the OH peak intensity increases. It was concluded that the increase in the OH groups in the low-k film is a sensitive indicator of low-k damage. We achieved the characterization of the process-induced damage that was not detected by the TEM-EELS and speculated that the proposed method is applicable to interconnects with line and space widths of 70 nm/70 nm and on shorter scales of leading edge devices. The location of process-induced damage and its mechanism for the Cu/low-k interconnect structure were revealed via the measurement method.« less
Calculating cellulose diffraction patterns

USDA-ARS?s Scientific Manuscript database

Although powder diffraction of cellulose is a common experiment, the patterns are not widely understood. The theory is mathematical, there are numerous different crystal forms, and the conventions are not standardized. Experience with IR spectroscopy is not directly transferable. An awful error, tha...
DOE Office of Scientific and Technical Information (OSTI.GOV)

Johnson, Timothy J.; Weise, David; Lincoln, E. N.

Objectives: Project RC-1649, “Advanced Chemical Measurement of Smoke from DoD-prescribed Burns” was undertaken to use advanced instrumental techniques to study in detail the particulate and vapor-phase chemical composition of the smoke that results from prescribed fires used as a land management tool on DoD bases, particularly bases in the southeastern U.S. The statement of need (SON) called for “(1) improving characterization of fuel consumption” and “(2) improving characterization of air emissions under both flaming and smoldering conditions with respect to volatile organic compounds, heavy metals, and reactive gases.” The measurements and fuels were from several bases throughout the southeast (Campmore » Lejeune, Ft. Benning, and Ft. Jackson) and were carried out in collaboration and conjunction with projects 1647 (models) and 1648 (particulates, SW bases). Technical Approach: We used an approach that featured developing techniques for measuring biomass burning emission species in both the laboratory and field and developing infrared (IR) spectroscopy in particular. Using IR spectroscopy and other methods, we developed emission factors (EF, g of effluent per kg of fuel burned) for dozens of chemical species for several common southeastern fuel types. The major measurement campaigns were laboratory studies at the Missoula Fire Sciences Laboratory (FSL) as well as field campaigns at Camp Lejeune, NC, Ft. Jackson, SC, and in conjunction with 1648 at Vandenberg AFB, and Ft. Huachuca. Comparisons and fusions of laboratory and field data were also carried out, using laboratory fuels from the same bases. Results: The project enabled new technologies and furthered basic science, mostly in the area of infrared spectroscopy, a broadband method well suited to biomass burn studies. Advances in hardware, software and supporting reference data realized a nearly 20x improvement in sensitivity and now provide quantitative IR spectra for potential detection of ~60 new species and actual field quantification of several new species such as nitrous acid, glycolaldehyde, α-/β-pinene and D-limonene. The new reference data also permit calculation of the global warming potential (GWP) of the greenhouse gases by enabling 1) detection of their ambient concentrations, and 2) quantifying their ability to absorb IR radiation.« less

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