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.

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.

Effect of substituent of terpyridines on the in vitro antioxidant, antitubercular, biocidal and fluorescence studies of copper(II) complexes with clioquinol

NASA Astrophysics Data System (ADS)

Kharadi, G. J.

2014-01-01

An octahedral complexes of copper with clioquinol(CQ) and substituted terpyridine have been synthesized. The Cu(II) complexes have been characterized by elemental analyses, thermogravimetric analyses, magnetic moment measurements, FT-IR, electronic, 1H NMR and FAB mass spectra. Antimycobacterial screening of ligand and its copper compound against Mycobacterium tuberculosis shows clear enhancement in the antitubercular activity upon copper complexation. Ferric-reducing anti-oxidant power of all complexes were measured. The fluorescence spectra of complexes show red shift, which may be due to the chelation by the ligands to the metal ion. It enhances ligand ability to accept electrons and decreases the electron transition energy. The antimicrobial efficiency of the complexes were tested on five different microorganisms and showed good biological activity.

Evaluation of inflammatory processes by FTIR spectroscopy.

PubMed

Rodrigues, Laís Morandini; Carvalho, Luís Felipe das Chagas E Silva; Bonnier, Franck; Anbinder, Ana Lia; Martinho, Herculano da Silva; Almeida, Janete Dias

2018-04-01

Fourier transform infrared (FTIR) spectroscopy is a powerful diagnosis technique and has been used to identify patterns of molecular changes based on vibration modes. The objective of this study was to evaluate inflammatory fibrous hyperplasia (IFH) lesions and oral normal mucosa (NM) initially with histopathological exam and then using micro-FTIR spectroscopy to analyse the samples. Eleven IFH and 11 NM samples were analysed at five different points to cover the largest area possible by the micro-FTIR technique. Bands were observed between 970 and 1743 cm -1 which corresponded to different structural components like collagen, lipids, fatty acids, proteins and amino acids. Spectral bands were more intense mostly for IFH lesions, including collagen bands, which are an important component of inflammatory fibrous hyperplasia. This study demonstrated that differentiation in the inflammatory tissue was observed in FTIR spectral differences, in terms of biochemical composition.

Ni(II)-tetrahedral complexes: Characterization, antimicrobial properties, theoretical studies and a new family of charge-transfer transitions

NASA Astrophysics Data System (ADS)

Sarı, Nurşen; Şahin, Songül Çiğdem; Öğütcü, Hatice; Dede, Yavuz; Yalcin, Soydan; Altundaş, Aliye; Doğanay, Kadir

2013-04-01

A new amine containing selenium and their five imine, (SeSchX)(X: -H, F, Cl, Br, CH3), and Ni (II) complexes, [Ni(SeSchX)(H2O)2]Cl/[Ni(SeSchCl)(H2O)Cl], were synthesized. The compounds were characterized by means of elemental analyses, 13C and 1H NMR (for imine), FT-IR, UV-Visible spectroscopy, TGA/DTA and elemental analyses. [Ni(SeSchCl)(H2O)Cl] complex from Ni(II) complexes changes color from yellow to orange in the range pH 5-7. [Ni(SeSchCl)(H2O)Cl] complex has ligand-to-metal charge-transfer (LMCT) transitions in the basic medium. Excitation characteristics and energetic of [Ni(SeSchCl)(H2O)Cl] complex, examined via TD-DFT calculations, reveals transitions of LMCT and π → π* character that matches the experimental values. [Ni(SeSchCl)(H2O)Cl] complex showed the highest antibacterial activity when compared to other complexes reported in this work.

Using new hetero-spectral two-dimensional correlation analyses and synchrotron-radiation-based spectromicroscopy to characterize binding of Cu to soil dissolved organic matter.

PubMed

Sun, Fusheng; Li, Yaqing; Wang, Xiang; Chi, Zhilai; Yu, Guanghui

2017-04-01

Understanding the binding characteristics of copper (Cu) to different functional groups in soil dissolved organic matter (DOM) is important to explore Cu toxicity, bioavailability and ultimate fate in the environment. However, the methods used to explore such binding characteristics are still limited. Here, two-dimensional correlation spectroscopy (2DCOS) integrated with Fourier transform infrared (FTIR), 29 Si nuclear magnetic resonance (NMR), 27 Al NMR, and synchrotron-radiation-based FTIR spectromicroscopy were used to explore the binding characteristics of Cu to soil DOM as part of a long-term (23 years) fertilization experiment. Compared with no fertilization and inorganic fertilization (NPK), long-term pig manure fertilization (M) treatment significantly increased the concentration of total and bioavailable Cu in soils. Furthermore, hetero-spectral 2DCOS analyses demonstrated that the binding characteristics of Cu onto functional groups in soil DOM were modified by fertilization regimes. In the NPK treatment, Cu was bound to aliphatic C, whereas in the manure treatment SiO groups had higher affinity toward Cu than aliphatic C. Also, the sequence of binding of functional groups to Cu was modified by the fertilization treatments. Moreover, synchrotron-radiation-based FTIR spectromicroscopy showed that Cu, clay minerals and sesquioxides, and C functional groups were heterogeneously distributed at the micro-scale. Specifically, clay-OH as well as mineral elements had a distribution pattern similar to Cu, but certain (but not all) C forms showed a distribution pattern inconsistent with that of Cu. The combination of synchrotron radiation spectromicroscopy and 2DCOS is a useful tool in exploring the interactions among heavy metals, minerals and organic components in soils. Copyright © 2017 Elsevier Ltd. All rights reserved.

A structural study of fentanyl by DFT calculations, NMR and IR spectroscopy

NASA Astrophysics Data System (ADS)

Asadi, Zahra; Esrafili, Mehdi D.; Vessally, Esmail; Asnaashariisfahani, Manzarbanou; Yahyaei, Saeideh; Khani, Ali

2017-01-01

N-(1-(2-phenethyl)-4-piperidinyl-N-phenyl-propanamide (fentanyl) is synthesized and characterized by FT-IR, 1H NMR, 13C NMR, mass spectroscopy and elemental analyses. The geometry optimization is performed using the B3LYP and M06 density functionals with 6-311 + G(d) and 6-311++G(d,p) basis sets. The complete assignments are performed on the basis of the potential energy distribution (PED) of the all vibrational modes. Almost a nice correlation is found between the calculated 13C chemical shifts and experimental data. The frontier molecular orbitals and molecular electrostatic potential of fentanyl are also obtained.

Synthesis and Antioxidant Activity of 2-Amino-5-methylthiazol Derivatives Containing 1,3,4-Oxadiazole-2-thiol Moiety

PubMed Central

Mohana, Kikkeri N.; Kumar, Chikkur B. Pradeep

2013-01-01

A series of new 5-(2-amino-5-methylthiazol-4-yl)-1,3,4-oxadiazole-2-thiol derivatives 6(a–j) were designed and synthesized with various substituted aldehydes. The chemical structures were confirmed by elemental analyses, FT-IR, 1H NMR, and mass spectral studies. The antioxidant activity of the synthesized compounds was evaluated by 2,2-diphenyl-1-picrylhydrazyl (DPPH), hydroxyl, nitric oxide, and superoxide radical scavenging assay methods. Compounds 6a, 6e, and 6c showed significant radical scavenging potential due to the presence of electron donating substituent on substituted aldehydes. PMID:24052865

Synthesis and Antioxidant Activity of 2-Amino-5-methylthiazol Derivatives Containing 1,3,4-Oxadiazole-2-thiol Moiety.

PubMed

Mohana, Kikkeri N; Kumar, Chikkur B Pradeep

2013-01-01

A series of new 5-(2-amino-5-methylthiazol-4-yl)-1,3,4-oxadiazole-2-thiol derivatives 6(a-j) were designed and synthesized with various substituted aldehydes. The chemical structures were confirmed by elemental analyses, FT-IR, (1)H NMR, and mass spectral studies. The antioxidant activity of the synthesized compounds was evaluated by 2,2-diphenyl-1-picrylhydrazyl (DPPH), hydroxyl, nitric oxide, and superoxide radical scavenging assay methods. Compounds 6a, 6e, and 6c showed significant radical scavenging potential due to the presence of electron donating substituent on substituted aldehydes.

[Detection of oil spills on water by differential polarization FTIR spectrometry].

PubMed

Yuan, Yue-ming; Xiong, Wei; Fang, Yong-hua; Lan, Tian-ge; Li, Da-cheng

2010-08-01

Detection of oil spills on water, by traditional thermal remote sensing, is based on the radiance contrast between the large area of clean water and the polluted area of water. And the categories of oil spills can not be identified by analysing the thermal infrared image. In order to find out the extent of pollution and identify the oil contaminants, an approach to the passive detection of oil spills on water by differential polarization FTIR spectrometry is proposed. This approach can detect the contaminants by obtaining and analysing the subtracted spectrum of horizontal and vertical polarization intensity spectrum. In the present article, the radiance model of differential polarization FTIR spectrometry is analysed, and an experiment about detection of No. O diesel and SF96 film on water by this method is presented. The results of this experiment indicate that this method can detect the oil contaminants on water without radiance contrast with clean water, and it also can identify oil spills by analysing the spectral characteristic of differential polarization FTIR spectrum. So it well makes up for the shortage of traditional thermal remote sensing on detecting oil spills on water.

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.

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

PubMed

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

2015-01-01

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

Syntheses, spectroscopic and thermal analyses of cyanide bridged heteronuclear polymeric complexes: [M(L)2Ni(CN)4]n (Ldbnd N-methylethylenediamine or N-ethylethylenediamine; Mdbnd Ni(II), Cu(II), Zn(II) or Cd(II))

NASA Astrophysics Data System (ADS)

Karaağaç, Dursun; Kürkçüoğlu, Güneş Süheyla

2016-02-01

Polymeric tetracyanonickelate(II) complexes of the type [M(L)2Ni(CN)4]n (Ldbnd N-methylethylenediamine (men) or N-ethylethylenediamine (neen); Mdbnd Ni(II), Cu(II), Zn(II) or Cd(II)) have been prepared and characterized by FT-IR, Raman spectroscopy, thermal and elemental analysis techniques. Additionally, FT-IR and Raman spectral analyses of men and neen have experimentally and theoretically investigated in the range of 4000-250 cm-1. The corresponding vibration assignments of men and neen are performed by using B3LYP density functional theory (DFT) method together with 6-31 G(d) basis set. The spectral features of the complexes suggest that the coordination environment of the M(II) ions are surrounded by the two symmetry related men and neen ligands and the two symmetry related N atom of cyanide groups, whereas the Ni(II) atoms are coordinated with a square-planar to four C atoms of the cyanide groups. Polymeric structures of the complexes consist of one dimensional alternative chains of [M(L)2]2+ and [Ni(CN)4]2- moieties. The thermal decompositions in the temperature range 30-700 °C of the complexes were investigated in the static air atmosphere.

Synthesis and spectroscopic characterization of 3,4-difluoroacetophenone-thiosemicarbazone and its palladium(II) complex: Evaluation of antimicrobial and antitumour activity

NASA Astrophysics Data System (ADS)

Jagadeesh, M.; Rashmi, H. K.; Subba Rao, Y.; Sreenath Reddy, A.; Prathima, B.; Uma Maheswari Devi, P.; Reddy, A. Varada

2013-11-01

A new cis-palladium(II)diaqua(3,4-difluoroacetophenonethiosemicarbazone complex (Pd(II) complex) is synthesized using 3,4-difluoroacetophenonethiosemicarbazone(L). The L and its Pd(II) complex are characterized and confirmed by elemental analyses, electrochemical analyses, FT-IR, FT-Raman, UV-Vis, HRMS and LC-MS techniques. Ligand L is further characterized by 1H, 13C and 19F NMR spectroscopy. The crystal structure of L is unambiguously characterized by single X-ray crystallography. The ligand (L) belongs to monoclinic system with P2(1)/C space group and the unit cell parameters are a(Å) = 9.1144(7), b(Å) = 13.7928(7), c(Å) = 8.4174(5), α(°) = 90, β(°) = 100.715, γ(°) = 90 and volume V(A3) = 1039.73(11). The Raman bands observed for the L and its Pd(II) complex are in good agreement with the FT-IR spectral data. The Pd(II) complex is found to be highly efficient in inhibiting the growth of human pathogens like Salmonella typhimurium and Klebsiella pneumonia with MIC value 10.0 μg/mL whose inhibition zones are almost comparable with the standard antibiotic. The synthesized compounds have shown antiproliferative activity against the human breast cancer cell lines MDA-MB231 by intermitting the regular pathway of ribonucleotidereductase.

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

PubMed

Pahla, G; Ntuli, F; Muzenda, E

2018-01-01

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

Plants and microbes assisted selenium nanoparticles: characterization and application

PubMed Central

2014-01-01

Selenium is an essential trace element and is an essential component of many enzymes without which they become inactive. The Se nanoparticles of varying shape and size may be synthesized from Se salts especially selenite and selenates in presence of reducing agents such as proteins, phenols, alcohols and amines. These biomolecules can be used to reduce Se salts in vitro but the byproducts released in the environment may be hazardous to flora and fauna. In this review, therefore, we analysed in depth, the biogenic synthesis of Se nanoparticles, their characterization and transformation into t- Se, m-Se, Se-nanoballs, Se-nanowires and Se-hollow spheres in an innocuous way preventing the environment from pollution. Their shape, size, FTIR, UV–vis, Raman spectra, SEM, TEM images and XRD pattern have been analysed. The weak forces involved in aggregation and transformation of one nano structure into the other have been carefully resolved. PMID:25128031

Plants and microbes assisted selenium nanoparticles: characterization and application.

PubMed

Husen, Azamal; Siddiqi, Khwaja Salahuddin

2014-08-16

Selenium is an essential trace element and is an essential component of many enzymes without which they become inactive. The Se nanoparticles of varying shape and size may be synthesized from Se salts especially selenite and selenates in presence of reducing agents such as proteins, phenols, alcohols and amines. These biomolecules can be used to reduce Se salts in vitro but the byproducts released in the environment may be hazardous to flora and fauna. In this review, therefore, we analysed in depth, the biogenic synthesis of Se nanoparticles, their characterization and transformation into t- Se, m-Se, Se-nanoballs, Se-nanowires and Se-hollow spheres in an innocuous way preventing the environment from pollution. Their shape, size, FTIR, UV-vis, Raman spectra, SEM, TEM images and XRD pattern have been analysed. The weak forces involved in aggregation and transformation of one nano structure into the other have been carefully resolved.

Characterization of Sorolla's gouache pigments by means of spectroscopic techniques

NASA Astrophysics Data System (ADS)

Roldán, Clodoaldo; Juanes, David; Ferrazza, Livio; Carballo, Jorgelina

2016-02-01

This paper presents the characterization of the Joaquín Sorolla's gouache sketches for the oil on canvas series "Vision of Spain" commissioned by A. M. Huntington to decorate the library of the Hispanic Society of America in New York. The analyses were focused on the identification of the elemental composition of the gouache pigments by means of portable EDXRF spectrometry in a non-destructive mode. Additionally, SEM-EDX and FTIR analyses of a selected set of micro-samples were carried out to identify completely the pigments, the paint technique and the binding media. The obtained results have confirmed the identification of lead and zinc white, vermillion, earth pigments, ochre, zinc yellow, chrome yellow, ultramarine, Prussian blue, chromium based and copper-arsenic based green pigments, bone black and carbon based black pigments, and the use of gum arabic as binding media in the gouache pigments.

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

PubMed

Dhanuskodi, S; Manivannan, S; Kirschbaum, K

2006-05-15

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

A Unique Collection of Palaeolithic Painted Portable Art: Characterization of Red and Yellow Pigments from the Parpalló Cave (Spain)

PubMed Central

Villaverde Bonilla, Valentín; Ródenas Marín, Isabel; Murcia Mascarós, Sonia

2016-01-01

In this work we analyze the pigments used in the decoration of red and yellow motifs present in the portable art of the Parpalló Cave (Gandía, Spain), one of the most important Palaeolithic sites in the Spanish Mediterranean region. Energy dispersive X-ray fluorescence spectrometry (EDXRF) and spectrophotometry in the visible region (CIEL*a*b*color coordinates and spectral reflectance curves) were used to perform in situ fast analyses of the red and yellow motifs with portable equipment and to characterize their elemental composition and their colorimetric perception, respectively. According to the elemental composition, the intensity of the fluorescence iron signals in red and yellow motifs are higher than average values in the rock substrates. As expected, red motifs possess high values of the chromatic coordinate a* and yellow motifs possess high values of b*. This characterization was complemented with FT-IR analyses of microsamples detached from the red and yellow colored zones of a small set of plaquettes. Our results show that the artists used red and yellow pigments in the decoration likely derived from natural iron oxides as hematite and goethite. PMID:27732605

A Unique Collection of Palaeolithic Painted Portable Art: Characterization of Red and Yellow Pigments from the Parpalló Cave (Spain).

PubMed

Roldán García, Clodoaldo; Villaverde Bonilla, Valentín; Ródenas Marín, Isabel; Murcia Mascarós, Sonia

2016-01-01

In this work we analyze the pigments used in the decoration of red and yellow motifs present in the portable art of the Parpalló Cave (Gandía, Spain), one of the most important Palaeolithic sites in the Spanish Mediterranean region. Energy dispersive X-ray fluorescence spectrometry (EDXRF) and spectrophotometry in the visible region (CIEL*a*b*color coordinates and spectral reflectance curves) were used to perform in situ fast analyses of the red and yellow motifs with portable equipment and to characterize their elemental composition and their colorimetric perception, respectively. According to the elemental composition, the intensity of the fluorescence iron signals in red and yellow motifs are higher than average values in the rock substrates. As expected, red motifs possess high values of the chromatic coordinate a* and yellow motifs possess high values of b*. This characterization was complemented with FT-IR analyses of microsamples detached from the red and yellow colored zones of a small set of plaquettes. Our results show that the artists used red and yellow pigments in the decoration likely derived from natural iron oxides as hematite and goethite.

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

PubMed Central

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

2017-01-01

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

Raman and FTIR spectroscopy of methane in olivine

NASA Astrophysics Data System (ADS)

Smith, A.; Oze, C.; Rossman, G. R.; Celestian, A. J.

2017-12-01

Olivine has been proposed to be a direct source of methane (CH4) in serpentinization systems and experiments. Here, Raman and Fourier Transform Infrared (FTIR) spectroscopy were used to verify the presence and abundance of CH4 in olivine samples from nine localities, including the San Carlos olivine. Raman analyses did not identify any methane in the olivine samples. As olivine is orthorhombic, three polarized FTIR spectra were obtained for the olivine samples. No methane was detected in any of the olivine samples using FTIR. Overall, olivine investigated in this study does not appear to be a primary source of methane.

Comparison of 13C Nuclear Magnetic Resonance and Fourier Transform Infrared spectroscopy for estimating humification and aromatization of soil organic matter

NASA Astrophysics Data System (ADS)

Rogers, K.; Cooper, W. T.; Hodgkins, S. B.; Verbeke, B. A.; Chanton, J.

2017-12-01

Solid state direct polarization 13C NMR spectroscopy (DP-NMR) is generally considered the most quantitatively reliable method for soil organic matter (SOM) characterization, including determination of the relative abundances of carbon functional groups. These functional abundances can then be used to calculate important soil parameters such as degree of humification and extent of aromaticity that reveal differences in reactivity or compositional changes along gradients (e.g. thaw chronosequence in permafrost). Unfortunately, the 13C NMR DP-NMR experiment is time-consuming, with a single sample often requiring over 24 hours of instrument time. Alternatively, solid state cross polarization 13C NMR (CP-NMR) can circumvent this problem, reducing analyses times to 4-6 hours but with some loss of quantitative reliability. Attenuated Total Reflectance Fourier Transform Infrared spectroscopy (ATR-FTIR) is a quick and relatively inexpensive method for characterizing solid materials, and has been suggested as an alternative to NMR for analysis of soil organic matter and determination of humification (HI) and aromatization (AI) indices. However, the quantitative reliability of ATR-FTIR for SOM analyses has never been verified, nor have any ATR-FTIR data been compared to similar measurements by NMR. In this work we focused on FTIR vibrational bands that correspond to the three functional groups used to calculate HI and AI values: carbohydrates (1030 cm-1), aromatics (1510, 1630 cm-1), and aliphatics (2850, 2920 cm-1). Data from ATR-FTIR measurements were compared to analogous quantitation by DP- and CP-NMR using peat samples from Sweden, Minnesota, and North Carolina. DP- and CP-NMR correlate very strongly, although the correlations are not always 1:1. Direct comparison of relative abundances of the three functional groups determined by NMR and ATR-FTIR yielded satisfactory results for carbohydrates (r2= 0.78) and aliphatics (r2=0.58), but less so for aromatics (r2= 0.395). ATR-FTIR has to this point been used primarily for relative abundance analyses (e.g. calculating HI and AI values), but these results suggest FTIR can provide quantitative reliability that approaches that of NMR.

Attenuated total internal reflection infrared microspectroscopic imaging using a large-radius germanium internal reflection element and a linear array detector.

PubMed

Patterson, Brian M; Havrilla, George J

2006-11-01

The number of techniques and instruments available for Fourier transform infrared (FT-IR) microspectroscopic imaging has grown significantly over the past few years. Attenuated total internal reflectance (ATR) FT-IR microspectroscopy reduces sample preparation time and has simplified the analysis of many difficult samples. FT-IR imaging has become a powerful analytical tool using either a focal plane array or a linear array detector, especially when coupled with a chemometric analysis package. The field of view of the ATR-IR microspectroscopic imaging area can be greatly increased from 300 x 300 microm to 2500 x 2500 microm using a larger internal reflection element of 12.5 mm radius instead of the typical 1.5 mm radius. This gives an area increase of 70x before aberrant effects become too great. Parameters evaluated include the change in penetration depth as a function of beam displacement, measurements of the active area, magnification factor, and change in spatial resolution over the imaging area. Drawbacks such as large file size will also be discussed. This technique has been successfully applied to the FT-IR imaging of polydimethylsiloxane foam cross-sections, latent human fingerprints, and a model inorganic mixture, which demonstrates the usefulness of the method for pharmaceuticals.

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

PubMed

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

2013-07-01

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

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

NASA Astrophysics Data System (ADS)

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

2011-07-01

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

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

NASA Astrophysics Data System (ADS)

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

2016-04-01

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

Methodological effects in Fourier transform infrared (FTIR) spectroscopy: Implications for structural analyses of biomacromolecular samples

NASA Astrophysics Data System (ADS)

Kamnev, Alexander A.; Tugarova, Anna V.; Dyatlova, Yulia A.; Tarantilis, Petros A.; Grigoryeva, Olga P.; Fainleib, Alexander M.; De Luca, Stefania

2018-03-01

A set of experimental data obtained by Fourier transform infrared (FTIR) spectroscopy (involving the use of samples ground and pressed with KBr, i.e. in a polar halide matrix) and by matrix-free transmission FTIR or diffuse reflectance infrared Fourier transform (DRIFT) spectroscopic methodologies (involving measurements of thin films or pure powdered samples, respectively) were compared for several different biomacromolecular substances. The samples under study included poly-3-hydroxybutyrate (PHB) isolated from cell biomass of the rhizobacterium Azospirillum brasilense; dry PHB-containing A. brasilense biomass; pectin (natural carboxylated heteropolysaccharide of plant origin; obtained from apple peel) as well as its chemically modified derivatives obtained by partial esterification of its galacturonide-chain hydroxyl moieties with palmitic, oleic and linoleic acids. Significant shifts of some FTIR vibrational bands related to polar functional groups of all the biomacromolecules under study, induced by the halide matrix used for preparing the samples for spectroscopic measurements, were shown and discussed. A polar halide matrix used for preparing samples for FTIR measurements was shown to be likely to affect band positions not only per se, by affecting band energies or via ion exchange (e.g., with carboxylate moieties), but also by inducing crystallisation of metastable amorphous biopolymers (e.g., PHB of microbial origin). The results obtained have important implications for correct structural analyses of polar, H-bonded and/or amphiphilic biomacromolecular systems using different methodologies of FTIR spectroscopy.

Development and Characterization of Edible Films Based on Fruit and Vegetable Residues.

PubMed

Andrade, Roberta M S; Ferreira, Mariana S L; Gonçalves, Édira C B A

2016-02-01

Edible films were developed from the solid residue of the processing of whole fruits and vegetables. The solid residue, processed into flour (FVR flour) was chemically and structurally characterized by microstructure, elemental composition, structural links, and moisture sorption isotherm. Films were prepared by casting using aqueous extracts of 8% and 10% of flour (w/w) and characterized in terms of thickness, water solubility, mechanical properties, water vapor permeability, and Fourier transform infrared (FTIR). The analysis of microstructure and elemental composition, performed on flour (mean particle size 350 μm), showed an essentially granular aspect, with the presence of fibrous particles having potassium as one of the most abundant elements. FTIR results showed similarity between the characteristic bands of other raw materials used in edible films. The sorption isotherm of FVR flour showed a typical profile of foods rich in soluble components, such as sugars. Dried films presented an average thickness of 0.263 ± 0.003 mm, a homogenous aspect, bright yellow color, pronounced fruit flavor, and high water solubility. The FTIR spectra of the edible films revealed that addition of potato skin flour did not change the molecular conformation. Moreover, the films presented low tensile strength at break when compared with fruit starch-based films. © 2016 Institute of Food Technologists®

Physico-chemistry and geochemistry of Balengou clay deposit (West Cameroon) with inference to an argillic hydrothermal alteration

NASA Astrophysics Data System (ADS)

Tassongwa, Bernard; Eba, François; Njoya, Dayirou; Tchakounté, Jacqueline Numbem; Jeudong, Narcisse; Nkoumbou, Charles; Njopwouo, Daniel

2017-09-01

Field description and sampling along two pits, granulometry, Atterberg limits, mineralogical (XRD, FTIR, DSC & TGA) and geochemical analyses of the Balengou clays help to determine their characteristics and the genesis of the deposit. The mineralogical composition is comprised of halloysite-kaolinite, quartz, montmorillonite, hematite, anatase, feldspar, zircon, chromite, and apatite. Gibbsite and illite occur at the shallow and deep depth, respectively. Dikes of sand-poor clays contain also cristobalite and tridymite. Pairs of elements Rb-Ba, Rb-Sr, Nb-Ta, Ta-Zr, TiO2-Zr display good positive correlations (R2 > 0.85). REE patterns are highly fractionated (LaN up to 3312, LaN/YbN: 19-10) and are marked by deep Ce and Eu negative anomalies. Immobile element canonical ratios indicate that the protoliths were commendite/pantelerite, rhyolite and dacite, or their plutonic equivalents. Mineralogical and geochemical features lead to the suggestion that the clays derived from an advanced argillic hydrothermal alteration.

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

Sukri, Shahratul Ain Mohd; Heng, Lee Yook; Karim, Nurul Huda Abd

A platinum (II) salphen complex was synthesised by condensation reaction of 2,4-dihydroxylbenzaldehyde and o-phenylenediamine with potassium tetrachloroplatinate to obtain N,N′-Bis-4-(hydroxysalicylidene)-phenylenediamine-platinum (II). The structure of the complex was confirmed by {sup 1}H and {sup 13}C NMR spectroscopy, FTIR spectroscopy, CHN elemental analyses and ESI-MS spectrometry. The platinum (II) salphen complex with four donor atoms N{sub 2}O{sub 2} from its salphen ligand coordinated to platinum (II) metal centre were determined. The binding mode and interaction of this complex with calf thymus DNA was determined by UV/Vis DNA titration and emission titration. The intercalation between the DNA bases by π-π stacking due tomore » its square planar geometry and aromatic rings structures was proposed.« less

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

NASA Astrophysics Data System (ADS)

Ajibade, Peter A.; Ejelonu, Benjamin C.

2013-09-01

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

The influence of organic-mineral complexes on micro-elements dynamic in ecological systems of vegetables cultivation

NASA Astrophysics Data System (ADS)

Bulgariu, D.; Buzgar, N.; Bulgariu, L.; Rusu, C.; Munteanu, N.

2009-04-01

In ecological systems of vegetable cultivation (hortic antrosols; soils from greenhouses), exists an ensemble of equilibriums between organic-mineral combinations, very sensitive even to relatively small variations of physical-chemical conditions in soils. As such, these can manifest a strong influence on organic matter, clay minerals and microelements from soil, which in turn impacts on the productivity of these soils and the quality of obtained products (vegetables, fruit). Although many studies consider these organic-mineral combinations are meta-stable combinations, our work has shown that the stability of organic-mineral combinations in hortic antrosols (especially for clay-humic, clay-ironhumic combinations and chelates) is higher. We believe that this is due to the higher flexibility of these combinations' structures with the variation of chemical-mineralogical composition and physical-chemical conditions in soil. This paper highlights the results of our research on the differentiation possibility of organic-mineral complexes, depending on their structure and composition (using Raman and FT-IR spectrometry) and the influences manifested by the organic-mineral complexes on the micro-elements dynamic from ecological systems of fresh vegetable cultivation. The non-destructive separation of organic-mineral compounds from soil samples was carried out through iso-dynamic magnetic separation and extraction in aqueous two-phase systems (PEG-based). The Raman and FT-IR spectrometry analyses on raw soil samples, extracts obtained from soil samples and separated mineral fractions have been supplemented by the results obtained through chemical, microscopic and thermal analyses and by UV-VIS absorption spectrometry. Ours experimental studies have been done on representative samples of hortic antrosol from Copou glasshouse (Iasi, Romania), and was studied five micro-elements: Zn, Ni, Cu, Mn, Cr and P. The total contents of the five microelements and their fractions differential bonded on mineral and organic components of hortic antrosols, have been determined by atomic absorption spectrometry after combined sequential extraction in solid phase extraction - aqueous biphasic (PEG based) systems. The specific mechanisms of the microelements interaction with organic components have been estimated on the basis of studies realized on fractions obtained after each extraction step by Raman and FTIR spectrometry. These data have been correlated with those obtained by chemical analysis and UV-VIS spectrometry. In conditions of hortic antrosol, from total contents of Zn, Ni, Cu, Mn and Cr, more than 65 % are binding on organic components. A specific phenomenon of hortic antrosols is the microelements complexation exclusively with the functional groups of organic macromolecules. This phenomenon has two important consequences: (i) the strong fixation of microelements (these can be extracted only in very extremely conditions, which implied the organic part destroying) and (ii) their presence determined major modifications in the structure, conformation and stability of organic macromolecules. Under these conditions, the type and structure of organic-mineral compounds represent determinant factors for the dynamic of micro-elements and organic compounds in ecological systems of vegetables cultivation. Acknowledgments The authors would like to acknowledge the financial support from Romanian Ministry of Education and Research (Project PNCDI 2-D5 no. 51045/07 an Project PNCDI 2-D5 no. 52141 / 08).

Predicting ambient aerosol thermal-optical reflectance measurements from infrared spectra: elemental carbon

NASA Astrophysics Data System (ADS)

Dillner, A. M.; Takahama, S.

2015-10-01

Elemental carbon (EC) is an important constituent of atmospheric particulate matter because it absorbs solar radiation influencing climate and visibility and it adversely affects human health. The EC measured by thermal methods such as thermal-optical reflectance (TOR) is operationally defined as the carbon that volatilizes from quartz filter samples at elevated temperatures in the presence of oxygen. Here, methods are presented to accurately predict TOR EC using Fourier transform infrared (FT-IR) absorbance spectra from atmospheric particulate matter collected on polytetrafluoroethylene (PTFE or Teflon) filters. This method is similar to the procedure developed for OC in prior work (Dillner and Takahama, 2015). Transmittance FT-IR analysis is rapid, inexpensive and nondestructive to the PTFE filter samples which are routinely collected for mass and elemental analysis in monitoring networks. FT-IR absorbance spectra are obtained from 794 filter samples from seven Interagency Monitoring of PROtected Visual Environment (IMPROVE) sites collected during 2011. Partial least squares regression is used to calibrate sample FT-IR absorbance spectra to collocated TOR EC measurements. The FT-IR spectra are divided into calibration and test sets. Two calibrations are developed: one developed from uniform distribution of samples across the EC mass range (Uniform EC) and one developed from a uniform distribution of Low EC mass samples (EC < 2.4 μg, Low Uniform EC). A hybrid approach which applies the Low EC calibration to Low EC samples and the Uniform EC calibration to all other samples is used to produce predictions for Low EC samples that have mean error on par with parallel TOR EC samples in the same mass range and an estimate of the minimum detection limit (MDL) that is on par with TOR EC MDL. For all samples, this hybrid approach leads to precise and accurate TOR EC predictions by FT-IR as indicated by high coefficient of determination (R2; 0.96), no bias (0.00 μg m-3, a concentration value based on the nominal IMPROVE sample volume of 32.8 m3), low error (0.03 μg m-3) and reasonable normalized error (21 %). These performance metrics can be achieved with various degrees of spectral pretreatment (e.g., including or excluding substrate contributions to the absorbances) and are comparable in precision and accuracy to collocated TOR measurements. Only the normalized error is higher for the FT-IR EC measurements than for collocated TOR. FT-IR spectra are also divided into calibration and test sets by the ratios OC/EC and ammonium/EC to determine the impact of OC and ammonium on EC prediction. We conclude that FT-IR analysis with partial least squares regression is a robust method for accurately predicting TOR EC in IMPROVE network samples, providing complementary information to TOR OC predictions (Dillner and Takahama, 2015) and the organic functional group composition and organic matter estimated previously from the same set of sample spectra (Ruthenburg et al., 2014).

Predicting ambient aerosol Thermal Optical Reflectance (TOR) measurements from infrared spectra: elemental carbon

NASA Astrophysics Data System (ADS)

Dillner, A. M.; Takahama, S.

2015-06-01

Elemental carbon (EC) is an important constituent of atmospheric particulate matter because it absorbs solar radiation influencing climate and visibility and it adversely affects human health. The EC measured by thermal methods such as Thermal-Optical Reflectance (TOR) is operationally defined as the carbon that volatilizes from quartz filter samples at elevated temperatures in the presence of oxygen. Here, methods are presented to accurately predict TOR EC using Fourier Transform Infrared (FT-IR) absorbance spectra from atmospheric particulate matter collected on polytetrafluoroethylene (PTFE or Teflon) filters. This method is similar to the procedure tested and developed for OC in prior work (Dillner and Takahama, 2015). Transmittance FT-IR analysis is rapid, inexpensive, and non-destructive to the PTFE filter samples which are routinely collected for mass and elemental analysis in monitoring networks. FT-IR absorbance spectra are obtained from 794 filter samples from seven Interagency Monitoring of PROtected Visual Environment (IMPROVE) sites collected during 2011. Partial least squares regression is used to calibrate sample FT-IR absorbance spectra to collocated TOR EC measurements. The FTIR spectra are divided into calibration and test sets. Two calibrations are developed, one which is developed from uniform distribution of samples across the EC mass range (Uniform EC) and one developed from a~uniform distribution of low EC mass samples (EC < 2.4 μg, Low Uniform EC). A hybrid approach which applies the low EC calibration to low EC samples and the Uniform EC calibration to all other samples is used to produces predictions for low EC samples that have mean error on par with parallel TOR EC samples in the same mass range and an estimate of the minimum detection limit (MDL) that is on par with TOR EC MDL. For all samples, this hybrid approach leads to precise and accurate TOR EC predictions by FT-IR as indicated by high coefficient of variation (R2; 0.96), no bias (0.00 μg m-3, concentration value based on the nominal IMPROVE sample volume of 32.8 m-3), low error (0.03 μg m-3) and reasonable normalized error (21 %). These performance metrics can be achieved with various degrees of spectral pretreatment (e.g., including or excluding substrate contributions to the absorbances) and are comparable in precision and accuracy to collocated TOR measurements. Only the normalized error is higher for the FT-IR EC measurements than for collocated TOR. FT-IR spectra are also divided into calibration and test sets by the ratios OC/EC and ammonium/EC to determine the impact of OC and ammonium on EC prediction. We conclude that FT-IR analysis with partial least squares regression is a robust method for accurately predicting TOR EC in IMPROVE network samples; providing complementary information to TOR OC predictions (Dillner and Takahama, 2015) and the organic functional group composition and organic matter (OM) estimated previously from the same set of sample spectra (Ruthenburg et al., 2014).

Reversible Data Hiding in FTIR Microspectroscopy Images with Tamper Indication and Payload Error Correction

PubMed Central

Seppänen, Tapio

2017-01-01

Fourier transform infrared (FTIR) microspectroscopy images contain information from the whole infrared spectrum used for microspectroscopic analyses. In combination with the FTIR image, visible light images are used to depict the area from which the FTIR spectral image was sampled. These two images are traditionally acquired as separate files. This paper proposes a histogram shifting-based data hiding technique to embed visible light images in FTIR spectral images producing single entities. The primary objective is to improve data management efficiency. Secondary objectives are confidentiality, availability, and reliability. Since the integrity of biomedical data is vital, the proposed method applies reversible data hiding. After extraction of the embedded data, the FTIR image is reversed to its original state. Furthermore, the proposed method applies authentication tags generated with keyed Hash-Based Message Authentication Codes (HMAC) to detect tampered or corrupted areas of FTIR images. The experimental results show that the FTIR spectral images carrying the payload maintain good perceptual fidelity and the payload can be reliably recovered even after bit flipping or cropping attacks. It has been also shown that extraction successfully removes all modifications caused by the payload. Finally, authentication tags successfully indicated tampered FTIR image areas. PMID:29259987

Evaluation of Fungal Deterioration in Liquidambar orientalis Mill. heartwood by FT-IR and light microscopy.

Treesearch

Nural Yilgor; Dilek Dogu; Roderquita Moore; Evren Terzi; S. Nami Kartal

2013-01-01

The chemical and morphological changes in heartwood specimens of Liquidambar orientalis Mill. caused by the white-rot fungus Trametes versicolor and the brown-rot fungi Tyromyces palustris and Gloeophyllum trabeum were studied by wet chemistry, FT-IR, GC-MS analyses, and photo-...

Thin lead sheets in the decorative features in Pavia Charterhouse.

PubMed

Colombo, Chiara; Realini, Marco; Sansonetti, Antonio; Rampazzi, Laura; Casadio, Francesca

2006-01-01

The facade of the church of the Pavia Charterhouse, built at the end of the 15th century, shows outstanding decorative features made of different stone materials, such as marbles, breccias and sandstones. Magnificent ornamental elements are made of thin lead sheets, and some marble slabs are inlaid with them. Metal elements are shaped in complex geometric and phytomorphic design, to form a Greek fret in black contrasting with the white Carrara marble. Lead pins were fixed to the back of the thin lead sheets with the aim of attaching the metal elements to the marble; in so doing the pins and the lead sheets constitute a single piece of metal. In some areas, lead elements have been lost, and they have been substituted with a black plaster, matching the colour of the metal. To the authors' knowledge, this kind of decorative technique is rare, and confirms the refinement of Renaissance Lombard architecture. This work reports on the results of an extensive survey of the white, orange and yellowish layers, which are present on the external surface of the lead. The thin lead sheets have been characterized and their state of conservation has been studied with the aid of Optical Microscopy, SEM-EDS, FTIR and Raman analyses. Lead sulphate, lead carbonates and oxides have been identified as decay products.

Changes in composition and porosity occurring during the thermal degradation of wood and wood components

USGS Publications Warehouse

Rutherford, David W.; Wershaw, Robert L.; Cox, Larry G.

2005-01-01

Samples of pine and poplar wood, pine bark, and purified cellulose and lignin were charred at temperatures ranging from 250?C to 500?C for times ranging from 1 hour to 168 hours. Changes in composition were examined by Fourier Transform Infrared (FTIR) and 13C Nuclear Magnetic Resonance (NMR) spectrometry, mass loss, and elemental composition (carbon, hydrogen, and oxygen) of the char. Structural changes were examined by changes in porosity as measured by nitrogen gas adsorption. 13C NMR spectrometry, mass loss, and elemental composition were combined to estimate the mass of aromatic and aliphatic carbon remaining in the char. Mass loss and elemental composition were combined to estimate the chemical composition of material lost for various time intervals of heating. These analyses showed that aliphatic components in the test materials were either lost or converted to aromatic carbon early in the charring process. Nitrogen adsorption showed that no porosity develops for any of the test materials with heating at 250?C, even though substantial loss of material and changes in composition occurred. Porosity development coincided with the loss of aromatic carbon, indicating that micropores were developing within a fused-ring matrix.

The Synthesis of Silicon Carbide in Rhombohedral Form with Different Chemicals

NASA Astrophysics Data System (ADS)

KARİPER, İ. AFŞIN

2017-06-01

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

The synthesis and characterization of azocalix[4]arene based chemosensors and investigation of their properties

NASA Astrophysics Data System (ADS)

Elçin, Serkan; Çılgı, Gülbanu Koyundereli; Bayrakdar, Alpaslan; Deligöz, Hasalettin

2015-05-01

In the present study, azocalix[4]arenes were prepared by linking 4-methoxy, 4-methyl, 4-ethyl, 4-chloro, 4-bromo and 4-nitroaniline to calix[4]arene through a diazo-coupling reaction. A new family of azocalix[4]arene tetraester derivatives, (4a-f), have been prepared with the incorporation of ethyl ester units to azocalix[4]arene. Characterization of the synthesized azocalix[4]arenes was carried using elemental analyses, UV-vis, FT-IR and 1H NMR spectroscopic techniques. The effect of varying pH levels and solvent types on the absorption ability of azocalix[n]arenes substituted with electron-donating and electron-withdrawing groups was examined. Thermal decomposition of azocalix[4]arene derivatives (4a-f) was investigated by means of thermogravimetry (TG), differential thermogravimetry (DTG) and differential thermal analysis (DTA) analyses. In conclusion of the examination of the extraction we found a selectivity characteristic of these compounds toward Ag+, Hg+ and Hg2+ cations.

Spectral, optical and cytotoxicity studies on 2-isonicotinoyl-N-phenylhydrazine-1-carboxamide(H3L) and some of its metal complexes

NASA Astrophysics Data System (ADS)

Hosny, Nasser M.; Hassan, Nader Y.; Mahmoud, Heba M.; Abdel-Rhman, Mohamed H.

2018-03-01

The ligand 2-isonicotinoyl-N-phenylhydrazine-1-carboxamide (H3L) and its metal complexes with Co(II), Ni(II), Cu(II) and Zn(II) acetates have been synthesized. The isolated compounds have been characterized by elemental analyses, FT-IR, 1H NMR, 13C NMR, ESR, mass, electronic spectra, electrical conductivity, effective magnetic moments and thermal analyses. The free organic ligand exists in the keto form, but in the metal complexes, it coordinates in the enol form. Four coordinated species were suggested for all the isolated metal complexes. The measured optical band gap values confirmed the presence of direct electronic transition and the semi-conductivity of the compounds. The ligand and its Zn(II) complex were examined as cytotoxic agent against HCT-116 and HePG-2. The ligand showed very strong cytotoxic effect against HePG-2, but moderate cytotoxicity against HCT-116. Zn(II) complex showed weak cytotoxicity against the two cell lines.

Synthesis, characterization and spectroscopic behavior of novel 2-oxo-1,4-disubstituted-1,2,5,6-tetrahydrobenzo[h]quinoline-3-carbonitrile dyes.

PubMed

Khan, Salman A; Asiri, Abdullah M; Al-Thaqafy, Saad H; Faidallah, Hassan M; El-Daly, Samy A

2014-12-10

Two synthetic pathways were adopted to synthesize the target 2-oxo-1,4-disubstituted-1,2,5,6-tetrahydro-benzo[h]quinoline-3-carbonitriles. Structure of the synthesized compounds has been characterized based on FT-IR, (1)H NMR, (13)C NMR and elemental analyses. UV-Vis and fluorescence spectroscopy measurements provided that all compounds are good absorbent and fluorescent. Fluorescence polarity study demonstrated that these compounds were sensitive to the polarity of the microenvironment provided by different solvents. In addition, spectroscopic and physicochemical parameters, including singlet absorption, extinction coefficient, Stokes shift, oscillator strength and dipole moment were investigated in order to explore the analytical potential of synthesized compounds. Copyright © 2014 Elsevier B.V. All rights reserved.

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

PubMed

Ajibade, Peter A; Ejelonu, Benjamin C

2013-09-01

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

Development of an automated method for determining oil in water by direct aqueous supercritical fluid extraction coupled on-line with infrared spectroscopy.

PubMed

Minty, B; Ramsey, E D; Davies, I

2000-12-01

A direct aqueous supercritical fluid extraction (SFE) system was developed which can be directly interfaced to an infrared spectrometer for the determination of oil in water. The technique is designed to provide an environmentally clean, automated alternative to established IR methods for oil in water analysis which require the use of restricted organic solvents. The SFE-FTIR method involves minimum sample handling stages, with on-line analysis of a 500 ml water sample being complete within 15 min. Method accuracy for determining water samples spiked with gasoline, white spirit, kerosene, diesel or engine oil was 81-100% with precision (RSD) ranging from 3 to 17%. An independent evaluation determined a 2 ppm limit of quantification for diesel in industrial effluents. The results of a comparative study involving an established IR method and the SFE-FTIR method indicate that oil levels calculated using an accepted equation which includes coefficients derived from reference hydrocarbon standards may result in significant errors. A new approach permitted the derivation of quantification coefficients for the SFE-FTIR analyses which provided improved results. In situations where the identity of the oil to be analysed is known, a rapid off-line SFE-FTIR system calibration procedure was developed and successfully applied to various oils. An optional in-line silica gel clean-up procedure incorporated within the SFE-FTIR system enables the same water sample to be analysed for total oil content including vegetable oils and selectively for petroleum oil content within a total of 20 min. At the end of an analysis the SFE system is cleaned using an in situ 3 min clean cycle.

Synthesis and Characterization of Mesoporous Silica Functionalized with Calix[4]arene Derivatives

PubMed Central

Alahmadi, Sana M.; Mohamad, Sharifah; Maah, Mohd Jamil

2012-01-01

This work reports a new method to covalently attach calix[4]arene derivatives onto MCM-41, using a diisocyanate as a linker. The modified mesoporous silicates were characterized by fourier transform infrared spectroscopy (FTIR), thermal analysis (TGA) and elemental analysis. The FTIR spectra and TGA analysis verified that the calix[4]arene derivates are covalently attached to the mesoporous silica. The preservation of the MCM-41 channel system was checked by X-ray diffraction and nitrogen adsorption analysis. PMID:23202977

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.

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

PubMed

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

2018-05-22

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

Synthesis and spectroscopic properties of novel asymmetric Schiff bases.

PubMed

Güngör, Ozlem; Gürkan, Perihan

2010-09-15

Three novel diimine Schiff bases including two asymmetric imines (2-OH)R-CHN-C(6)H(4)-CHN-R'(2-OH) type [where R=R'=phenyl for H(2)L(1); R=naphthyl, R'=phenyl for H(2)L(2) and R=R'=naphthyl for H(2)L(3)] have been synthesized with a new two step method. For this purpose, the starting Schiff bases 4-nitrobenzylidene-2-hydroxyaniline (SB(1)-NO(2)) and 4-nitrobenzylidene-2-hydroxy-3-naphthylamine (SB(2)-NO(2)) have been synthesized, previously. Nitro groups of them have been reduced into their amino derivatives (SB(1)-NH(2) and SB(2)-NH(2)) with sodium dithionite as selective reductant and the other imino groups have been formed by adding salicylaldehyde or 2-hydroxy-1-naphthaldehyde to the same solutions. The structures of the diimine Schiff bases were confirmed by elemental analyses, ESI-MS, FT-IR, (1)H NMR and (13)C NMR spectroscopy. The phenol-imine and keto-amine tautomerism of the Schiff bases were investigated by FT-IR, (1)H NMR, (13)C NMR techniques and UV-vis spectra in different solvents (DMSO, methanol, chloroform, toluene and cyclohexane). The effects of acidic and basic media on the tautomeric equilibria were discussed. Copyright 2010 Elsevier B.V. All rights reserved.

Energy profile, spectroscopic (FT-IR, FT-Raman and FT-NMR) and DFT studies of 4-bromoisophthalic acid

NASA Astrophysics Data System (ADS)

Arjunan, V.; Thirunarayanan, S.; Mohan, S.

2018-04-01

The stable conformer of 4-bromoisophthalic acid (BIPA) has been identified by potential energy profile analysis. All the structural parameters of 4-bromoisophthalic acid are determined by B3LYP method with 6-311++G**, 6-31G** and cc-pVTZ basis sets. The fundamental vibrations are analysed with the use of FT-IR (4000-400 cm-1) and FT-Raman (4000-100 cm-1) spectra. The harmonic vibrational frequencies are theoretically calculated and compared with experimental FTIR and FT-Raman frequencies. The 1H and 13C NMR spectra have been analysed and compared with theoretical 1H and 13C NMR chemical shifts calculated by gauge independent atomic orbital (GIAO) method. The electronic properties, such as HOMO (highest occupied molecular orbital) and LUMO (lowest unoccupied molecular orbital) energies are determined by B3LYP/cc-pVTZ method. The electron density distribution and site of chemical reactivity of BIPA molecule have been obtained by mapping electron density isosurface with molecular electrostatic potential (MEP). Stability of the molecules arising from hyperconjugative interactions, charge delocalizations have been analysed by using natural bond orbital (NBO) analysis. The thermodynamic properties and atomic natural charges of the compound are analysed and the reactive sites of the molecule are identified. The global and local reactivity descriptors are evaluated to analyse the chemical reactivity and site selectivity of molecule through Fukui functions.

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

NASA Astrophysics Data System (ADS)

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

2015-01-01

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

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 Parr® reactor. Residues were characterized by wet chemical analyses, Fourier transform infrared (FT-IR) spectroscopy, and X-ray diffraction (XRD). The FT-IR...

Quantification of material state using reflectance FTIR spectroscopy

NASA Astrophysics Data System (ADS)

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

2018-04-01

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

Hydrothermal carbonization (HTC) of wheat straw: influence of feedwater pH prepared by acetic acid and potassium hydroxide.

PubMed

Reza, M Toufiq; Rottler, Erwin; Herklotz, Laureen; Wirth, Benjamin

2015-04-01

In this study, influence of feedwater pH (2-12) was studied for hydrothermal carbonization (HTC) of wheat straw at 200 and 260°C. Acetic acid and KOH were used as acidic and basic medium, respectively. Hydrochars were characterized by elemental and fiber analyses, SEM, surface area, pore volume and size, and ATR-FTIR, while HTC process liquids were analyzed by HPLC and GC. Both hydrochar and HTC process liquid qualities vary with feedwater pH. At acidic pH, cellulose and elemental carbon increase in hydrochar, while hemicellulose and pseudo-lignin decrease. Hydrochars produced at pH 2 feedwater has 2.7 times larger surface area than that produced at pH 12. It also has the largest pore volume (1.1 × 10(-1) ml g(-1)) and pore size (20.2 nm). Organic acids were increasing, while sugars were decreasing in case of basic feedwater, however, phenolic compounds were present only at 260°C and their concentrations were increasing in basic feedwater. Copyright © 2015 Elsevier Ltd. All rights reserved.

[Spectroscopic methods applied to component determination and species identification for coffee].

PubMed

Chen, Hua-zhou; Xu, Li-li; Qin, Qiang

2014-06-01

Spectroscopic analysis was applied to the determination of the nutrient quality of ground, instant and chicory coffees. By using inductively coupled plasma atomic emission spectrometry (ICP-ES), nine mineral elements were determined in solid coffee samples. Caffeine was determined by ultraviolet (UV) spectrometry and organic matter was investigated by Fourier transform infrared (FTIR) spectroscopy. Oxidation-reduction titration was utilized for measuring the oxalate. The differences between ground coffee and instant coffee was identified on the basis of the contents of caffeine, oxalate and mineral elements. Experimental evidence showed that, caffeine in instant coffee was 2-3 times higher than in ground coffee. Oxalate in instant coffee was significantly higher in ground coffee. Mineral elements of Mg, P and Zn in ground coffee is lower than in instant coffee, while Cu is several times higher. The mineral content in chicory coffee is overall lower than the instant coffee. In addition, we determined the content of Ti for different types of coffees, and simultaneously detected the elements of Cu, Ti and Zn in chicory coffee. As a fast detection technique, FTIR spectroscopy has the potential of detecting the differences between ground coffee and instant coffee, and is able to verify the presence of caffeine and oxalate.

Characterization of ancient glass excavated in Enez (Ancient Ainos) Turkey by combined Instrumental Neutron Activation Analysis and Fourier Transform Infrared spectrometry techniques

NASA Astrophysics Data System (ADS)

Akyuz, Sevim; Akyuz, Tanil; Mukhamedshina, Nuranya M.; Mirsagatova, A. Adiba; Basaran, Sait; Cakan, Banu

2012-05-01

Ancient glass fragments excavated in the archaeological district Enez (Ancient Ainos)-Turkey were investigated by combined Instrumental Neutron Activation Analysis (INAA) and Fourier Transform Infrared (FTIR) spectrometry techniques. Multi-elemental contents of 15 glass fragments that belong to Hellenistic, Roman, Byzantine, and Ottoman Periods, were determined by INAA. The concentrations of twenty six elements (Na, K, Ca, Sc, Cr, Mn, Fe, Co, Cu, Zn, As, Rb, Sr, Sb, Cs, Ba, Ce, Sm, Eu, Tb, Yb, Lu, Hf, Ta, Au and Th), which might be present in the samples as flux, stabilizers, colorants or opacifiers, and impurities, were examined. Chemometric treatment of the INAA data was performed and principle component analysis revealed presence of 3 distinct groups. The thermal history of the glass samples was determined by FTIR spectrometry.

Synthesis and characterization of starch-poly(methyl acrylate) graft copolymers using horseradish peroxidase.

PubMed

Wang, Su; Wang, Qiang; Fan, Xuerong; Xu, Jin; Zhang, Ying; Yuan, Jiugang; Jin, Heling; Cavaco-Paulo, Artur

2016-01-20

Horseradish peroxidase (HRP)-mediated graft polymerization in the presence of hydrogen peroxide (H2O2) and acetylacetone (Acac) has been successfully applied to the synthesis of starch-poly(methyl acrylate) (PMA). The graft copolymer was characterized by Fourier transform infrared (FT-IR), elemental analysis, nuclear magnetic resonance ((1)H NMR and (13)C NMR), and differential scanning calorimetry (DSC). FT-IR, elemental analysis and NMR confirmed that methyl acrylate (MA) was grafted onto starch successfully. DSC results showed the graft reaction had changed the crystalline regions of the gelatinized starch. The effects of pH, MA content, HRP dosage, incubation temperature and time on grafting percentage (GP) and grafting efficiency (GE) were also investigated. The GP and GE under optimal conditions reached 30.21% and 45.13%, respectively. Copyright © 2015 Elsevier Ltd. All rights reserved.

Fourier transform infrared (FTIR) spectroscopy to monitor the cellular impact of newly synthesized platinum derivatives.

PubMed

Berger, Gilles; Gasper, Régis; Lamoral-Theys, Delphine; Wellner, Anja; Gelbcke, Michel; Gust, Ronald; Nève, Jean; Kiss, Robert; Goormaghtigh, Erik; Dufrasne, François

2010-09-01

Platinum complexes remain widely used to combat various types of cancers. Three platinum complexes, cisplatin, carboplatin and oxaliplatin, are marketed for various oncological purposes. Additionally, nedaplatin, lobaplatin and heptaplatin have gained regionally limited approval for oncology purposes. Furthermore, various platinum derivatives are currently under clinical trials. More than 40 years after their discovery, however, the precise mechanism of action of platinum antitumor complexes remains elusive, partly because these compounds display numerous intracellular targets. Structure-activity-relationship analyses are therefore difficult to conduct to optimize the synthesis of novel platinum derivatives. The aim of the present study is to illustrate the potential of using Fourier Transform Infrared (FTIR) analyses to monitor the cellular modifications induced by the new platinum derivatives that we have synthesized. We show in the present study the advantages of combining an in vitro assay to determine the IC50 growth inhibition concentrations of a series of compounds belonging to a given chemical series and FTIR analyses carried out at the IC50 concentrations for each compound to identify potential hits within this series of compounds. The original pharmacological approach proposed here could, therefore, avoid large-scale pharmacological experiments to find hits within a given chemical series.

A porous Cd(II) metal-organic framework with high adsorption selectivity for CO2 over CH4

NASA Astrophysics Data System (ADS)

Zhu, Chunlan

2017-05-01

Metal-organic frameworks (MOFs) have attracted a lot of attention in recent decades. We applied a semi-rigid four-carboxylic acid linker to assemble with Cd(II) ions to generate a novel microporous Cd(II) MOF material. Single crystal X-ray diffraction study reveals the different two dimension (2D) layers can be further packed together with an AB fashion by hydrogen bonds (O4sbnd H4⋯O7 = 1.863 Å) to construct a three dimension (3D) supermolecular architecture. The resulting sample can be synthesized under solvothermal reactions successfully, which exhibits high selectivity adsorption of CO2 over CH4 at room temperature. In addition, the obtained sample was characterized by thermal gravimetric analyses (TGA), Fourier-transform infrared spectra (FT-IR), elemental analysis (CHN) and powder X-ray diffraction (PXRD).

Sonochemical synthesis of magnetic responsive Fe3O4@TMU-17-NH2 composite as sorbent for highly efficient ultrasonic-assisted denitrogenation of fossil fuel.

PubMed

Mirzaie, Abbas; Musabeygi, Tahereh; Afzalinia, Ahmad

2017-09-01

In this work, a novel magnetic responsive composite was fabricated by encapsulation of Fe 3 O 4 nanoparticles into an amino-functionalized MOF (TMU-17-NH 2 ) under ultrasound irradiation. The prepared materials were characterized by several techniques such as elemental analyses, PXRD, FT-IR, N 2 adsorption, TGA and ICP. This composite has been applied to the adsorptive removal of nitrogen-contain compounds in model liquid fuel. The prepared composite demonstrates very good performance for the removal of NCCs. The maximum adsorption capacity of IND and QUI over prepared composite calculated 375.93 and 310.18mg·g -1 at 25°C, respectively. The composite material is magnetically separable and reusable for several times. Copyright © 2016 Elsevier B.V. All rights reserved.

Design, synthesis and characterization of macrocyclic ligand based transition metal complexes of Ni(II), Cu(II) and Co(II) with their antimicrobial and antioxidant evaluation

NASA Astrophysics Data System (ADS)

Gull, Parveez; Malik, Manzoor Ahmad; Dar, Ovas Ahmad; Hashmi, Athar Adil

2017-04-01

Three new complexes Ni(II), Cu(II) and Co(II) were synthesized of macrocyclic ligand derived from 1, 4-dicarbonyl-phenyl-dihydrazide and O-phthalaldehyde in the ratio of 2:2. The synthesized compounds were characterized by elemental analyses, molar conductance, magnetic susceptibility measurements, FTIR, UV-Vis., Mass and 1H NMR spectral studies. The electronic spectra of the metal complexes indicate a six coordinate octahedral geometry of the central metal ion. These metal complexes and the ligand were evaluated for antimicrobial activity against bacteria (E. coli, B. subtilis, S. aureus) and fungi (A. niger, A. flavus, C. albicans) and compared against standard drugs chloramphenicol and nystatin respectively. In addition, the antioxidant activity of the compounds was also investigated through scavenging effect on DPPH radicals.

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

USGS Publications Warehouse

Mastalerz, Maria; Hower, J.C.

1996-01-01

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

Elemental identification of blue paintings traces present in historic cemeteries in the São Martinho region, southern Brazil

NASA Astrophysics Data System (ADS)

Costa, Thiago G.; Richter, Fábio Andreas; Castro, Elisiana Trilha; Gonçalves, Samantha; Spudeit, Daniel A.; Micke, Gustavo A.

2018-03-01

Cemeteries are of great significance in many communities, often being considered of invaluable historical, artistic, architectural and cultural significance and thus they need to be preserved. In this regard, understanding the historical aspects and the construction techniques used is essential for their protection. The purpose of this paper is to describe historical aspects of the funerary heritage present in the region of São Martinho in southern Brazil, along with an analysis of the blue paint found in cemeteries of German colonies in the region studied. FTIR analysis suggests that the binder is composed mostly of a protein resin and a small amount of lipid. The morphology of the pigment was investigated by SEM and EDS and the spectra revealed that the major elements present in the blue pigment are Na, Al, Si and S, with an overlap in the elemental mapping, indicative of ultramarine pigments. The GC-MS results are consistent with the type of binder identified by FTIR and indicate a mixture of oils, probably from vegetal sources, and proteins.

Synthesis, characterization and biological investigations of novel Schiff base ligands containing imidazoline moiety and their Co(II) and Cu(II) complexes

NASA Astrophysics Data System (ADS)

Radha, V. P.; Jone Kirubavathy, S.; Chitra, S.

2018-08-01

Novel imidazoline based Schiff base ligands L1 and L2 were synthesized from o-phenylenediamine/o-aminophenol with creatinine. The ligands were complexed with Co(II) and Cu(II) by direct reaction with metal salts. The synthesized ligands and the metal complexes were characterized by elemental analysis, FT-IR, 1H NMR, mass, electronic, thermal analyses, conductivity and magnetic susceptibility measurements. The conductivity measurements showed the non-electrolytic nature of the complexes. The thermogravimetric analyses confirmed the presence of lattice and coordinated water molecules in the complexes. The DFT calculations were carried out at B3LYP/6-31G(d,p) level for the determination of the optimized structure of the ligands. The synthesized ligands and the metal complexes were screened for their antimicrobial activity against two gram positive bacteria (Staphylococcus aureus and Bacillus subtilis) and two gram negative bacteria (Escherichia coli and Pseudomonas aeruginosa) and two fungal strains (Aspergillus niger and Candida albicans). The outcomes revealed that the metal complexes showed pronounced activity than the ligands.

Synthesis, structural, optical and anti-rheumatic activity of metal complexes derived from (E)-2-amino-N-(1-(2-aminophenyl)ethylidene)benzohydrazide (2-AAB) with Ru(III), Pd(II) and Zr(IV)

NASA Astrophysics Data System (ADS)

Hosny, Nasser Mohammed; Sherif, Yousery E.

2015-02-01

Three new metal complexes derived from Pd(II), Ru(III) and Zr(IV) with (E)-2-amino-N-(1-(2-aminophenyl)ethylidene)benzohydrazide (2-AAB) have been synthesized. The isolated complexes were characterized by elemental analyses, FT-IR, UV-Vis, ES-MS, 1H NMR, XRD, thermal analyses (TGA and DTA) and conductance. The morphology and the particle size were determined by transmittance electron microscope (TEM). The results showed that, the ligand coordinates to Pd(II) in the enol form, while it coordinates to Ru(III) and Zr(IV) in the keto form. A square planar geometry is suggested for Pd(II) complex and octahedral geometries are suggested for Ru(III) and Zr(IV) complexes. The optical band gaps of the isolated complexes were measured and indicated the semi-conductivity nature of the complexes. The anti-inflammatory and analgesic activities of the ligand and its complexes showed that, Ru(III) complex has higher effect than the well known drug "meloxicam".

[Spectral characteristics of decomposition of incorporated straw in compound polluted arid loess].

PubMed

Fan, Chun-Hui; Zhang, Ying-Chao; Xu, Ji-Ting; Wang, Jia-Hong

2014-04-01

The original loess from western China was used as soil sample, the spectral methods of scanning electron microscope-energy dispersive X-ray spectroscopy (SEM-EDS), elemental analysis, Fourier transform infrared spectroscopy (FT-IR) and 13C nuclear magnetic resonance (13C NMR) were used to investigate the characteristics of decomposed straw and formed humic acids in compound polluted arid loess. The SEM micrographs show the variation from dense to decomposed surface, and finally to damaged structure, and the EDS data reveal the phenomenon of element transfer. The newly-formed humic acids are of low aromaticity, helpful for increasing the activity of organic matters in loess. The FTIR spectra in the whole process are similar, indicating the complexity of transformation dynamics of humic acids. The molecular structure of humic acids becomes simpler, shown from 13C NMR spectra. The spectral methods are useful for humic acids identification in loess region in straw incorporation process.

Study of consumer fireworks post-blast residues by ATR-FTIR.

PubMed

Martín-Alberca, Carlos; Zapata, Félix; Carrascosa, Héctor; Ortega-Ojeda, Fernando E; García-Ruiz, Carmen

2016-03-01

Specific analytical procedures are requested for the forensic analysis of pre- and post-blast consumer firework samples, which present significant challenges. Up to date, vibrational spectroscopic techniques such as Fourier transform infrared spectroscopy (FTIR) have not been tested for the analysis of post-blast residues in spite of their interesting strengths for the forensic field. Therefore, this work proposes a simple and fast procedure for the sampling and analysis of consumer firework post-blast residues by a portable FTIR instrument with an Attenuated Total Reflection (ATR) accessory. In addition, the post-blast residues spectra of several consumer fireworks were studied in order to achieve the identification of their original chemical compositions. Hence, this work analysed 22 standard reagents usually employed to make consumer fireworks, or because they are related to their combustion products. Then, 5 different consumer fireworks were exploded, and their residues were sampled with dry cotton swabs and directly analysed by ATR-FTIR. In addition, their pre-blast fuses and charges were also analysed in order to stablish a proper comparison. As a result, the identification of the original chemical compositions of the post-blast samples was obtained. Some of the compounds found were potassium chlorate, barium nitrate, potassium nitrate, potassium perchlorate or charcoal. An additional study involving chemometric tools found that the results might greatly depend on the swab head type used for the sampling, and its sampling efficiency. The proposed procedure could be used as a complementary technique for the analysis of consumer fireworks post-blast residues. Copyright © 2015 Elsevier B.V. All rights reserved.

C-O volatiles in Apollo 15 and Apollo 17 picritic glasses

NASA Technical Reports Server (NTRS)

Rutherford, Malcolm J.; Fogel, Robert A.

1993-01-01

A15 and A17 primitive picritic glasses have been examined by FTIR for the presence of dissolved C-O species to determine the role of C-O gasses on driving lunar fire-fountains. A15 green and yellow glasses were extensively studied and found to be free of dissolved C species down to FTIR detection limits (10-100 ppm; species and sample specific). Preliminary data on A17 orange glasses are similarly devoid of FTIR detectable C-O species. Re-analyses of the C-O driving mechanism theory for mare volcanism demonstrates the need to determine the fO2 of the lunar interior; the factor that most critically determined the role of C gasses in the fire-fountaining events. Oxygen fugacities equivalent to IW-0.5 and above imply dissolved CO3(=) in the primitive glasses at levels above FTIR detection. The f02's below IW-0.5 imply concentrations of CO3(=) below FTIR detection. Recent data suggesting lunar mantle fO2's of IW-2 or less, strongly mitigate against finding FTIR measurable dissolved CO3(=) consistent with the findings of this study.

Ground-based FTIR retrievals of SF6 on Reunion Island

NASA Astrophysics Data System (ADS)

Zhou, Minqiang; Langerock, Bavo; Vigouroux, Corinne; Wang, Pucai; Hermans, Christian; Stiller, Gabriele; Walker, Kaley A.; Dutton, Geoff; Mahieu, Emmanuel; De Mazière, Martine

2018-02-01

SF6 total columns were successfully retrieved from FTIR (Fourier transform infrared) measurements (Saint Denis and Maïdo) on Reunion Island (21° S, 55° E) between 2004 and 2016 using the SFIT4 algorithm: the retrieval strategy and the error budget were presented. The FTIR SF6 retrieval has independent information in only one individual layer, covering the whole of the troposphere and the lower stratosphere. The trend in SF6 was analysed based on the FTIR-retrieved dry-air column-averaged mole fractions (XSF6) on Reunion Island, the in situ measurements at America Samoa (SMO) and the collocated satellite measurements (Michelson Interferometer for Passive Atmospheric Sounding, MIPAS, and Atmospheric Chemistry Experiment Fourier Transform Spectrometer, ACE-FTS) in the southern tropics. The SF6 annual growth rate from FTIR retrievals is 0.265 ± 0.013 pptv year-1 for 2004-2016, which is slightly weaker than that from the SMO in situ measurements (0.285 ± 0.002 pptv year-1) for the same time period. The SF6 trend in the troposphere from MIPAS and ACE-FTS observations is also close to the ones from the FTIR retrievals and the SMO in situ measurements.

The preservation and degradation of filamentous bacteria and biomolecules within iron oxide deposits at Rio Tinto, Spain.

PubMed

Preston, L J; Shuster, J; Fernández-Remolar, D; Banerjee, N R; Osinski, G R; Southam, G

2011-05-01

One of the keys to understanding and identifying life on other planets is to study the preservation of organic compounds and their precursor micro-organisms on Earth. Rio Tinto in southwestern Spain is a well documented site of microbial preservation within iron sulphates and iron oxides over a period of 2.1 Ma. This study has investigated the preservation of filamentous iron oxidising bacteria and organics through optical microscopy, scanning electron microscopy (SEM) and Fourier transform infra-red (FTIR) spectroscopy, from laboratory cultures of natural samples to contemporary natural materials to million-year old river terraces. Up to 40% elemental carbon and >7% nitrogen has been identified within microbial filaments and cell clusters in all samples through SEM EDS analyses. FTIR spectroscopy identified C-H(x) absorption bands between 2960 and 2800 cm(-1), Amide I and II absorption bands at 1656 and 1535 cm(-1), respectively and functional group vibrations from within nucleic acids at 917, 1016 and 1124 cm(-1). Absorption bands tracing the diagenetic transformation of jarosite to goethite to hematite through the samples are also identified. This combination of mineralogy, microbial morphology and biomolecular evidence allows us to further understand how organic fossils are created and preserved in iron-rich environments, and ultimately will aid in the search for the earliest life on Earth and potential organics on Mars. © 2011 Blackwell Publishing Ltd.

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.

In situ investigation of Geobacillus stearothermophilus spore germination and inactivation mechanisms under moderate high pressure.

PubMed

Georget, Erika; Kapoor, Shobhna; Winter, Roland; Reineke, Kai; Song, Youye; Callanan, Michael; Ananta, Edwin; Heinz, Volker; Mathys, Alexander

2014-08-01

Bacterial spores are a major concern for food safety due to their high resistance to conventional preservation hurdles. Innovative hurdles can trigger bacterial spore germination or inactivate them. In this work, Geobacillus stearothermophilus spore high pressure (HP) germination and inactivation mechanisms were investigated by in situ infrared spectroscopy (FT-IR) and fluorometry. G. stearothermophilus spores' inner membrane (IM) was stained with Laurdan fluorescent dye. Time-dependent FT-IR and fluorescence spectra were recorded in situ under pressure at different temperatures. The Laurdan spectrum is affected by the lipid packing and level of hydration, and provided information on the IM state through the Laurdan generalized polarization. Changes in the -CH2 and -CH3 asymmetric stretching bands, characteristic of lipids, and in the amide I' band region, characteristic of proteins' secondary structure elements, enabled evaluation of the impact of HP on endospores lipid and protein structures. These studies were complemented by ex situ analyses (plate counts and microscopy). The methods applied showed high potential to identify germination mechanisms, particularly associated to the IM. Germination up to 3 log10 was achieved at 200 MPa and 55 °C. A molecular-level understanding of these mechanisms is important for the development and validation of multi-hurdle approaches to achieve commercial sterility. Copyright © 2014 Elsevier Ltd. All rights reserved.

Micro-FTIR Spectroscopy of Experimentally Shocked Basaltic Andesite (SP Flow, AZ)

NASA Astrophysics Data System (ADS)

Johnson, J. R.; Jaret, S.; Glotch, T. D.; Sims, M.

2017-12-01

As part of an ongoing systematic study of experimental shock transformations in plagioclase using micro-Raman and micro-FTIR thermal infrared hyperspectral imaging and point spectroscopy [1-7], we report new micro-FTIR results on experimentally shocked, fine-grained basaltic andesite from SP Flow (AZ). This sample has relatively high primary glass content and an average plagioclase composition of labradorite/bytownite. The powder propellant gun at the Johnson Space Center was used to conduct the original shock experiments at peak pressures from 15 to 60 GPa [6-8], from which <10 mm fragments were recovered. Polished thin sections were made from portions of these fragments, and micro-FTIR point spectra were collected from 400-4000 cm-1 (2.5-25 µm) using a spot size of 40 x 40 mm at 8 cm-1 spectral sampling. Micro-FTIR hyperspectral maps of thin sections were acquired using the same instrument equipped with a 16 pixel HgCdTe linear array detector to provide spectra between 7000 and 715 cm-1 (1.4-14.0 µm) at 25 µm/pixel and 8 cm-1 spectral sampling (see figure for color composite and band depth images from unshocked sample). Micro-FTIR results show that the unshocked sample is dominated by the glassy matrix (light green in the color composite), with contributions from plagioclase and pyroxene. Initial analyses suggest that the SP Flow samples become dominantly amorphous at relatively low shock pressures, reflective of the high primary glass content and consistent with macro-scale spectra from [7]. Results from additional shock pressures and Raman spectra will be presented at the conference. Future work will include (1) Raman and FTIR analyses of basalt from Grand Falls (AZ), which has minimal primary glass content and relatively higher calcic plagioclase than SP Flow; and (2) comparison of these basalts to results from shocked plagioclase and to similar analyses of naturally shocked samples from Ries and Lonar Craters. [1] Jaret, S. et al., 11th Internat. GeoRaman Conf., #5095, 2014; [2] Jaret, S., et al., LPSC # 2056, 2015; [3] Jaret, S., et al., LPSC #1530, 2016; [4] Jaret, S., et al., LPSC, abs. #2484, 2017; [5] Jaret, S., et al. GSA, abstract #267947, 2015; [6] Johnson, J., et al., Amer. Mineral., 88, 1575-1582, 2003; [7] Johnson, J., Icarus 221 359-364, 2012; [8] Johnson, J., et al., Amer. Mineral., 92, 1148-1157, 2007.

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.

Sulfato/thiosulfato reducing bacteria characterization by FT-IR spectroscopy: a new approach to biocorrosion control.

PubMed

Rubio, Celine; Ott, Christelle; Amiel, Caroline; Dupont-Moral, Isabelle; Travert, Josette; Mariey, Laurence

2006-03-01

Sulfato and Thiosulfato Reducing Bacteria (SRB, TRB) can induce corrosion process on steel immersed in seawater. This phenomenon, called biocorrosion, costs approximatively 5 billion euros in France each year. We provide the first evidence that Fourier Transformed InfraRed (FTIR) spectroscopy is a competitive technique to evaluate the sulfurogen flora involved in biocorrosion in comparison with time consuming classical identification methods or PCR analyses. A great discrimination was obtained between SRB, TRB and some contamination bacteria known to be present in seawater and seem to be able to reduce sulfate under particular conditions. Moreover, this preliminary study demonstrates that FTIR spectroscopic and genotypic results present a good correlation (these results are confirmed by other data obtained before or later, data not shown here). The advantages gained by FTIR spectroscopy are to give information on strain phenotype and bacterial metabolism which are of great importance in corrosion processes.

Simultaneous and continuous measurements of dissolved CO2, CH4, N2O and CO in rivers using Fourier-Transform-InfraRed (FTIR) spectrometry

NASA Astrophysics Data System (ADS)

Warneke, Thorsten; Müller, Denise; Caldow, Christopher; Rixen, Tim; Notholt, Justus

2015-04-01

We have coupled a Fourier-Transform InfraRed (FTIR) trace gas analyser to an equilibrator, which allows the simultaneous and continuous measurement of dissolved CO2, CH4, N2O and CO in water. The FTIR-technique has a high precision over a wide range of concentrations, making it very suitable for the measurement of these gases in freshwater systems. We have employed this measurement system on a commercial river barge on the Elbe river (Czech Republic, Germany) and on a fisher boat in the coastal area of Sarawak (Malaysia). In addition we have performed stationary continuous measurements at a small river in Northern Germany over the duration of 3 months. The presentation will outline the advantages and disadvantages of the FTIR-technique for freshwater measurements and will present results from the measurement campaigns.

Scanning electron microscopic and X-ray micro analysis on tooth enamel exposed to alkaline agents.

PubMed

Taubee, Fabian; Steiniger, Frank; Nietzsche, Sandor; Norén, Jörgen G

2010-01-01

The background of this study comprises two clinical cases, where patients exposed to aerosols of an alkaline and surface active cleaning agent developed loss of enamel substance on their teeth, further resulting in loss of teeth and partially destroyed soft tissues. The alkaline cleaning agent consisted of potassium hydroxide and various surfactants. The purpose of this study was to investigate possible changes in morphology and composition in human teeth enamel exposed to alkaline solutions, by means of X-ray micro analysis (XRMA), FTIR-spectroscopic analyses and scanning electron microscopy (SEM). Extracted premolars, exposed to potassium hydroxide solutions and alkaline cleaning solution,were analyzed by means of XRMA and SEM. Enamel powder, exposed to cleaning solution, was analyzed by means of FTIR. The SEM analysis revealed an increased porosity of the enamel surface and partially loss of enamel substance after exposure to alkaline solutions. The XRMA analyses revealed a decrease in carbon concentration while phosphorous and calcium showed no marked changes. The FTIR analyses showed no significant changes in peak heights or peak positions for phosphate, carbonate or hydroxide. It was concluded that human teeth enamel exposed to alkaline solutions showed loss of organic substance, marked pores in enamel surface and loss of substance in the enamel surface.

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

NASA Astrophysics Data System (ADS)

Karpuraranjith, M.; Thambidurai, S.

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

A novel polydentate ligand chromophore for simultaneously colorimetric detection of trace Ag + and Fe3 +

NASA Astrophysics Data System (ADS)

Yan, Zhengquan; Zhao, Qi; Wen, Meijun; Hu, Lei; Zhang, Xuezhong; You, Jinmao

2017-11-01

A novel polydentate ligand chromophore, 3,6-di-(N-ethyl-N-ethoxyl phenylazo) acridine (EEPA), was identified and synthesized. After its structure was characterized by FTIR, 1H NMR, mass spectra and element analyses, it was noted to find that there was a simultaneously colorimetric response to Ag+ and Fe3 + accompanying with different color changes, i.e., from brown to light purple for Ag+ and further to purple-red for Fe3 +, respectively. Their different action mechanisms, a 1:2 complex mode for EEPA-Ag+ and 1:1 for EEPA-Fe3 +, were investigated and confirmed by means of Job's plot and theoretical calculation. EEPA would be a potential colorimetric chemo-dosimeter for simultaneous detection of Ag+ and Fe3 + with the detection limits of 1.6 nmol·L- 1 and 69 nmol·L- 1, respectively.

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

NASA Astrophysics Data System (ADS)

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

2010-05-01

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

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

NASA Astrophysics Data System (ADS)

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

2018-01-01

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

Sonochemical synthesis and characterization of a novel hetro-binuclear metal organic nano polymer based on picolinic acid ligand

NASA Astrophysics Data System (ADS)

Hayati, Payam; Souri, Bagher; Rezvani, Ali Reza; Morsali, Ali; Gutierrez, Angel

2017-12-01

Nanoparticles of one new lead and K coordination polymer (CP), {[Pb6(pyc)6(N3)7K].½H2O}n (1) Hpyc = picolinic acid ligand, has been synthesized by use of a sonochemical process and characterized by scanning electron microscopy (SEM), X-ray powder diffraction (XRPD), Fourier transform infrared spectroscopy (FTIR) spectroscopy and elemental analyses. The single crystal X-ray data of compound 1 imply that the Pb ion is seven coordinated. The thermal stability of compound 1 has been studied by thermogravimetric (TG) and differential scanning calorimetry (DSC). The role of temperature, reaction time and ultrasound irradiation power on the size and morphfology of the nano-structured compound obtained from 1, have been investigated. Results indicate that an increase of temperature and sonication power and a decrease in time reaction led to a decrease of particle size.

Physicochemical and Critical Micelle Concentration (CMC) of Cationic (CATB) and Anionic (SDS) Surfactants with Environmentally Benign Blue Emitting TTQC Dye.

PubMed

Khan, Salman A; Asiri, Abdullah M

2015-11-01

4-(3,4,5-trimethoxyphenyl)-8-methoxy-2-oxo-1,2,5,6 tetrahydrobenzo[h]quinoline-3-carbonitrile (TTQC) dye has synthesized by one-pot multicomponent reactions (MCRs) of 3,4,5-trimethoxybenzaldehyd, ethyl cyanoacetate, 6-methoxy-1,2,3,4-tetrahydro-naphthalin-1-one and ammonium acetate under microwave irradiation. The structures of the synthesized compound was established by spectroscopic (FT-IR, (1)H-NMR, (13)C-NMR, EI-MS) and elemental analyses. In addition, spectroscopic and physicochemical parameters, including electronic absorption, excitation coefficient, Stokes shift, oscillator strength, transition dipole moment and fluorescence quantum yield were investigated in order to explore the analytical potential of synthesized compound. TTQC dye undergoes solubilization in different micelles and may be used as a probe to determine the critical micelle concentration (CMC) of CTAB and SDS.

Synthesis, crystal structure, biological activity and theoretical calculations of novel isoxazole derivatives

NASA Astrophysics Data System (ADS)

Jin, R. Y.; Sun, X. H.; Liu, Y. F.; Long, W.; Chen, B.; Shen, S. Q.; Ma, H. X.

2016-01-01

Series of isoxazole derivatives were synthesized by substituted chalcones and 2-chloro-6-fluorobenzene formaldehyde oxime with 1,3-dipolar cycloaddition. The target compounds were determined by melting point, IR, 1H NMR, elemental analyses and HRMS. The crystal structure of compound 3a was detected by X-ray diffraction and it crystallizes in the triclinic space group p2(1)/c with z = 4. The molecular geometry of compound 3a was optimized using density functional theory (DFT/B3LYP) method with the 6-31G+(d,p) basis set in the ground state. From the optimized geometry of the molecule, FT-IR, FT-Raman, HOMO-LUMO and natural bond orbital (NBO) were calculated at B3LYP/6-31G+(d,p) level. Finally, the antifungal activity of the synthetic compounds were evaluated against Pythium solani, Gibberella nicotiancola, Fusarium oxysporium f.sp. niveum and Gibberella saubinetii.

Preparation and characterization of a novel adsorbent from Moringa oleifera leaf

NASA Astrophysics Data System (ADS)

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

2017-06-01

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

Enhancement of porous silicon photoluminescence property by lithium chloride treatment

NASA Astrophysics Data System (ADS)

Azaiez, Khawla; Zaghouani, Rabia Benabderrahmane; Khamlich, Saleh; Meddeb, Hosny; Dimassi, Wissem

2018-05-01

Porous silicon (PS) decorated by several nanostructured metal elements has still aroused interests as promising composites in many industrial applications. With the focus mainly on the synthesis, the aspect of stability against optical irradiation of such materials has so far not been thoroughly addressed. This work focuses primarily on the influence of lithium chloride solution (LiCl) treatment on the physical properties of PS. Variations in the structural and optoelectronic properties of PS were observed after immersion in (LiCl), as revealed by the obtained analyses. Moreover, enhanced photoluminescence (PL) property of the PS after passivation by lithium particles was clearly shown, and their presence on the surface of the microporous silicon was confirmed by FTIR spectroscopy and atomic force microscopy. An improvement of the minority carrier lifetime was also obtained, which was attributed to the decrease of the surface recombination velocity after LiCl treatment.

Single-photon and two-photon excited fluorescence behavior of a novel fluorene-based compound

NASA Astrophysics Data System (ADS)

Ma, Wenbo; Wu, Yiquan; Gu, Donghong; Gan, Fuxi

2005-09-01

A D-π-D type compound, 2,7-bis(4-methoxystyryl)-9,9-bis(2-ethylhexyl)-9H-fluorene (abbreviated as MO-Flu-MO), where electron-donor D is methoxy group andπis fluorene unit, has been synthesized. The molecular structures of the compound were characterized by elemental analyses, EI-MS and FT-IR spectra. UV-Vis spectra in the region 230--1000 nm and single-photon excited fluorescence in tetrahydrofuran (THF) of the compound were measured. It is found that the new compound exhibits strong two-photon excited fluorescence in the region 380--500 nm and moderate two-photon absorption (TPA) value in the femtoseconds regime (TPA cross-section as high as 55×10-50 cm4 s photon-1 with 13fs laser pulses). The results demonstrate that the compound is a promising candidate for two-photon three-dimensional (3D) optical data storage.

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

NASA Astrophysics Data System (ADS)

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

2015-12-01

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

Synthesis, characterization, DNA-binding study and anticancer properties of ternary metal(II) complexes of edda and an intercalating ligand.

PubMed

Ng, Chew Hee; Kong, King Chow; Von, Sze Tin; Balraj, Pauline; Jensen, Paul; Thirthagiri, Eswary; Hamada, Hirokazu; Chikira, Makoto

2008-01-28

A series of ternary metal(ii) complexes {M(phen)(edda); 1a (Cu), 1b (Co), 1c (Zn), 1d (Ni); H(2)edda = N,N(')-ethylenediaminediacetic acid} of N,N'-ethylene-bridged diglycine and 1,10-phenanthroline were synthesized and characterized by elemental analysis, FTIR, UV-visible spectroscopy and magnetic susceptibility measurement. The interaction of these complexes with DNA was investigated using CD and EPR spectroscopy. MTT assay results of 1a-1c , screened on MCF-7 cancer cell lines, show that synergy between the metal and ligands results in significant enhancement of their antiproliferative properties. Preliminary results from apoptosis and cell cycle analyses with flow cytometry are reported. seems to be able to induce cell cycle arrest at G(0)/G(1). The crystal structure of 1a is also included.

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

NASA Astrophysics Data System (ADS)

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

2016-12-01

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

FT-IR, micro-Raman and UV-vis spectroscopic and quantum chemical investigations of free 2,2'-dithiodipyridine and its metal (Co, Cu and Zn) halide complexes.

PubMed

Gökce, Halil; Bahçeli, Semiha

2013-10-01

In this study the elemental analysis results, molecular geometries, vibrational and electronic absorption spectra of free 2,2'-dithiodipyridine(C10H8N2S2), (or DTDP) (with synonym, 2,2'-dipyridyl disulfide) and M(C10H8N2S2)Cl2 (M=Co, Cu and Zn) complexes have been reported. Vibrational wavenumbers of free DTDP and its metal halide complexes have been calculated by using DFT/B3LYP calculation method with 6-31++G(d,p) and Lanl2DZ basis sets, respectively, in the ground state, for the first time. The calculated fundamental vibrational frequencies are in a good agreement with experimental data. The HOMO, LUMO and MEP analyses of all compounds are performed by DFT method. Copyright © 2013. Published by Elsevier B.V.

Stabilization of Co{sup 2+} in layered double hydroxides (LDHs) by microwave-assisted ageing

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

Herrero, M.; Benito, P.; Labajos, F.M.

2007-03-15

Co-containing layered double hydroxides at different pH have been prepared, and aged following different routes. The solids prepared have been characterized by element chemical analysis, powder X-ray diffraction, thermogravimetric and differential thermal analyses (both in nitrogen and in oxygen), FT-IR and Vis-UV spectroscopies, temperature-programmed reduction and surface area assessment by nitrogen adsorption at -196 deg. C. The best conditions found to preserve the cobalt species in the divalent oxidation state are preparing the samples at controlled pH, and then submit them to ageing under microwave irradiation. - Graphical abstract: The use of microwave-hydrothermal treatment, controlling both temperature and ageing time,more » permits to synthesize well-crystallized nanomaterials with controlled surface properties. An enhancement in the crystallinity degree and an increase in the particle size are observed when the irradiation time is prolonged.« less

Valorisation of chicken feathers: Characterisation of chemical properties.

PubMed

Tesfaye, Tamrat; Sithole, Bruce; Ramjugernath, Deresh; Chunilall, Viren

2017-10-01

The characterisation of the chemical properties of the whole chicken feather and its fractions (barb and rachis), was undertaken to identify opportunities for valorizing this waste product. The authors have described the physical, morphological, mechanical, electrical and thermal properties of the chicken feathers and related them to potential valorisation routes of the waste. However, identification of their chemical properties is necessary to complete a comprehensive description of chicken feather fractions. Hence, the chicken feathers were thoroughly characterised by proximate and ultimate analyses, elemental composition, spectroscopic analyses, durability in different solvents, burning test, and hydrophobicity. The proximate analysis of chicken feathers revealed the following compositions: crude lipid (0.83%), crude fibre (2.15%), crude protein (82.36%), ash (1.49%), NFE (1.02%) and moisture content (12.33%) whereas the ultimate analyses showed: carbon (64.47%), nitrogen (10.41%), oxygen (22.34%), and sulphur (2.64%). FTIR analysis revealed that the chicken feather fractions contain amide and carboxylic groups indicative of proteinious functional groups; XRD showed a crystallinity index of 22. Durability and burning tests confirmed that feathers behaved similarly to animal fibre. This reveals that chicken feather can be a valuable raw material in textile, plastic, cosmetics, pharmaceuticals, biomedical and bioenergy industries. Copyright © 2017 Elsevier Ltd. All rights reserved.

Analysis of Alkaloids from Physalis peruviana by Capillary GC, Capillary GC-MS, and GC-FTIR.

PubMed

Kubwabo, C; Rollmann, B; Tilquin, B

1993-04-01

The alkaloid composition of the aerial parts and roots of PHYSALIS PERUVIANA was analysed by capillary GC (GC (2)), GC (2)-MS and GC (2)-FTIR. Eight alkaloids were identified, three of those alkaloids are 3beta-acetoxytropane and two N-methylpyrrolidinylhygrine isomers, which were not previously found in the genus PHYSALIS. A reproduction of the identification of alkaloids detected in the plant by the use of retention indices has been proposed.

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

PubMed

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

2016-04-01

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

[Establishment of the Mathematical Model for PMI Estimation Using FTIR Spectroscopy and Data Mining Method].

PubMed

Wang, L; Qin, X C; Lin, H C; Deng, K F; Luo, Y W; Sun, Q R; Du, Q X; Wang, Z Y; Tuo, Y; Sun, J H

2018-02-01

To analyse the relationship between Fourier transform infrared （FTIR） spectrum of rat's spleen tissue and postmortem interval （PMI） for PMI estimation using FTIR spectroscopy combined with data mining method. Rats were sacrificed by cervical dislocation, and the cadavers were placed at 20 ℃. The FTIR spectrum data of rats' spleen tissues were taken and measured at different time points. After pretreatment, the data was analysed by data mining method. The absorption peak intensity of rat's spleen tissue spectrum changed with the PMI, while the absorption peak position was unchanged. The results of principal component analysis （PCA） showed that the cumulative contribution rate of the first three principal components was 96%. There was an obvious clustering tendency for the spectrum sample at each time point. The methods of partial least squares discriminant analysis （PLS-DA） and support vector machine classification （SVMC） effectively divided the spectrum samples with different PMI into four categories （0-24 h, 48-72 h, 96-120 h and 144-168 h）. The determination coefficient （ R ²） of the PMI estimation model established by PLS regression analysis was 0.96, and the root mean square error of calibration （RMSEC） and root mean square error of cross validation （RMSECV） were 9.90 h and 11.39 h respectively. In prediction set, the R ² was 0.97, and the root mean square error of prediction （RMSEP） was 10.49 h. The FTIR spectrum of the rat's spleen tissue can be effectively analyzed qualitatively and quantitatively by the combination of FTIR spectroscopy and data mining method, and the classification and PLS regression models can be established for PMI estimation. Copyright© by the Editorial Department of Journal of Forensic Medicine.

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).

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

NASA Astrophysics Data System (ADS)

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

2018-05-01

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

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

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

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

2015-06-24

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

Characterization of Archaeological Sediments Using Fourier Transform Infrared (FT-IR) and Portable X-ray Fluorescence (pXRF): An Application to Formative Period Pyro-Industrial Sites in Pacific Coastal Southern Chiapas, Mexico.

PubMed

Neff, Hector; Bigney, Scott J; Sakai, Sachiko; Burger, Paul R; Garfin, Timothy; George, Richard G; Culleton, Brendan J; Kennett, Douglas J

2016-01-01

Archaeological sediments from mounds within the mangrove zone of far-southern Pacific coastal Chiapas, Mexico, are characterized in order to test the hypothesis that specialized pyro-technological activities of the region's prehistoric inhabitants (salt and ceramic production) created the accumulations visible today. Fourier transform infrared spectroscopy (FT-IR) is used to characterize sediment mineralogy, while portable X-ray fluorescence (pXRF) is used to determine elemental concentrations. Elemental characterization of natural sediments by both instrumental neutron activation analysis (INAA) and pXRF also contribute to understanding of processes that created the archaeological deposits. Radiocarbon dates combined with typological analysis of ceramics indicate that pyro-industrial activity in the mangrove zone peaked during the Late Formative and Terminal Formative periods, when population and monumental activity on the coastal plain and piedmont were also at their peaks. © The Author(s) 2015.

Assessing dysplasia of a bronchial biopsy with FTIR spectroscopic imaging

NASA Astrophysics Data System (ADS)

Foreman, Liberty; Kimber, James A.; Oliver, Katherine V.; Brown, James M.; Janes, Samuel M.; Fearn, Tom; Kazarian, Sergei G.; Rich, Peter

2015-03-01

An FTIR image of an 8 µm section of de-paraffinised bronchial biopsy that shows a histological transition from normal to severe dysplasia/squamous cell carcinoma (SCC) in situ was obtained in transmission by stitching together images of 256 x 256 µm recorded using a 96 x 96 element FPA detector. Each pixel spectrum was calculated from 128 co-added interferograms at 4 cm-1 resolution. In order to improve the signal to noise ratio, blocks of 4x4 adjacent pixels were subsequently averaged. Analyses of this spectral image, after conversion of the spectra to their second derivatives, show that the epithelium and the lamina propria tissue types can be distinguished using the area of troughs at either 1591, 1334, 1275 or 1215 cm-1 or, more effectively, by separation into two groups by hierarchical clustering (HCA) of the 1614-1465 region. Due to an insufficient signal to noise ratio, disease stages within the image could not be distinguished with this extent of pixel averaging. However, after separation of the cell types, disease stages within either the epithelium or the lamina propria could be distinguished if spectra were averaged from larger, manually selected areas of the tissue. Both cell types reveal spectral differences that follow a transition from normal to cancerous histology. For example, spectral changes that occurred in the epithelium over the transition from normal to carcinoma in situ could be seen in the 1200-1000 cm-1 region, particularly as a decrease in the second derivative troughs at 1074 and 1036 cm-1 , consistent with changes in some form of carbohydrate. Spectral differences that indicate a disease transition from normal to carcinoma in the lamina propria could be seen in the 1350-1175 cm-1 and 1125-1030 cm-1 regions. Thus demonstrating that a progression from healthy to severe dysplasia/squamous cell carcinoma (SCC) in situ can be seen using FTIR spectroscopic imaging and multivariate analysis.

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

NASA Astrophysics Data System (ADS)

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

2014-05-01

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

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

NASA Astrophysics Data System (ADS)

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

2014-10-01

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

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

PubMed

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

2002-10-01

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

Application of Attenuated Total Reflectance-Fourier Transformed Infrared (ATR-FTIR) Spectroscopy To Determine the Chlorogenic Acid Isomer Profile and Antioxidant Capacity of Coffee Beans.

PubMed

Liang, Ningjian; Lu, Xiaonan; Hu, Yaxi; Kitts, David D

2016-01-27

The chlorogenic acid isomer profile and antioxidant activity of both green and roasted coffee beans are reported herein using ATR-FTIR spectroscopy combined with chemometric analyses. High-performance liquid chromatography (HPLC) quantified different chlorogenic acid isomer contents for reference, whereas ORAC, ABTS, and DPPH were used to determine the antioxidant activity of the same coffee bean extracts. FTIR spectral data and reference data of 42 coffee bean samples were processed to build optimized PLSR models, and 18 samples were used for external validation of constructed PLSR models. In total, six PLSR models were constructed for six chlorogenic acid isomers to predict content, with three PLSR models constructed to forecast the free radical scavenging activities, obtained using different chemical assays. In conclusion, FTIR spectroscopy, coupled with PLSR, serves as a reliable, nondestructive, and rapid analytical method to quantify chlorogenic acids and to assess different free radical-scavenging capacities in coffee beans.

Crystal structure, molecular docking, and biological activity of the zinc complexes with 2-thenoyltrifluoroacetone and N-donor heterocyclic ligands

NASA Astrophysics Data System (ADS)

Eshaghi Malekshah, Rahime; Salehi, Mehdi; Kubicki, Maciej; Khaleghian, Ali

2017-12-01

Two novel mononuclear complexes, [Zn (TTA) (bipy)Cl] (1) and [Zn (TTA) (phen)Cl] (2) (TTA = 4,4,4-Trifluoro-1-(2-furyl)-1,3-butanedione, phen = 1,10-phenanthroline and bipy 2, 2ʹ-bipyridine), were synthesized and fully characterized by elemental analyses, 1H NMR, UV-Vis, FTIR spectroscopy, and conductivity measurements. The crystal structures of these two mono-nuclear zinc (II) complexes were determined by X-ray single-crystal diffraction. The result of X-ray diffraction analyses revealed that both complexes have distorted tetragonal-pyramid structures. In MTT cytotoxicity studies, these Zn (II) complexes exhibited antitumor activity against MCF-7 and MKN-45 cell lines. It was also found that the proliferation rate of MCF-7 and MKN-45 cells decreased after treatment with the above-mentioned complexes. In addition, the apoptosis-inducing activity was assessed by AO/EB (Acridine Orange/Ethidium bromide) staining assay and found that they have the potential to act as effective metal-based anticancer drugs. Finally, the molecular docking studies showed that complex 2 strongly binds through minor groove with DNA by relative binding energy -7.33 kcal mol-1.

One dimensional coordination polymers: Synthesis, crystal structures and spectroscopic properties

NASA Astrophysics Data System (ADS)

Karaağaç, Dursun; Kürkçüoğlu, Güneş Süheyla; Şenyel, Mustafa; Şahin, Onur

2016-11-01

Two new one dimensional (1D) cyanide complexes, namely [M(4-aepy)2(H2O)2][Pt(CN)4], (4-aepy = 4-(2-aminoethyl)pyridine M = Cu(II) (1) or Zn(II) (2)), have been synthesized and characterized by vibrational (FT-IR and Raman) spectroscopy, single crystal X-ray diffraction, thermal and elemental analyses techniques. The crystallographic analyses reveal that 1 and 2 are isomorphous and isostructural, and crystallize in the monoclinic system and C2 space group. The Pt(II) ions are coordinated by four cyanide-carbon atoms in the square-planar geometry and the [Pt(CN)4]2- ions act as a counter ion. The M(II) ions display an N4O2 coordination sphere with a distorted octahedral geometry, the nitrogen donors belonging to four molecules of the organic 4-aepy that act as unidentate ligands and two oxygen atoms from aqua ligands. The crystal structures of 1 and 2 are similar each other and linked via intermolecular hydrogen bonding, Pt⋯π interactions to form 3D supramolecular network. Vibration assignments of all the observed bands are given and the spectral features also supported to the crystal structures of the complexes.

Ultrasonic-assisted synthesis of nano lead(II) coordination polymer as precursors for preparation of lead(II) oxide nano-structures: Thermal, optical properties and XRD studies.

PubMed

Ghavidelaghdam, Elham; Shahverdizadeh, Gholam Hossein; Motameni Tabatabai, Javad; Mirtamizdoust, Babak

2018-04-01

Nano structure of a lead (II) coordination polymer [Pb 2 (C 2 Cl 3 O 2 ) 2 (NO 3 ) 2 (C l2 H 8 N 2 ) 2 ] n (1), has been synthesized by a sonochemical method in different concentrations. The nano particles were characterized by scanning electron microscopy (SEM) X-ray powder diffraction (XRD), FT-IR spectroscopy and elemental analyses. The thermal stability of nano structure is closely investigated via thermal gravimetric (TGA), and compared with crystalline structure. The compounds are then heated to 600 °C to produce PbO nano particles. The resulting PbO is characterized through XRD and SEM analyses. Concentration of initial reagents effects on size and morphology of nano-structured compound 1 have been studied and show that low concentrations of initial reagents decreased particles size and leaded to uniform nano particles morphology. The photoluminescence properties of the prepared compound, as crystalline and as nanoparticles, have been investigated. The result showed a good correlation between the size and emission wavelength. Copyright © 2017. Published by Elsevier B.V.

Fe (III), Co(II), Ni(II), Cu(II) and Zn(II) complexes of schiff bases based-on glycine and phenylalanine: Synthesis, magnetic/thermal properties and antimicrobial activity

NASA Astrophysics Data System (ADS)

Sevgi, Fatih; Bagkesici, Ugur; Kursunlu, Ahmed Nuri; Guler, Ersin

2018-02-01

Zinc (II), copper (II), nickel (II), cobalt (II) and iron (III) complexes of Schiff bases (LG, LP) derived from 2-hydroxynaphthaldehyde with glycine and phenylalanine were reported and characterized by 1H NMR, 13C NMR, elemental analyses, melting point, FT-IR, magnetic susceptibility and thermal analyses (TGA). TGA data show that iron and cobalt include to the coordinated water and metal:ligand ratio is 1:2 while the complex stoichiometry for Ni (II), Cu (II) and Zn (II) complexes is 1:1. As expected, Ni (II) and Zn (II) complexes are diamagnetic; Cu (II), Co (II) and Fe (III) complexes are paramagnetic character due to a strong ligand of LG and LP. The LG, LP and their metal complexes were screened for their antimicrobial activities against five Gram-positive (Staphylococcus aureus, Methicillin resistant Staphylococcus aureus (MRSA), Bacillus cereus, Streptococcus mutans and Enterococcus faecalis) and three Gram-negative (Escherichia coli, Klebsiella pneumoniae and Pseudomonas aeruginosa) and one fungi (Candida albicans) by using broth microdilution techniques. The activity data show that ligands and their metal complexes exhibited moderate to good activity against Gram-positive bacteria and fungi.

Serum-based diagnostic prediction of oral submucous fibrosis using FTIR spectrometry

NASA Astrophysics Data System (ADS)

Rai, Vertika; Mukherjee, Rashmi; Routray, Aurobinda; Ghosh, Ananta Kumar; Roy, Seema; Ghosh, Barnali Paul; Mandal, Puspendu Bikash; Bose, Surajit; Chakraborty, Chandan

2018-01-01

Oral submucous fibrosis (OSF) is found to have the highest malignant potentiality among all other pre-cancerous lesions. However, its detection prior to tissue biopsy can be challenging in clinics. Moreover, biopsy examination is invasive and painful. Hence, there is an urgent need of new technology that facilitates accurate diagnostic prediction of OSF prior to biopsy. Here, we used FTIR spectroscopy coupled with chemometric techniques to distinguish the serum metabolic signatures of OSF patients (n = 30) and healthy controls (n = 30). Serum biochemical analyses have been performed to further support the FTIR findings. Absorbance intensities of 45 infrared wavenumbers differed significantly between OSF and normal serum FTIR spectra representing alterations in carbohydrates, proteins, lipids and nucleic acids. Nineteen prominent significant wavenumbers (P ≤ 0.001) at 1020, 1025, 1035, 1039, 1045, 1078, 1055, 1100, 1117, 1122, 1151, 1169, 1243, 1313, 1398, 1453, 1544, 1650 and 1725 cm- 1 provided excellent segregation of OSF spectra from normal using multivariate statistical techniques. These findings provided essential information on the metabolic features of blood serum of OSF patients and established that FTIR spectroscopy coupled with chemometric analysis can be potentially useful in the rapid and accurate preoperative screening/diagnosis of OSF.

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

NASA Astrophysics Data System (ADS)

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

2018-01-01

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

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-).

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

PubMed Central

Chojnacka, Katarzyna

2014-01-01

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

Instrumental studies on silicone oil adsorption to the surface of intraocular lenses

NASA Astrophysics Data System (ADS)

Kim, Chun Ho; Joo, Choun-Ki; Chun, Heung Jae; Yoo, Bok Ryul; Noh, Dong Il; Shim, Young Bock

2012-12-01

The purpose of this study was to examine the degree of adherence of silicone oil to various intraocular lenses (IOLs) through comparison of the physico-chemical properties of the oil and IOLs. Four kinds of IOLs comprising various biomaterials were examined: PMMA (720A™), PHEMA (IOGEL 1103™), Acrysof (MA60BM™), and silicone (SI30NB™). Each lens was immersed in silicone oil or carboxylated silicone (CS-PDMS) oil for 72 h. For determination of the changes in chemical and elemental compositions on the surfaces of IOLs caused by the contact with silicone oil, IOLs were washed and rinsed with n-pentane to remove as much of the adsorbed silicone oil as possible, then subjected to Fourier transform infrared spectroscopic (FTIR) and X-ray photoelectron spectroscopic (XPS) analyses. The results of FTIR studies strongly indicate that washing with n-pentane completely removed the adhered silicone oil on the surfaces of PHEMA and Acrysof IOLs, whereas the residual silicone oil was detected on the surfaces of PMMA and silicone IOLs. XPS studies showed that silicone oil coverage of PMMA lenses was 12%, even after washing with n-pentane. In the case of silicone IOLs, the relative O1s peak area of carboxyl group in the residual CS-PDMS oil was found to be ˜2.7%. Considering that 2.8% carboxyl group-substituted silicone oil was used in the present study, CS-PDMS oil covered the entire surface of the silicone IOLs.

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

PubMed

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

2016-11-01

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

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.

Synthesize and Characterization of Hydroxypropyl-N-octanealkyl Chitosan Ramification

NASA Astrophysics Data System (ADS)

Tan, Fu-neng

2018-03-01

A new type of amphiphilic ramification, hydroxypropyl-N-octanealkyl chitosan was prepared from chitosan via hydrophilic group and hydrophobic group were introduced. We could protect the amino group of chitosan via the reaction of chitosan and benzaldehyde could get Schiff base structure. Structures of the products were characterized with FT-IR, elemental analysis, themogrammetry (TG) analysis and X-ray diffraction. The degree of substitution of hydrophobic group was studied by elemental analysis. The result showed this chitosan ramification was soluble, biocompatible, biodegradable and nontoxic.

Differential protein folding and chemical changes in lung tissues exposed to asbestos or particulates

PubMed Central

Pascolo, Lorella; Borelli, Violetta; Canzonieri, Vincenzo; Gianoncelli, Alessandra; Birarda, Giovanni; Bedolla, Diana E.; Salomé, Murielle; Vaccari, Lisa; Calligaro, Carla; Cotte, Marine; Hesse, Bernhard; Luisi, Fernando; Zabucchi, Giuliano; Melato, Mauro; Rizzardi, Clara

2015-01-01

Environmental and occupational inhalants may induce a large number of pulmonary diseases, with asbestos exposure being the most risky. The mechanisms are clearly related to chemical composition and physical and surface properties of materials. A combination of X-ray fluorescence (μXRF) and Fourier Transform InfraRed (μFTIR) microscopy was used to chemically characterize and compare asbestos bodies versus environmental particulates (anthracosis) in lung tissues from asbestos exposed and control patients. μXRF analyses revealed heterogeneously aggregated particles in the anthracotic structures, containing mainly Si, K, Al and Fe. Both asbestos and particulates alter lung iron homeostasis, with a more marked effect in asbestos exposure. μFTIR analyses revealed abundant proteins on asbestos bodies but not on anthracotic particles. Most importantly, the analyses demonstrated that the asbestos coating proteins contain high levels of β-sheet structures. The occurrence of conformational changes in the proteic component of the asbestos coating provides new insights into long-term asbestos effects. PMID:26159651

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

PubMed

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

2010-12-01

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

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.

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.

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

USGS Publications Warehouse

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

2010-01-01

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

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

USGS Publications Warehouse

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

2010-01-01

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

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

NASA Technical Reports Server (NTRS)

Pugel, Diane

2012-01-01

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

Recycling and Resistance of Petrogenic Particulate Organic Carbon: Implications from A Chemical Oxidation Method

NASA Astrophysics Data System (ADS)

Zhang, T.; Li, G.; Ji, J.

2013-12-01

Petrogenic particulate organic carbon (OCpetro) represents a small fraction of photosynthetic carbon which escapes pedogenic-petrogenic degradation and gets trapped in the lithosphere. Exhumation and recycling of OCpetro are of significant importance in the global carbon cycle because OCpetro oxidation represents a substantial carbon source to the atmosphere while the re-burial of OCpetro in sediment deposits has no net effect. Though studies have investigated various behaviors of OCpetro in the surface environments (e.g., riverine mobilization, marine deposition, and microbial remineralization), less attention has been paid to the reaction kinetics and structural transformations during OCpetro oxidation. Here we assess the OCpetro-oxidation process based on a chemical oxidation method adopted from soil studies. The employed chemical oxidation method is considered an effective simulation of natural oxidation in highly oxidative environments, and has been widely used in soil studies to isolate the inert soil carbon pool. We applied this chemical method to the OCpetro-enriched black shale samples from the middle-lower Yangtze (Changjiang) basin, China, and performed comprehensive instrumental analyses (element analysis, Fourier transform infrared (FTIR) spectrum, and Raman spectrum). We also conducted step-oxidizing experiments following fixed time series and monitored the reaction process in rigorously controlled lab conditions. In this work, we present our experiment results and discuss the implications for the recycling and properties of OCpetro. Particulate organic carbon concentration of black shale samples before and after oxidation helps to quantify the oxidability of OCpetro and constrain the preservation efficiency of OCpetro during fluvial erosion over large river basin scales. FTIR and Raman analyses reveal clear structural variations on atomic and molecular levels. Results from the step-oxidizing experiments provide detailed information about the reaction kinetics and allow differentiation of different components in OCpetro characterized by distinct reaction rates. All these results lead to a better understanding of OCpetro recycling in the surface environments, and furthermore, the role of OCpetro in the global carbon cycle.

Synthesis and characterization of nano-hydroxyapatite using Sapindus Mukorossi extract

NASA Astrophysics Data System (ADS)

Subha, B.; Prasath, P. Varun; Abinaya, R.; Kavitha, R. J.; Ravichandran, K.

2015-06-01

Nano-Hydroxyapatite (HAP) powders were successfully synthesised by hydrothermal method using Sapindus Mukorossi extract as an additive. The structural and morphological analyses of thus synthesised powders were carried out using FT-IR, XRD and FESEM/EDX. The FT-IR spectra confirm the presence of phosphate and hydroxyl groups corresponding to HAP. The XRD analysis reveals the formation of HAP phase and found to reduce the crystallite size with addition of Sapindus Mukorossi extract. The morphology changes from sphere to flake shape by the influence of extract.

FT-IR spectroscopic analysis for studying Clostridium cell response to conversion of enzymatically hydrolyzed hay

NASA Astrophysics Data System (ADS)

Grube, Mara; Gavare, Marita; Nescerecka, Alina; Tihomirova, Kristina; Mezule, Linda; Juhna, Talis

2013-07-01

Grass hay is one of assailable cellulose containing non-food agricultural wastes that can be used as a carbohydrate source by microorganisms producing biofuels. In this study three Clostridium strains Clostridium acetobutylicum, Clostridium beijerinckii and Clostridium tetanomorphum, capable of producing acetone, butanol and ethanol (ABE) were adapted to convert enzymatically hydrolyzed hay used as a growth media additive. The results of growth curves, substrate degradation kinetics and FT-IR analyses of bacterial biomass macromolecular composition showed diverse strain-specific cell response to the growth medium composition.

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

PubMed

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

2009-01-01

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

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.

Development of methodology for identification the nature of the polyphenolic extracts by FTIR associated with multivariate analysis

NASA Astrophysics Data System (ADS)

Grasel, Fábio dos Santos; Ferrão, Marco Flôres; Wolf, Carlos Rodolfo

2016-01-01

Tannins are polyphenolic compounds of complex structures formed by secondary metabolism in several plants. These polyphenolic compounds have different applications, such as drugs, anti-corrosion agents, flocculants, and tanning agents. This study analyses six different type of polyphenolic extracts by Fourier transform infrared spectroscopy (FTIR) combined with multivariate analysis. Through both principal component analysis (PCA) and hierarchical cluster analysis (HCA), we observed well-defined separation between condensed (quebracho and black wattle) and hydrolysable (valonea, chestnut, myrobalan, and tara) tannins. For hydrolysable tannins, it was also possible to observe the formation of two different subgroups between samples of chestnut and valonea and between samples of tara and myrobalan. Among all samples analysed, the chestnut and valonea showed the greatest similarity, indicating that these extracts contain equivalent chemical compositions and structure and, therefore, similar properties.

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

NASA Astrophysics Data System (ADS)

Baran, Talat; Menteş, Ayfer

2016-07-01

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

[Analysis and identification of emulsifying viscosity reducer by FTIR and 1H NMR].

PubMed

Zhu, Hong; Guan, Run-ling; Shen, Jing-mei

2007-01-01

Separation and purification of viscosity reducer for crude oil were performed with distillation and dissolution-precipitation. The functional group of its main component was identified by FTIR It was deduced that the main component of the crude oil viscosity reducer is the tricopolymer of poly ethyl acrylate/methyl methacrylate/acrylic acid. The structure of the component was also ascertained and quantitively analysed with 1 H NMR and MS. The mol ratio of the three monomers is 37. 1 : 25. 8 : 37. 1, and the mass ratio is 41. 1 : 28. 8 : 29. 8. The structure of the part soluble in methanol was identified by FTIR. The result showed that the nonionic sufactant is poly ethylene oxide with the moleculear mass range of 800-1600, and the anionic surfactant is alkylbenzene sulfonate. The residue is accessory ingredient and water.

Analysis of Colonial Currency

NASA Astrophysics Data System (ADS)

Kurkowski, Michael; Cangany, Catherine; Jordan, Louis; Manukyan, Khachatur; Schultz, Zachary; Wiescher, Michael

2017-09-01

This project entailed studying the cellulose in paper, the ink, colorants, and other materials used to produce American colonial currency. The technique primarily used in this project was X-Ray Fluorescence Spectroscopy (XRF). XRF mapping was used to provide both elemental analysis of large-scale objects as well as microscopic examination of individual pigment particles in ink, in addition to the inorganic additives used to prepare paper. The combination of elemental mapping with Fourier Transform Infrared (FTIR) and Raman Spectroscopies permits an efficient analysis of the currency. These spectroscopic methods help identify the molecular composition of the pigments. This combination of atomic and molecular analytical techniques provided an in-depth characterization of the paper currency on the macro, micro, and molecular levels. We have identified several of pigments that were used in the preparation of inks and colorants. Also, different inorganic crystals, such as alumina-silicates, have been detected in different papers. The FTIR spectroscopy allowed us to determine the type of cellulose fiber used in the production of paper currency. Our future research will be directed toward revealing important historical relationships between currencies printed throughout the colonies. ISLA Da Vinci Grant.

Synthesis and surface activity properties of alkylphenol polyoxyethylene nonionic trimeric surfactants

NASA Astrophysics Data System (ADS)

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

2010-10-01

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

Developments in FTIR spectroscopy of diamonds and better constraints on diamond thermal histories

NASA Astrophysics Data System (ADS)

Kohn, Simon; Speich, Laura; Smith, Christopher; Bulanova, Galina

2017-04-01

Fourier Transform Infrared (FTIR) spectroscopy is a commonly-used technique for investigating diamonds. It gives the most useful information if spatially-resolved measurements are used [1]. In this contribution we discuss the best way to acquire and present FTIR data from diamonds, using examples from Murowa (Zimbabwe), Argyle (Australia) and Machado River (Brazil). Examples of FTIR core-to-rim line scans, maps with high spatial resolution and maps with high spectral resolution that are fitted to extract the spatial variation of different nitrogen and hydrogen defects are presented. Model mantle residence temperatures are calculated from the concentration of A and B nitrogen-containing defects in the diamonds using known times of annealing in the mantle. A new, two-stage thermal annealing model is presented that better constrains the thermal history of the diamond and that of the mantle lithosphere in which the diamond resided. The effect of heterogeneity within the analysed FTIR volume is quantitatively assessed and errors in model temperatures that can be introduced by studying whole diamonds instead of thin plates are discussed. The kinetics of platelet growth and degradation will be discussed and the potential for two separate, kinetically-controlled defect reactions to be used to constrain a full thermal history of the diamond will be assessed. [1] Kohn, S.C., Speich, L., Smith, C.B. and Bulanova, G.P., 2016. FTIR thermochronometry of natural diamonds: A closer look. Lithos, 265, pp.148-158.

Analysis of clay smoking pipes from archeological sites in the region of the Guanabara Bay (Rio de Janeiro, Brazil) by FT-IR

NASA Astrophysics Data System (ADS)

Freitas, Renato P.; Ribeiro, Iohanna M.; Calza, Cristiane; Oliveira, Ana L.; Silva, Mariane L.; Felix, Valter S.; Ferreira, Douglas S.; Coelho, Felipe A.; Gaspar, Maria D.; Pimenta, André R.; Medeiros, Elanio A.; Lopes, Ricardo T.

2016-06-01

In this study, twenty samples of clay smoking pipes excavated in an 18 km2 area between the Macacu and Caceribu rivers, in the municipality of Itaboraí, Rio de Janeiro, Brazil were analyzed by FT-IR technique. The samples, excavated in different archeological sites of the region, are dated between the seventeenth and the nineteenth centuries and are part of the material culture left by Africans and African descendants that lived in the complex. FT-IR analyses and complementary SEM-EDS studies showed that the clay paste used in the manufacture of smoking pipes, mostly handcrafted, is composed of quartz, feldspar, phyllosilicates and iron oxides. Multivariate statistical tests (PCA) were applied to FT-IR data to assess the interactions between the archeological sites. The results indicated that one archeological site - Macacu IV - is greatly related to the other sites. The results obtained have helped archeologists and anthropologists in better understanding the manufacturing process employed in ancient ceramic artifacts produced during the period of colonial Brazil.

Analysis of clay smoking pipes from archeological sites in the region of the Guanabara Bay (Rio de Janeiro, Brazil) by FT-IR.

PubMed

Freitas, Renato P; Ribeiro, Iohanna M; Calza, Cristiane; Oliveira, Ana L; Silva, Mariane L; Felix, Valter S; Ferreira, Douglas S; Coelho, Felipe A; Gaspar, Maria D; Pimenta, André R; Medeiros, Elanio A; Lopes, Ricardo T

2016-06-15

In this study, twenty samples of clay smoking pipes excavated in an 18km(2) area between the Macacu and Caceribu rivers, in the municipality of Itaboraí, Rio de Janeiro, Brazil were analyzed by FT-IR technique. The samples, excavated in different archeological sites of the region, are dated between the seventeenth and the nineteenth centuries and are part of the material culture left by Africans and African descendants that lived in the complex. FT-IR analyses and complementary SEM-EDS studies showed that the clay paste used in the manufacture of smoking pipes, mostly handcrafted, is composed of quartz, feldspar, phyllosilicates and iron oxides. Multivariate statistical tests (PCA) were applied to FT-IR data to assess the interactions between the archeological sites. The results indicated that one archeological site - Macacu IV - is greatly related to the other sites. The results obtained have helped archeologists and anthropologists in better understanding the manufacturing process employed in ancient ceramic artifacts produced during the period of colonial Brazil. Copyright © 2016 Elsevier B.V. All rights reserved.

[Analysis and discrimination of Collocalia esculenta L. via FTIR spectroscopy].

PubMed

Deng, Yue-E; Sun, Su-Qin; Zhou, Qun; Li, Ao

2006-07-01

Collocalia esculenta L. is called Yanwo in China. Thirty kinds of dry yanwo were identified by Fourier transform infrared spectroscopy (FTIR) . The results indicated that there were some obvious differences in FTIR between the dry yanwo and the natural yanwo, mainly represented in some absorption peaks of protein, amino acid (1 634, 1 535 cm(-1)) and amylase (1 034 cm9-1)). Meanwhile, the shape, position and intensity of the peaks from methylene (2 935 cm(-1)), protein and amino acid (1 647, 1 533, 1 447 cm(-1)) in dry yanwo were similar to those of the glutin. Therefore, different amounts of glutin were added in dry yanwo samples. The content of candy in some dry candy yanwo products was as high as 99%, but the content of yanwo was only 1%. The characteristic peaks of yanwo in these products even could not be found. So the quality of yanwo in the market could not be guaranteed from these results. FTIR is fast and direct to analyse and evaluate the quality of yanwo product.

Synthesis and characterization of tetra phenoxy-substituted halogen-rich metallophthalocyanine derivatives: A study on their LCD color filter requirements

NASA Astrophysics Data System (ADS)

Muthukumar, Palanisamy; Kim, Hak-Soo; Jeong, Jong Woo; Son, Young-A.

2016-09-01

This study addresses the synthesis and characterization of new tetra phenoxy-substituted halogen-rich metallophthalocyanine derivatives (MPcs) 4-7 (M = Co, Ni, Cu and Zn). The synthesized new compounds were characterized using UV-Vis, FT-IR, MALDI-TOF, 1H NMR and elemental analyses. In addition, the basic requirements such as aggregation behavior, thermal stability, transmittance and solubility in propylene glycol monomethyl ether acetate (PGMEA) of MPcs 4-7 were investigated for their usage as a green color filter in Liquid Crystal Displays (LCDs). All of the MPcs showed thermal stability and sufficient solubility in PGMEA. However, the addition of binder into PGMEA solution of MPcs 5 and 6 leads to precipitation. Among the four MPcs, zinc phthalocyanine (7) showed higher transmittance. The higher transmittance of zinc phthalocyanine (7) along with its thermal stability and sufficient solubility in PGMEA are promising for its application as a green color filter in LCDs.

A new mixed-ligand copper(II) complex of (E)-N";-(2-hydroxybenzylidene) acetohydrazide: Synthesis, characterization, NLO behavior, DFT calculation and biological activities

NASA Astrophysics Data System (ADS)

Yousef Ebrahimipour, S.; Sheikhshoaie, Iran; Crochet, Aurelien; Khaleghi, Moj; Fromm, Katharina M.

2014-08-01

A tridentate hydrazone Schiff base ligand, (E)-N";-(2-hydroxybenzylidene)acetohydrazide [HL], and its mixed-ligand Cu(II) complex [CuL(phen)], have been synthesized and characterized by elemental analyses, FT-IR, molar conductivity, UV-Vis spectroscopy. The structure of the complex has been determined by X-ray diffraction. This complex has square pyramidal geometry and the positions around central atom are occupied with donor atoms of Schiff base ligand and two nitrogens of 1,10-phenanthroline. Computational studies of compounds were performed by using DFT calculations. The linear polarizabilities and first hyperpolarizabilities of the studied molecules indicate that these compounds can be good candidates of nonlinear optical materials. It is in accordance with experimental data. In addition, invitro antimicrobial results show that these compounds specially [CuL(phen)] have great potential of antibacterial activity against Escherichia coli, Staphylococcus aureus, Pseudomonas aeruginosa, Listeria monocytogenes bacteria and antifungal activity against Candida Albicans in comparison to some standard drugs.

Tuning effect of polysaccharide Chitosan on structural, morphological, optical and photoluminescence properties of ZnO nanoparticles

NASA Astrophysics Data System (ADS)

Magesh, G.; Bhoopathi, G.; Nithya, N.; Arun, A. P.; Ranjith Kumar, E.

2018-05-01

Chitosan/ZnO nanocomposites was synthesized by in-situ chemical precipitation method. The effect of polysaccharide Chitosan concentration (0.1 g, 0.5 g, 1 g and 3 g) was investigated by X-ray diffraction (XRD), Field Emission Scanning Electron Microscopy (FESEM) with Energy dispersive spectroscopy (EDX), High Resolution Transmission Electron Microscopy (HRTEM), UV-visible (UV), Fourier Transform Infrared (FTIR) and Photoluminescence Spectroscopy (PL). XRD pattern confirms the hexagonal wurtzite structure of the Chitosan/ZnO nanocomposites. The structural morphology and the elemental composition of the samples were analysed by FESEM and EDX respectively. From TEM analysis, it is observed that the particles in spindle shape morphology with average particle size ranges 10-20 nm. UV-Vis analysis reveals that the Chitosan concentration affect the absorption band edge and shift towards lower wavelength. The oxygen vacancy induced photoluminescence of ZnO nanoparticles was observed and its intensity decreases by tuning the Chitosan concentration.

Two Voriconazole salts: Syntheses, crystal structures, solubility and bioactivities

NASA Astrophysics Data System (ADS)

Tang, Gui-Mei; Wang, Yong-Tao

2018-01-01

Two Voriconazole salts, namely, (H2FZ)2+·2(Cl-) (1) and (HFZ)+·NO3- (2) (FZ = (2R,3S)-2-(2,4-difluorophenyl)-3-(5-fluoro-4-pyrimidiny)-1-(1H-1,2,4-triazol-1-yl)-2-butanol) have been obtained through the reaction of Voriconazole, hydrochloric acid and nitrate acid, respectively. They were structurally characterized by FT-IR, elemental analyses (EA), single crystal X-ray diffraction, and thermogravimetric analysis (TGA). A variety of hydrogen bonds (Osbnd H⋯N, Nsbnd H⋯Cl/O, Csbnd H⋯N/OF/Cl) were observed in the compounds 1 and 2, through which a 3D supramolecular architecture is generated. Both two salts 1 and 2 show the promising bioactivities against Aspergillus species (Aspergillus niger, Aspergillus terreus, Aspergillus fumigatus and Aspergillus flavus) and Candida ones (Candida albicans, Candida krusei, Candida glabrata and Cryptococcus neoformans), which is obviously more excellent than that of FZ. Additionally, the solubility of two salts is considerably higher than that of the drug Voriconazole.

Synthesis and characterization of a metal complex containing naringin and Cu, and its antioxidant, antimicrobial, antiinflammatory and tumor cell cytotoxicity.

PubMed

Pereira, Regina M S; Andrades, Norma E D; Paulino, Niraldo; Sawaya, Alexandra C H F; Eberlin, Marcos N; Marcucci, Maria C; Favero, Giovani Marino; Novak, Estela Maria; Bydlowski, Sérgio Paulo

2007-07-09

The antioxidant activity of flavonoids is believed to increase when they are coordinated with transition metal ions. However, the literature on this subject is contradictory and the outcome seems to largely depend on the experimental conditions. In order to understand the contribution of the metal coordination and the type of interaction between a flavonoid and the metal ion, in this study a new metal complex of Cu (II) with naringin was synthesized and characterized by FT-IR, UV-VIS, mass spectrometry (ESI-MS/MS), elemental analysis and 1H-NMR. The results of these analyses indicate that the complex has a Cu (II) ion coordinated via positions 4 and 5 of the flavonoid. The antioxidant, anti-inflammatory and antimicrobial activities of this complex were studied and compared with the activity of free naringin. The Naringin-Cu (II) complex 1 showed higher antioxidant, anti-inflammatory and tumor cell cytotoxicity activities than free naringin without reducing cell viability.

Synthesis, structural, spectroscopic and optical studies of charge transfer complex salts.

PubMed

Manikandan, Maruthappan; Mahalingam, Thaiyan; Hayakawa, Yasuhiro; Ravi, Ganesan

2013-01-15

New charge transfer molecular complex adducts of picric acid (C6H3N3O7) with triethylamine (C6H15N) and dimethylformamide (HCON(CH3)2) were synthesized successfully for the first time. Chemical composition and stoichiometry of the synthesized complex salts were verified by CHN elemental analysis. Solubility of the complex salts have been determined by gravimetric method and single crystals of two new salts were grown by low temperature solution growth technique. Crystal system, crystalline nature and cell parameters of the grown crystals were determined by single crystal X-ray diffraction (SXRD) and powder X-ray diffraction (PXRD) analyses. The formations of the charge-transfer complex, functional groups and the modes of vibrations have been confirmed by Fourier transform infrared (FTIR) spectroscopy. In order to know the linear and nonlinear optical suitability for device fabrication, UV-Vis (UV) spectral analysis and relative second harmonic generation (SHG) efficiency test were performed for the grown crystals. Copyright © 2012 Elsevier B.V. All rights reserved.

Synthesis, spectral, structural prediction and computational studies of octylcarbazole ornamented 3-phenothiazinal

NASA Astrophysics Data System (ADS)

Karuppasamy, Ayyanar; Udhaya kumar, Chandran; Karthikeyan, Subramanian; Velayutham Pillai, Muthiah Pillai; Ramalingan, Chennan

2017-11-01

A novel conjugated octylcarbazole ornamented 3-phenothiazinal, 10-(9-octyl-9H-carbazol-3-yl)-10H-phenothiazine-3-carbaldehyde (OCPTC) was synthesized and fully characterized by 1H-NMR, 13C-NMR, elemental and single crystal XRD analyses. The optimized geometrical structure, vibrational frequencies and NMR have been computed with M06-2X method using 6-31+G(d,p) basis set. Total electronic energies and HOMO-LUMO energy gaps in gas phase are discussed. The geometrical parameters of the title compound obtained from single crystal XRD studies have been found in accord with the calculated (DFT) values. The experimental and theoretical FT-IR and NMR results of the title molecule have been investigated. The experimentally observed vibrational frequencies have been compared with the calculated ones, which are in good agreement with each other. Single crystal X-ray structural analysis of OCPTC, evidences the ''butterfly conformation'' of phenothiazine ring with nearly perpendicular orientation of the carbazole structural motif to the phenothiazine moiety.

Compositional insights and valorization pathways for carbonaceous material deposited during bio-oil thermal treatment.

PubMed

Ochoa, Aitor; Aramburu, Borja; Ibáñez, María; Valle, Beatriz; Bilbao, Javier; Gayubo, Ana G; Castaño, Pedro

2014-09-01

This work analyses the composition, morphology, and thermal behavior of the carbonaceous materials deposited during the thermal treatment of bio-oil (thermal pyrolytic lignin-TPL). The bio-oil was obtained by flash pyrolysis of lignocellulosic biomass (pine sawdust), and the TPLs were obtained in the 400-700 °C range. The TPLs were characterized by performing elemental analysis; (13)C NMR, Raman, FTIR, and X-ray photoelectron spectroscopy; SEM; and temperature-programmed oxidation analyzed by differential thermogravimetry and differential scanning calorimetry. The results are compared to a commercial lignin (CL). The TPLs have lower oxygen and hydrogen contents and a greater aromaticity and structural order than the CL material. Based on these features, different valorization routes are proposed: the TPL obtained at 500 °C is suitable for use as a fuel, and the TPL obtained at 700 °C has a suitable morphology and composition for use as an adsorbent or catalyst support. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A novel methanol sensor based on gas-penetration through a porous polypyrrole-coated polyacrylonitrile nanofiber mat.

PubMed

Jun, Tae-Sun; Ho, Thi Anh; Rashid, Muhammad; Kim, Yong Shin

2013-09-01

In this work, we propose a novel chemoresistive gas sensor operated under a vertical analyte flow passing through a permeable sensing membrane. Such a configuration is different from the use of a planar sensor implemented under a conventional horizontal flow. A highly porous core-shell polyacrylonitrile-polypyrrole (PAN@PPy) nanofiber mat was prepared as the sensing element via electrospinning and two-step vapor-phase polymerization (VPP). Various analysis methods such as SEM, TEM, FT-IR and XPS measurements were employed in order to characterize structural features of the porous sensing mat. These analyses confirmed that very thin (ca. 10 nm) conductive PPy sheath layers were deposited by VPP on electrospun PAN nanofibers with an average diameter of 258 nm. Preliminary results revealed that the gas penetration-type PAN@PPy sensor had a higher sensor response and shorter detection and recovery times upon exposure to methanol analyte when compared with a conventional horizontal flow sensor due to efficient and fast analyte transfer into the sensing layer.

Fabrication and characterization of magnesium and calcium trimesate complexes via ion-exchange and one-pot self-assembly reaction

NASA Astrophysics Data System (ADS)

Ozer, Demet; Oztas, Nursen Altuntas; Köse, Dursun A.; Şahin, Onur

2018-03-01

Using two different synthesis methods, two diversified magnesium and calcium complexes were successfully prepared. When the ion exchange method was used, C9H14MgO11.H2O and C18H30Ca3O24 complexes were obtained. When the one-pot self-assembly reaction was used, C18H34Mg3O26.4H2O and C9H12CaO10 complexes were produced. The structural characterizations were performed by using X-ray diffraction, FT-IR and elemental analyses. Thermal behavior of complexes were also determined via TGA method. The both complexes of magnesium and calcium trimesate have micro and mesoporosity with low porosity because of hydrogen bonds. Then hydrogen storage capacities of complexes were also determined. The differences in synthesis method result in the differences on complexes structure, morphology (shape, particle size and specific surface area) and hydrogen storage capacities.

Synthesis and characterization of boric acid mediated metal-organic frameworks based on trimesic acid and terephthalic acid

NASA Astrophysics Data System (ADS)

Ozer, Demet; Köse, Dursun A.; Şahin, Onur; Oztas, Nursen Altuntas

2017-08-01

The new metal-organic framework materials based on boric acid reported herein. Sodium and boron containing metal-organic frameworks were synthesized by one-pot self-assembly reaction in the presence of trimesic acid and terephthalic acid in water/ethanol solution. Boric acid is a relatively cheap boron source and boric acid mediated metal-organic framework prepared mild conditions compared to the other boron source based metal-organic framework. The synthesized compounds were characterized by FT-IR, p-XRD, TGA/DTA, elemental analysis, 13C-MAS NMR, 11B-NMR and single crystal measurements. The molecular formulas of compounds were estimated as C18H33B2Na5O28 and C8H24B2Na2O17 according to the structural analysis. The obtained complexes were thermally stable. Surface properties of inorganic polymer complexes were investigated by BET analyses and hydrogen storage properties of compound were also calculated.

Synthesis, structural, spectroscopic and optical studies of charge transfer complex salts

NASA Astrophysics Data System (ADS)

Manikandan, Maruthappan; Mahalingam, Thaiyan; Hayakawa, Yasuhiro; Ravi, Ganesan

2013-01-01

New charge transfer molecular complex adducts of picric acid (C6H3N3O7) with triethylamine (C6H15N) and dimethylformamide (HCON(CH3)2) were synthesized successfully for the first time. Chemical composition and stoichiometry of the synthesized complex salts were verified by CHN elemental analysis. Solubility of the complex salts have been determined by gravimetric method and single crystals of two new salts were grown by low temperature solution growth technique. Crystal system, crystalline nature and cell parameters of the grown crystals were determined by single crystal X-ray diffraction (SXRD) and powder X-ray diffraction (PXRD) analyses. The formations of the charge-transfer complex, functional groups and the modes of vibrations have been confirmed by Fourier transform infrared (FTIR) spectroscopy. In order to know the linear and nonlinear optical suitability for device fabrication, UV-Vis (UV) spectral analysis and relative second harmonic generation (SHG) efficiency test were performed for the grown crystals.

Synthesis 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.

Chromium and yttrium-doped magnesium aluminum oxides prepared from layered double hydroxides

NASA Astrophysics Data System (ADS)

García-García, J. M.; Pérez-Bernal, M. E.; Ruano-Casero, R. J.; Rives, V.

2007-12-01

Layered double hydroxides with the hydrotalcite-like structures, containing Mg 2+ and Al 3+, doped with Cr 3+ and Y 3+, have been prepared by precipitation at constant pH. The weight percentages of Cr 3+ and Y 3+ were 1, 2, or 3%, and 0.5 or 1%, respectively. Single phases were obtained in all cases, whose crystallinity decreased as the content in Cr and Y was increased. The solids have been characterised by element chemical analysis, powder X-ray diffraction, thermal analyses (differential, thermogravimetric and programmed reduction), FT-IR and UV-vis spectroscopies; the specific surface areas have been determined from nitrogen adsorption isotherms at -196 °C. Upon calcination at 1200 °C for 5 h in air all solids display a mixed structure (spinel and rock salt for MgO); these solids have also been characterised by these techniques and their chromatic coordinates (CIE - L∗a∗b∗) have been determined. Their pink colour makes these solids suitable for being used as ceramic pigments.

Isolation and characterization of cellulose nanofibers from bamboo using microwave liquefaction combined with chemical treatment and ultrasonication.

PubMed

Xie, Jiulong; Hse, Chung-Yun; De Hoop, Cornelis F; Hu, Tingxing; Qi, Jinqiu; Shupe, Todd F

2016-10-20

Cellulose nanofibers were successfully isolated from bamboo using microwave liquefaction combined with chemical treatment and ultrasonic nanofibrillation processes. The microwave liquefaction could eliminate almost all the lignin in bamboo, resulting in high cellulose content residues within 7min, and the cellulose enriched residues could be readily purified by subsequent chemical treatments with lower chemical charging and quickly. The results of wet chemistry analyses, SEM images, and FTIR and X-ray spectra indicated the combination of microwave liquefaction and chemical treatment was significantly efficient in removing non-cellulosic compounds. Ultrasonication was used to separate the nanofibrils from the purified residues to extract nanofibers. The TEM images confirmed the presence of elementary fibrils, nano-sized fibril bundles, and aggregated fibril bundles. As evidenced by the TGA analysis, cellulose nanofibers isolated by this novel technique had high thermal stability indicating that the isolated nanofibers could possibly be applied as reinforcing elements in biomaterials. Copyright © 2016 Elsevier Ltd. All rights reserved.

The Study of Blocking Agent on Lengkeng (Euphoria Logan Lour) Fruit Shell and Seed for Adsorption of Pb (II) from Aqueous Solution

NASA Astrophysics Data System (ADS)

Kurniawati, D.; Zein, R.; Chaidir, Z.; Aziz, H.

2018-04-01

The study focuses on the roles played by mayor functional groups(carboxyl) in the lengkeng shell for sorption of Pb (II). The biosorbent was characterized by FTIR and elemental analyses. The parameters such as pH, initial concentration, particle sizes, adsorbent dose and flow rate were also studied. The results showed that the optimum condition was at pH = 3, concentration 400 mg/l, 250 μm particle sizes, adsorbent dose 0,5 g and 2 ml/min flow rate with adsorption capacity 4,8933 mg/g(shell) and 5,2720 mg/g(seed). It is show that ion exchange play as a more important role in the sorption of Pb (II) on lengkeng shell and seed. Blocking of COOH groups by chemical esterification resulted in Pb important reduction in metal binding.The result showed that adsorption capacity of lengkeng shell uncreases until 63.67 % and lengkeng seed uncreases 98.70%.

Preparation, characterization, and anti-Helicobacter pylori activity of Bi3+-Hericium erinaceus polysaccharide complex.

PubMed

Zhu, Yang; Chen, Yao; Li, Qian; Zhao, Ting; Zhang, Ming; Feng, Weiwei; Takase, Mohammed; Wu, Xueshan; Zhou, Zhaoxiang; Yang, Liuqing; Wu, Xiangyang

2014-09-22

Two new Bi3+-Hericium erinaceus polysaccharide (BiHEP) complexes were prepared using Bi3+ and two purified polysaccharides from H. erinaceus (HEPs), respectively. The complexes were characterized by elemental analysis, FT-IR, CD, SEM, AFM, XRD, and TG. The anti-Helicobacter pylori (Hp) activities in vitro by agar dilution assay of the complexes were evaluated. The molecular weights of HEPs were 197 and 20 kDa, respectively. All the analyses confirmed the formation of new BiHEP complexes with lower content of Bi3+ compared with colloidal bismuth subcitrate (CBS), the most utilized bismuth preparation clinically. Furthermore, HEPs themselves have definite inhibition effects on Hp, and BiHEP complexes have lower content of Bi exhibited strong inhibition effects on Hp (MIC=20 μg/mL), similar to that of CBS with higher content of Bi. The study provides a basis for further development of multiple treatments of Hp infection or new medicines. Copyright © 2014 Elsevier Ltd. All rights reserved.

The BALDER Beamline at the MAX IV Laboratory

NASA Astrophysics Data System (ADS)

Klementiev, K.; Norén, K.; Carlson, S.; Sigfridsson Clauss, K. G. V.; Persson, I.

2016-05-01

X-ray absorption spectroscopy (XAS) includes well-established methods to study the local structure around the absorbing element - extended X-ray absorption fine structure (EXAFS), and the effective oxidation number or to quantitatively determine the speciation of an element in a complex matrix - X-ray absorption near-edge structure (XANES). The increased brilliance and intensities available at the new generation of synchrotron light sources makes it possible to study, in-situ and in-operando, much more dilute systems with relevance for natural systems, as well as the micro-scale variability and dynamics of chemical reactions on the millisecond time-scale. The design of the BALDER beamline at the MAX IV Laboratory 3 GeV ring has focused on a high flux of photons in a wide energy range, 2.4-40 keV, where the K-edge is covered for the elements S to La, and the L 3-edge for all elements heavier than Sb. The overall design of the beamline will allow large flexibility in energy range, beam size and data collection time. The other focus of the beamline design is the possibility to perform multi-technique analyses on samples. Development of sample environment requires focus on implementation of auxiliary methods in such a way that techniques like Fourier transform infrared (FTIR) spectroscopy, UV-Raman spectroscopy, X-ray diffraction and/or mass spectrometry can be performed simultaneously as the XAS study. It will be a flexible system where different instruments can be plugged in and out depending on the needs for the particular investigation. Many research areas will benefit from the properties of the wiggler based light source and the capabilities to perform in-situ and in-operando measurements, for example environmental and geochemical sciences, nuclear chemistry, catalysis, materials sciences, and cultural heritage.

A Novel Synthesis Routine for Woodwardite and Its Affinity towards Light (La, Ce, Nd) and Heavy (Gd and Y) Rare Earth Elements.

PubMed

Consani, Sirio; Balić-Žunić, Tonci; Cardinale, Anna Maria; Sgroi, Walter; Giuli, Gabriele; Carbone, Cristina

2018-01-14

A synthetic Cu-Al-SO₄ layered double hydroxide (LDH), analogue to the mineral woodwardite [Cu 1-x Al x (SO₄) x/2 (OH)₂·nH₂O], with x < 0.5 and n ≤ 3x/2, was synthesised by adding a solution of Cu and Al sulphates to a solution with NaOH. The pH values were kept constant at 8.0 and 10.0 by a continuous addition of NaOH. The material obtained had poor crystallinity, turbostratic structure, and consisted of nanoscopic crystallites. The analyses performed in order to characterise the obtained materials (X-ray diffraction (XRD), thermogravimetry (TG), and Fourier Transform Infra-Red (FTIR) spectroscopy) showed that the Cu-Al-SO₄ LDH is very similar to woodwardite, although it has a smaller layer spacing, presumably due to a lesser water content than in natural samples. The synthesis was performed by adding light rare earth elements (LREEs) (La, Ce, and Nd) and heavy rare earth elements (HREEs) (Gd and Y) in order to test the affinity of the Cu-Al-SO₄ LDH to the incorporation of REEs. The concentration of rare earth elements (REEs) in the solid fraction was in the range of 3.5-8 wt %. The results showed a good affinity for HREE and Nd, especially for materials synthesised at pH 10.0, whereas the affinities for Ce and La were much lower or non-existent. The thermal decomposition of the REE-doped materials generates a mixture of Cu, Al, and REE oxides, making them interesting as precursors in REE oxide synthesis.

A Novel Synthesis Routine for Woodwardite and Its Affinity towards Light (La, Ce, Nd) and Heavy (Gd and Y) Rare Earth Elements

PubMed Central

Consani, Sirio; Balić-Žunić, Tonci; Cardinale, Anna Maria; Sgroi, Walter; Giuli, Gabriele; Carbone, Cristina

2018-01-01

A synthetic Cu-Al-SO4 layered double hydroxide (LDH), analogue to the mineral woodwardite [Cu1−xAlx(SO4)x/2(OH)2·nH2O], with x < 0.5 and n ≤ 3x/2, was synthesised by adding a solution of Cu and Al sulphates to a solution with NaOH. The pH values were kept constant at 8.0 and 10.0 by a continuous addition of NaOH. The material obtained had poor crystallinity, turbostratic structure, and consisted of nanoscopic crystallites. The analyses performed in order to characterise the obtained materials (X-ray diffraction (XRD), thermogravimetry (TG), and Fourier Transform Infra-Red (FTIR) spectroscopy) showed that the Cu-Al-SO4 LDH is very similar to woodwardite, although it has a smaller layer spacing, presumably due to a lesser water content than in natural samples. The synthesis was performed by adding light rare earth elements (LREEs) (La, Ce, and Nd) and heavy rare earth elements (HREEs) (Gd and Y) in order to test the affinity of the Cu-Al-SO4 LDH to the incorporation of REEs. The concentration of rare earth elements (REEs) in the solid fraction was in the range of 3.5–8 wt %. The results showed a good affinity for HREE and Nd, especially for materials synthesised at pH 10.0, whereas the affinities for Ce and La were much lower or non-existent. The thermal decomposition of the REE-doped materials generates a mixture of Cu, Al, and REE oxides, making them interesting as precursors in REE oxide synthesis. PMID:29342887

Characterization of minerals in air dust particles in the state of Tamilnadu, India through FTIR, XRD and SEM analyses

NASA Astrophysics Data System (ADS)

Senthil Kumar, R.; Rajkumar, P.

2014-11-01

The abstract of this paper explains the presence of minerals in air which causes great concern regarding public health issues. The spectroscopic investigation of air dust particles of several samples in various locations in the state of Tamilnadu, India is reported. Qualitative analyses were carried out to determine the major and minor constituent minerals present in the samples based on the FTIR, XRD absorption peaks. This study also identified the minerals like quartz, asbestos, kaolinite, calcite, hematite, montmorillonite, nacrite and several other trace minerals in the air dust particles. The presents of quartz is mainly found in all the samples invariably. Hence the percentage of quartz and its crystalline nature were determined with the help of extinction co-efficient and crystallinity index respectively. The shape and size of the particulates are studied with SEM analysis.

Development of methodology for identification the nature of the polyphenolic extracts by FTIR associated with multivariate analysis.

PubMed

Grasel, Fábio dos Santos; Ferrão, Marco Flôres; Wolf, Carlos Rodolfo

2016-01-15

Tannins are polyphenolic compounds of complex structures formed by secondary metabolism in several plants. These polyphenolic compounds have different applications, such as drugs, anti-corrosion agents, flocculants, and tanning agents. This study analyses six different type of polyphenolic extracts by Fourier transform infrared spectroscopy (FTIR) combined with multivariate analysis. Through both principal component analysis (PCA) and hierarchical cluster analysis (HCA), we observed well-defined separation between condensed (quebracho and black wattle) and hydrolysable (valonea, chestnut, myrobalan, and tara) tannins. For hydrolysable tannins, it was also possible to observe the formation of two different subgroups between samples of chestnut and valonea and between samples of tara and myrobalan. Among all samples analysed, the chestnut and valonea showed the greatest similarity, indicating that these extracts contain equivalent chemical compositions and structure and, therefore, similar properties. Copyright © 2015 Elsevier B.V. All rights reserved.

Structure-activity relations of 2-(methylthio)benzimidazole by FTIR, FT-Raman, NMR, DFT and conceptual DFT methods.

PubMed

Arjunan, V; Raj, Arushma; Ravindran, P; Mohan, S

2014-01-24

The vibrational fundamental modes of 2-(methylthio)benzimidazole (2MTBI) have been analysed by combining FTIR, FT-Raman and quantum chemical calculations. The structural parameters of the compound are determined from the optimised geometry by B3LYP with 6-31G(∗∗), 6-311++G(∗∗) and cc-pVTZ basis sets and giving energies, harmonic vibrational frequencies, depolarisation ratios, IR intensities and Raman activities. (1)H and (13)C NMR spectra have been analysed and (1)H and (13)C nuclear magnetic resonance chemical shifts are calculated using the gauge independent atomic orbital (GIAO) method. The structure-activity relationship of the compound is also investigated by conceptual DFT methods. The chemical reactivity and site selectivity of the molecule has been determined with the help of global and local reactivity descriptors. Copyright © 2013 Elsevier B.V. All rights reserved.

Chemical and biological evaluation of moxifloxacin-benzimidazole mixed ligands complexes: Anti-cancer and anti-oxidant activities

NASA Astrophysics Data System (ADS)

Refaat, Heba M.; Noor El-Din, Doaa A.

2018-07-01

Novel complexes of the formula [M(MOX)(Ben)Cl(H2O)m].nH2O and [Ag(MOX)(Ben)] 3.5H2O; M = Co, Ni, and Zn, n = 1.5, 2 and 1, m = 0 or 2, MOX; Moxifloxacin and Ben; benzimidazole, were synthesized. Their effect on different cancer cells together with bacterial and fungal activity was determined. Formulation of the complexes was based on elemental analyses, different spectrophotometric methods (FT-IR, UV/Vis, NMR), and magnetic studies. FT-IR data indicated that the bonding of the Co(II), Ni(II) and Zn(II) ions with MOX to be achieved through the quinolone and carboxylate oxygen atoms. On the other hand Ag(I) bonded to the MOX through hydro-pyrrolopyridine nitrogen atom. TGA and DTA studies for the metal complexes showed them to possess considerable stability. Thermodynamic parameters ΔE*, ΔS* and ΔH* were evaluated and the appearance of fractional orders suggested that the reactions proceed via complicated mechanisms. The novel mixed ligands complexes were evaluated for their biological activity against the bacterial species (S. aureus) and (E. coli) and the fungal species Aspergillus flavus and Candida albicans. The complexes were found to possess better antibacterial and antifungal activities compared to the Moxifloxacin ligand. The compounds' effects were also screened for their anti-oxidant activity by DPPH method and were tested for their cytotoxicity activity against Breast cancer cell lines (MCF-7), Colon carcinoma cells (HCT) and Hepatocellular carcinoma cells (HepG2) by viability assay method.

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%.

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

PubMed

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

2017-07-06

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

Site-selective modification of cellulose nanocrystals with isophorone diisocyanate and formation of polyurethane-CNC composites

Treesearch

Natalie M. Girouard; Shanhong Xu; Gregory T. Schueneman; Meisha L. Shofner; J. Carson Meredith

2016-01-01

The unequal reactivity of the two isocyanate groups in an isophorone diisocyante (IPDI) monomer was exploited to yield modified cellulose nanocrystals (CNCs) with both urethane and isocyanate functionality. The chemical functionality of the modified CNCs was verified with ATR-FTIR analysis and elemental analysis. The selectivity for the secondary isocyanate group using...

Ultrasound-assisted facile synthesis of a new tantalum(V) metal-organic framework nanostructure: Design, characterization, systematic study, and CO2 adsorption performance

NASA Astrophysics Data System (ADS)

Sargazi, Ghasem; Afzali, Daryoush; Mostafavi, Ali; Ebrahimipour, S. Yousef

2017-06-01

This work presents a fast route for the preparation of a new Ta(V) metal-organic framework nanostructure with high surface area, significant porosity, and small size distribution. X-ray diffraction (XRD), scanning electron microscopy (SEM), Transition electron microscopy (TEM), energy dispersive spectrometer (EDS), thermo-gravimetric analysis (TGA), differential scanning calorimetry (DSC), fourier transform infrared spectroscopy (FTIR), CHNS/O elemental analyser, and Brunauer-Emmett-Teller (BET) surface area analysis were applied to characterize the synthesized product. Moreover, the influences of ultrasonic irradiation including temperature, time, and power on different features of the final products were systematically studied using 2k-1 factorial design experiments, and the response surface optimization was used for determining the best welding parameter combination. The results obtained from analyses of variances showed that ultrasonic parameters affected the size distribution, thermal behaviour, and surface area of Ta-MOF samples. Based on response surface methodology, Ta-MOF could be obtained with mean diameter of 55 nm, thermal stability of 228 °C, and high surface area of 2100 m2/g. The results revealed that the synthesized products could be utilized in various applications such as a novel candidate for CO2 adsorption.

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

PubMed Central

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

2018-01-01

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

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

PubMed

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

2018-01-01

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

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

PubMed

Ryu, JiYeon; Ro, Chul-Un

2009-08-15

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

Development of acceptance criteria for batches of silane primer for external tank thermal protection system bonding applications

NASA Technical Reports Server (NTRS)

Mikes, F.

1985-01-01

Concluding tests for the thermogravimetric and FTIR analyses of DC 1200 silane primers are discussed as well as methods for HPLC and GC analyses and for determining titanium and silicon by atomic absorption spectroscopy. Tables summarizes results obtained for residue, ash, titanium, silicone, Si/Ti ratio, OH-absorption, the lap-shear test, and the GC headspace for alcohols.

Study of melanoma invasion by FTIR spectroscopy

NASA Astrophysics Data System (ADS)

Yang, Y.; Sulé-Suso, J.; Sockalingum, G. D.

2008-02-01

Compared to other forms of skin cancer, a malignant melanoma has a high risk of spreading to other parts of the body. Melanoma invasion is a complex process involving changes in cell-extracellular matrix (ECM) interaction and cell-cell interactions. To fully understand the factors which control the invasion process, a human skin model system was reconstructed. HBL (a commercially available cell line) melanoma cells were seeded on a skin model with and without the presence of keratinocytes and/or fibroblasts. After 14 days culture, the skin specimens were fixed, parafin embedded and cut into 7 µm sections. The de-parafinised sections were investigated by synchrotron Fourier transformed infrared (FTIR) microspectroscopy to study skin cell invasion behaviour. The advantage of using FTIR is its ability to obtain the fingerprint information of the invading cells in terms of protein secondary structure in comparison to non-invading cells and the concentration of the enzyme (matrix-metalloproteinase) which digests protein matrix, near the invading cells. With aid of the spectral mapping images, it is possible to pinpoint the cells in non-invasion and invasion area and analyse the respective spectra. It has been observed that the protein bands in cells and matrix shifted between non-invasive and invasive cells in the reconstructed skin model. We hypothesise that by careful analysis of the FTIR data and validation by other models, FTIR studies can reveal information on which type of cells and proteins are involved in melanoma invasion. Thus, it is possible to trace the cell invasion path by mapping the spectra along the interface of cell layer and matrix body by FTIR spectroscopy.

Rapid estimation of sugar release from winter wheat straw during bioethanol production using FTIR-photoacoustic spectroscopy

DOE PAGES

Bekiaris, Georgios; Lindedam, Jane; Peltre, Clément; ...

2015-06-18

Complexity and high cost are the main limitations for high-throughput screening methods for the estimation of the sugar release from plant materials during bioethanol production. In addition, it is important that we improve our understanding of the mechanisms by which different chemical components are affecting the degradability of plant material. In this study, Fourier transform infrared photoacoustic spectroscopy (FTIR-PAS) was combined with advanced chemometrics to develop calibration models predicting the amount of sugars released after pretreatment and enzymatic hydrolysis of wheat straw during bioethanol production, and the spectra were analysed to identify components associated with recalcitrance. A total of 1122more » wheat straw samples from nine different locations in Denmark and one location in the United Kingdom, spanning a large variation in genetic material and environmental conditions during growth, were analysed. The FTIR-PAS spectra of non-pretreated wheat straw were correlated with the measured sugar release, determined by a high-throughput pretreatment and enzymatic hydrolysis (HTPH) assay. A partial least square regression (PLSR) calibration model predicting the glucose and xylose release was developed. The interpretation of the regression coefficients revealed a positive correlation between the released glucose and xylose with easily hydrolysable compounds, such as amorphous cellulose and hemicellulose. Additionally, we observed a negative correlation with crystalline cellulose and lignin, which inhibits cellulose and hemicellulose hydrolysis. FTIR-PAS was used as a reliable method for the rapid estimation of sugar release during bioethanol production. The spectra revealed that lignin inhibited the hydrolysis of polysaccharides into monomers, while the crystallinity of cellulose retarded its hydrolysis into glucose. Amorphous cellulose and xylans were found to contribute significantly to the released amounts of glucose and xylose, respectively.« less

Rapid estimation of sugar release from winter wheat straw during bioethanol production using FTIR-photoacoustic spectroscopy

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

Bekiaris, Georgios; Lindedam, Jane; Peltre, Clément

Complexity and high cost are the main limitations for high-throughput screening methods for the estimation of the sugar release from plant materials during bioethanol production. In addition, it is important that we improve our understanding of the mechanisms by which different chemical components are affecting the degradability of plant material. In this study, Fourier transform infrared photoacoustic spectroscopy (FTIR-PAS) was combined with advanced chemometrics to develop calibration models predicting the amount of sugars released after pretreatment and enzymatic hydrolysis of wheat straw during bioethanol production, and the spectra were analysed to identify components associated with recalcitrance. A total of 1122more » wheat straw samples from nine different locations in Denmark and one location in the United Kingdom, spanning a large variation in genetic material and environmental conditions during growth, were analysed. The FTIR-PAS spectra of non-pretreated wheat straw were correlated with the measured sugar release, determined by a high-throughput pretreatment and enzymatic hydrolysis (HTPH) assay. A partial least square regression (PLSR) calibration model predicting the glucose and xylose release was developed. The interpretation of the regression coefficients revealed a positive correlation between the released glucose and xylose with easily hydrolysable compounds, such as amorphous cellulose and hemicellulose. Additionally, we observed a negative correlation with crystalline cellulose and lignin, which inhibits cellulose and hemicellulose hydrolysis. FTIR-PAS was used as a reliable method for the rapid estimation of sugar release during bioethanol production. The spectra revealed that lignin inhibited the hydrolysis of polysaccharides into monomers, while the crystallinity of cellulose retarded its hydrolysis into glucose. Amorphous cellulose and xylans were found to contribute significantly to the released amounts of glucose and xylose, respectively.« less

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

NASA Astrophysics Data System (ADS)

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

2018-01-01

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

Propellant's differentiation using FTIR-photoacoustic detection for forensic studies of improvised explosive devices.

PubMed

Álvarez, Ángela; Yáñez, Jorge; Contreras, David; Saavedra, Renato; Sáez, Pedro; Amarasiriwardena, Dulasiri

2017-11-01

The use of propellant for making improvised explosive devices (IED) is an incipient criminal practice. Propellant can be used as initiator in explosive mixtures along with other components such as coal, ammonium nitrate, sulfur, etc. The identification of the propellant's brand used in homemade explosives can provide additional forensic information of this evidence. In this work, four of the most common propellant brands were characterized by Fourier-transform infrared photoacoustic spectroscopy (FTIR-PAS) which is a non-destructive micro-analytical technique. Spectra shows characteristic signals of typical compounds in the propellants, such as nitrocellulose, nitroglycerin, guanidine, diphenylamine, etc. The differentiation of propellant components was achieved by using FTIR-PAS combined with chemometric methods of classification. Principal component analysis (PCA) and soft independent modelling of class analogy (SIMCA) were used to achieve an effective differentiation and classification (100%) of propellant brands. Furthermore, propellant brand differentiation was also assessed using partial least squares discriminant analyses (PLS-DA) by leave one out cross (∼97%) and external (∼100%) validation method. Our results show the ability of FTIR-PAS combined with chemometric analysis to identify and differentiate propellant brands in different explosive formulations of IED. Copyright © 2017 Elsevier B.V. All rights reserved.

Exploiting external reflection FTIR spectroscopy for the in-situ identification of pigments and binders in illuminated manuscripts. Brochantite and posnjakite as a case study

NASA Astrophysics Data System (ADS)

Zaffino, Chiara; Guglielmi, Vittoria; Faraone, Silvio; Vinaccia, Alessandro; Bruni, Silvia

2015-02-01

In the present work, the use of portable instrumentation allowing in-situ reflection FTIR analyses is exploited to identify the coloring matters of northern-Italian illuminations dating to the XVI century. In order to build a database of spectra, reference paint samples were prepared spreading the pigments on parchment with two different binders, i.e. gum arabic and egg white, used in antiquity. Pigments for the database were chosen considering their use in the Middle Ages and in the Renaissance and their response in the mid- and near-IR region. The reflection FTIR spectra obtained resulted to be dominated by the specular reflection component, allowing the use of the Kramers-Kronig transform to convert them to the more conventional absorbance FTIR spectra. Several pigments could thus be identified in ancient illuminations, even if some green details showed a spectral pattern different with respect to the most common commercial green pigments of the database. Therefore, in addition, basic copper sulfates brochantite and posnjakite were synthesized and characterized. In three green details, posnjakite was identified, both as a pure compound and together with malachite.

Exploiting external reflection FTIR spectroscopy for the in-situ identification of pigments and binders in illuminated manuscripts. Brochantite and posnjakite as a case study.

PubMed

Zaffino, Chiara; Guglielmi, Vittoria; Faraone, Silvio; Vinaccia, Alessandro; Bruni, Silvia

2015-02-05

In the present work, the use of portable instrumentation allowing in-situ reflection FTIR analyses is exploited to identify the coloring matters of northern-Italian illuminations dating to the XVI century. In order to build a database of spectra, reference paint samples were prepared spreading the pigments on parchment with two different binders, i.e. gum arabic and egg white, used in antiquity. Pigments for the database were chosen considering their use in the Middle Ages and in the Renaissance and their response in the mid- and near-IR region. The reflection FTIR spectra obtained resulted to be dominated by the specular reflection component, allowing the use of the Kramers-Kronig transform to convert them to the more conventional absorbance FTIR spectra. Several pigments could thus be identified in ancient illuminations, even if some green details showed a spectral pattern different with respect to the most common commercial green pigments of the database. Therefore, in addition, basic copper sulfates brochantite and posnjakite were synthesized and characterized. In three green details, posnjakite was identified, both as a pure compound and together with malachite. Copyright © 2014 Elsevier B.V. All rights reserved.

FTIR Rotational Spectroscopy.

ERIC Educational Resources Information Center

Woods, Ron; Henderson, Giles

1987-01-01

Presented are representative examples of the spectra and the analyses for a linear molecule (HC1), a symmetric top molecule (NH3), and an asymmetric top (H2O). Any combination of these projects could be incorporated in a physical chemistry or molecular spectroscopy laboratory. (RH)

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 bioscouring performance of four polygalacturonase enzymes

USDA-ARS?s Scientific Manuscript database

Fourier Transform Infrared Attenuated Total Reflectance (FTIR-ATR) analyses of greige cotton fabrics bioscoured with a combination of ultrasound and endo- and exo-polygalacturonase enzymes obtained from Rhizopus sp. fungi were used in a fractional factorial design experiment to examine their perform...

Interlaboratory comparison of mineral constituents in a sample from the Herrin (No. 6) coal bed from Illinois

USGS Publications Warehouse

Finkelman, Robert B.; Fiene, F.L.; Miller, R.N.; Simon, F.O.

1984-01-01

Approximately 20 kg of the Herrin (No. 6) coal was collected from a strip mine in St. Clair County, Ill. A 10-kg portion was ground to -60 mesh, homogenized, and riffled into 128 splits of 70-80 g each. Homogeneity of these splits was confirmed by moisture, ash, and sulfur analyses of six randomly selected splits. Results of these analyses were within the ASTM (American Society for Testing and Materials) guidelines for interlaboratory precision. Splits of the Herrin (No. 6) coal were then transmitted to more than 30 laboratories for analysis. Low-temperature plasma oxidation was used to isolate inorganic matter for quantitative chemical and mineralogical analysis. Despite a wide variation in ashing conditions, only minor variations in ash yields were obtained; these variations were attributed to differences in operating temperature and moisture content. Mineralogical analyses of low-temperature ash (LTA) concentrates prepared by five different laboratories indicated variations within the limits of analytical error. The mean values, in weight percent, for the major minerals are as follows: calcite, 9; quartz, 20; pyrite, 23; kaolinite, 14; and illite+mixed-layer clays, 31. Normative mineralogical calculations and Fourier transform infrared analysis (FTIR) yielded results similar to those obtained from X-ray diffraction (XRD). Choosing appropriate mineral standards was found to be critical for the proper use of analytical techniques such as XRD and FTIR. Good interlaboratory agreement was obtained for most major, minor, and trace elements despite differences in analytical procedures and in the type of sample analyzed (coal, high-temperature ash, or LTA). Discrepancies between analyses for zinc, strontium, manganese, and iron may be attributed to sampling inhomogeneity problems. Mossbauer spectroscopy showed that approximately 44 percent of the pyritic sulfur was lost through weathering in the first year after preparation of the interlaboratory sample. Szomolnokite and possibly coquimbite and jarosite were also identified. Scanning electron microscopy studies indicated ubiquitous pyrite framboids and, less commonly, euhedral crystals, skeletal grains, irregularly shaped particles, and vein fillings. Minor accessory minerals such as rare-earth phosphates and possibly silicates, zircon, barium sulfate, titanium oxide, and sphalerite were also found. The textural evidence indicates that the minerals in the banded material are detrital whereas the minerals occurring as vein and pore fillings are authigenic. Magnetic measurements indicate that coal crushed in a steel pulverizer is contaminated by small quantities of abrasion fragments from the crusher, which seriously affect the measured magnetic properties of the coal.

Molecules with polymerizable ligands as precursors to porous doped materials

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

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

1996-12-31

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

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

PubMed

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

2018-05-29

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

FT-IR spectroscopic analyses of 2-(2-furanylmethylene) propanedinitrile

NASA Astrophysics Data System (ADS)

Soliman, H. S.; Eid, Kh. M.; Ali, H. A. M.; El-Mansy, M. A. M.; Atef, S. M.

2013-03-01

In the present work, a computational study for the optimized molecular structural parameters, thermo-chemical parameters, total dipole moment, HOMO-LUMO energy gap and a combined experimental and computational study for FT-IR spectra for 2-(2-furanylmethylene) propanedinitrile have been investigated using B3LYP utilizing 6-31G and 6-311G basis set. Our calculated results showed that the investigated compound possesses a dipole moment of 7.5 D and HOMO-LUMO energy gap of 3.92 eV using B3LYP/6-311G which indicates that our investigated compound is highly applicable for photovoltaic solar cell applications.

Chemical interactions in the subduction factory: New insights from an in situ trace element and hydrogen study of the Ichinomegata and Oki-Dogo mantle xenoliths (Japan)

NASA Astrophysics Data System (ADS)

Satsukawa, Takako; Godard, Marguerite; Demouchy, Sylvie; Michibayashi, Katsuyoshi; Ildefonse, Benoit

2017-07-01

The uppermost mantle in back arc regions is the site of complex interactions between partial melting, melt percolation, and fluid migration. To constrain these interactions and evaluate their consequences on geochemical cycles, we carried out an in situ trace element and water study of a suite of spinel peridotite xenoliths from two regions of the Japan back arc system, Ichinomegata (NE Japan) and Oki-Dogo (SW Japan), using LA-ICPMS and FTIR spectrometry, respectively. This study provides the first full dataset of trace element and hydrogen compositions in peridotites including analyses of all their main constitutive silicate minerals: olivine, orthopyroxene and clinopyroxene. The Ichinomegata peridotites sample a LREE-depleted refractory mantle (Mg# olivine = 0.90; Cr# spinel = 0.07-0.23; Yb clinopyroxene = 7.8-13.3 × C1-chondrite, and La/Yb clinopyroxene = 0.003-0.086 × C1-chondrite), characterized by Th-U positive anomalies and constant values of Nb/Ta. The composition of the studied Ichinomegata samples is consistent with that of an oceanic mantle lithosphere affected by cryptic metasomatic interactions with hydrous/aqueous fluids (crypto-hydrous metasomatism). In contrast, the Oki-Dogo peridotites have low Mg# olivine (0.86-0.93) and a broad range of compositions with clinopyroxene showing "spoon-shaped" to flat, and LREE-enriched patterns. They are also characterized by their homogeneous compositions in the most incompatible LILE (e.g., Rb clinopyroxene = 0.01-0.05 × primitive mantle) and HFSE (e.g., Nb clinopyroxene = 0.01-2.16 × primitive mantle). This characteristic is interpreted as resulting from various degrees of melting and extensive melt-rock interactions. FTIR spectroscopy shows that olivine in both Ichinomegata and Oki-Dogo samples has low water contents ranging from 2 to 7 ppm wt. H2O. In contrast, the water contents of pyroxenes from Ichinomegata peridotites (113-271 ppm wt. H2O for orthopyroxene, and 292-347 ppm wt. H2O for clinopyroxene) are significantly higher than in Oki-Dogo peridotites (9-35 ppm wt. H2O for orthopyroxene, and 15-98 ppm wt. H2O for clinopyroxene). This indicates a relationship between melt-rock interaction and water concentrations in pyroxenes. Our study suggests that the water content of the Japan mantle wedge is controlled by the late melt/fluid/rock interactions evidenced by trace element geochemistry: a mechanism triggered by magma-rock interactions may have acted as an efficient dehydrating process in the Oki-Dogo region while the Ichinomegata mantle water content is controlled by slab-derived crypto-hydrous metasomatism.

Tropospheric water vapour isotopologue data (H216O, H218O, and HD16O) as obtained from NDACC/FTIR solar absorption spectra

NASA Astrophysics Data System (ADS)

Barthlott, Sabine; Schneider, Matthias; Hase, Frank; Blumenstock, Thomas; Kiel, Matthäus; Dubravica, Darko; García, Omaira E.; Sepúlveda, Eliezer; Mengistu Tsidu, Gizaw; Takele Kenea, Samuel; Grutter, Michel; Plaza-Medina, Eddy F.; Stremme, Wolfgang; Strong, Kim; Weaver, Dan; Palm, Mathias; Warneke, Thorsten; Notholt, Justus; Mahieu, Emmanuel; Servais, Christian; Jones, Nicholas; Griffith, David W. T.; Smale, Dan; Robinson, John

2017-01-01

We report on the ground-based FTIR (Fourier transform infrared) tropospheric water vapour isotopologue remote sensing data that have been recently made available via the database of NDACC (Network for the Detection of Atmospheric Composition Change; ftp://ftp.cpc.ncep.noaa.gov/ndacc/MUSICA/) and via doi:10.5281/zenodo.48902. Currently, data are available for 12 globally distributed stations. They have been centrally retrieved and quality-filtered in the framework of the MUSICA project (MUlti-platform remote Sensing of Isotopologues for investigating the Cycle of Atmospheric water). We explain particularities of retrieving the water vapour isotopologue state (vertical distribution of H216O, H218O, and HD16O) and reveal the need for a new metadata template for archiving FTIR isotopologue data. We describe the format of different data components and give recommendations for correct data usage. Data are provided as two data types. The first type is best-suited for tropospheric water vapour distribution studies disregarding different isotopologues (comparison with radiosonde data, analyses of water vapour variability and trends, etc.). The second type is needed for analysing moisture pathways by means of H2O, δD-pair distributions.

Spectroscopic characterization of collagen cross-links in bone

NASA Technical Reports Server (NTRS)

Paschalis, E. P.; Verdelis, K.; Doty, S. B.; Boskey, A. L.; Mendelsohn, R.; Yamauchi, M.

2001-01-01

Collagen is the most abundant protein of the organic matrix in mineralizing tissues. One of its most critical properties is its cross-linking pattern. The intermolecular cross-linking provides the fibrillar matrices with mechanical properties such as tensile strength and viscoelasticity. In this study, Fourier transform infrared (FTIR) spectroscopy and FTIR imaging (FTIRI) analyses were performed in a series of biochemically characterized samples including purified collagen cross-linked peptides, demineralized bovine bone collagen from animals of different ages, collagen from vitamin B6-deficient chick homogenized bone and their age- and sex-matched controls, and histologically stained thin sections from normal human iliac crest biopsy specimens. One region of the FTIR spectrum of particular interest (the amide I spectral region) was resolved into its underlying components. Of these components, the relative percent area ratio of two subbands at approximately 1660 cm(-1) and approximately 1690 cm(-1) was related to collagen cross-links that are abundant in mineralized tissues (i.e., pyridinoline [Pyr] and dehydrodihydroxylysinonorleucine [deH-DHLNL]). This study shows that it is feasible to monitor Pyr and DHLNL collagen cross-links spatial distribution in mineralized tissues. The spectroscopic parameter established in this study may be used in FTIRI analyses, thus enabling the calculation of relative Pyr/DHLNL amounts in thin (approximately 5 microm) calcified tissue sections with a spatial resolution of approximately 7 microm.

[Identification of Dendrobium varieties by infrared spectroscopy].

PubMed

Liu, Fei; Wang, Yuan-Zhong; Yang, Chun-Yan; Jin, Hang

2014-11-01

The difference of Dendrobium varieties were analyzed by Fourier transform infrared (FTIR) spectroscopy. The infrared spectra of 206 stems from 30 Dendrobium varieties were obtained, and showed that polysaccharides, especially fiber, were the main components in Dendrobium plants. FTIR combined with Wilks' Lambda stepwise discriminative analysis was used to identify Dendrobium varieties. The effects of spectral range and number of training samples on the discrimination results were also analysed. Two hundred eighty seven variables in the spectral range of 1 800-1 250 cm(-1) were studied, and showed that the return discrimination is 100% correct when the training samples number of each species was 2, 3, 4, 5, and 6, respectively, whereas for the remaining samples the correct rates of identification were equal to 79.4%, 91.3%, 93.0%, 98.2%, and 100%, respectively. The same discriminative analyses on five different training samples in the spectral range of 1 800-1 500, 1 500-1 250, 1 250-600, 1 250-950 and 950-650 cm(-1) were compared, which showed that the variables in the range of 1 800-1 250, 1 800-1 500 and 950-600 cm(-1) were more suitable for variety identification, and one can obtain the satisfactory result for discriminative analysis when the training sample is more than 3. Our results indicate that FTIR combined with stepwise discriminative analysis is an effective way to distinguish different Dendrobium varieties.

The Effects of a Macromolecular Charring Agent with Gas Phase and Condense Phase Synergistic Flame Retardant Capability on the Properties of PP/IFR Composites

PubMed Central

Chen, Hongda; Wang, Jihui; Ding, Anxin; Han, Xia; Sun, Ziheng

2018-01-01

In order to improve the efficiency of intumescent flame retardants (IFRs), a novel macromolecular charring agent named poly(ethanediamine-1,3,5-triazine-p-4-amino-2,2,6,6-tetramethylpiperidine) (PETAT) with gas phase and condense phase synergistic flame-retardant capability was synthesized and subsequently dispersed into polypropylene (PP) in combination with ammonium polyphosphate (APP) via a melt blending method. The chemical structure of PETAT was investigated by Fourier transform infrared spectroscopy (FTIR), and 1H nuclear magnetic resonance (NMR) spectroscopy. Thermal properties of the PETAT and IFR systems were tested by thermogravimetric-derivative thermogravimetric analysis (TGA-DTG) and thermogravimetry–Fourier transform infrared spectroscopy (TG-FTIR). The mechanical properties, thermal stability, flame-retardant properties, water resistance, and structures of char residue in flame-retardant composites were characterized using tensile and flexural strength property tests, TGA, limiting oxygen index (LOI) values before and after soaking, underwritten laboratory-94 (UL-94) vertical burning test, cone calorimetric test (CCT), scanning electron microscopy with energy dispersive X-ray spectrometry (SEM-EDXS), and FTIR. The results indicated that PETAT was successfully synthesized, and when the ratio of APP to PETAT was 2:1 with 25 wt % loading, the novel IFR system could reduce the deterioration of tensile strength and enhance the flexural strength of composites. Meanwhile, the flame-retardant composite was able to pass the UL-94 V-0 rating with an LOI value of 30.3%, and the peak of heat release rate (PHRR), total heat release (THR), and material fire hazard values were considerably decreased compared with others. In addition, composites also exhibited excellent water resistance properties compared with traditional IFR composites. SEM-EDXS and FTIR analyses of the char residues, as well as TG-FTIR analyses of IFR were used to investigate the flame-retardant mechanism of the APP/PETAT IFR system. The results indicated that the efficient flame retardancy of PP/IFR composites could be attributed to the synergism of the free radical-quenching and char layer-protecting mechanisms in the gas phase and condense phase, respectively. PMID:29324716

The Effects of a Macromolecular Charring Agent with Gas Phase and Condense Phase Synergistic Flame Retardant Capability on the Properties of PP/IFR Composites.

PubMed

Chen, Hongda; Wang, Jihui; Ni, Aiqing; Ding, Anxin; Han, Xia; Sun, Ziheng

2018-01-11

In order to improve the efficiency of intumescent flame retardants (IFRs), a novel macromolecular charring agent named poly(ethanediamine-1,3,5-triazine-p-4-amino-2,2,6,6-tetramethylpiperidine) (PETAT) with gas phase and condense phase synergistic flame-retardant capability was synthesized and subsequently dispersed into polypropylene (PP) in combination with ammonium polyphosphate (APP) via a melt blending method. The chemical structure of PETAT was investigated by Fourier transform infrared spectroscopy (FTIR), and ¹H nuclear magnetic resonance (NMR) spectroscopy. Thermal properties of the PETAT and IFR systems were tested by thermogravimetric-derivative thermogravimetric analysis (TGA-DTG) and thermogravimetry-Fourier transform infrared spectroscopy (TG-FTIR). The mechanical properties, thermal stability, flame-retardant properties, water resistance, and structures of char residue in flame-retardant composites were characterized using tensile and flexural strength property tests, TGA, limiting oxygen index (LOI) values before and after soaking, underwritten laboratory-94 (UL-94) vertical burning test, cone calorimetric test (CCT), scanning electron microscopy with energy dispersive X-ray spectrometry (SEM-EDXS), and FTIR. The results indicated that PETAT was successfully synthesized, and when the ratio of APP to PETAT was 2:1 with 25 wt % loading, the novel IFR system could reduce the deterioration of tensile strength and enhance the flexural strength of composites. Meanwhile, the flame-retardant composite was able to pass the UL-94 V-0 rating with an LOI value of 30.3%, and the peak of heat release rate (PHRR), total heat release (THR), and material fire hazard values were considerably decreased compared with others. In addition, composites also exhibited excellent water resistance properties compared with traditional IFR composites. SEM-EDXS and FTIR analyses of the char residues, as well as TG-FTIR analyses of IFR were used to investigate the flame-retardant mechanism of the APP/PETAT IFR system. The results indicated that the efficient flame retardancy of PP/IFR composites could be attributed to the synergism of the free radical-quenching and char layer-protecting mechanisms in the gas phase and condense phase, respectively.

Enhancing forensic science with spectroscopic imaging

NASA Astrophysics Data System (ADS)

Ricci, Camilla; Kazarian, Sergei G.

2006-09-01

This presentation outlines the research we are developing in the area of Fourier Transform Infrared (FTIR) spectroscopic imaging with the focus on materials of forensic interest. FTIR spectroscopic imaging has recently emerged as a powerful tool for characterisation of heterogeneous materials. FTIR imaging relies on the ability of the military-developed infrared array detector to simultaneously measure spectra from thousands of different locations in a sample. Recently developed application of FTIR imaging using an ATR (Attenuated Total Reflection) mode has demonstrated the ability of this method to achieve spatial resolution beyond the diffraction limit of infrared light in air. Chemical visualisation with enhanced spatial resolution in micro-ATR mode broadens the range of materials studied with FTIR imaging with applications to pharmaceutical formulations or biological samples. Macro-ATR imaging has also been developed for chemical imaging analysis of large surface area samples and was applied to analyse the surface of human skin (e.g. finger), counterfeit tablets, textile materials (clothing), etc. This approach demonstrated the ability of this imaging method to detect trace materials attached to the surface of the skin. This may also prove as a valuable tool in detection of traces of explosives left or trapped on the surfaces of different materials. This FTIR imaging method is substantially superior to many of the other imaging methods due to inherent chemical specificity of infrared spectroscopy and fast acquisition times of this technique. Our preliminary data demonstrated that this methodology will provide the means to non-destructive detection method that could relate evidence to its source. This will be important in a wider crime prevention programme. In summary, intrinsic chemical specificity and enhanced visualising capability of FTIR spectroscopic imaging open a window of opportunities for counter-terrorism and crime-fighting, with applications ranging from analysis of trace evidence (e.g. in soil), tablets, drugs, fibres, tape explosives, biological samples to detection of gunshot residues and imaging of fingerprints.

Improving FTIR imaging speciation of organic compound residues or their degradation products in wall painting samples, by introducing a new thin section preparation strategy based on cyclododecane pre-treatment.

PubMed

Papliaka, Zoi Eirini; Vaccari, Lisa; Zanini, Franco; Sotiropoulou, Sophia

2015-07-01

Fourier transform infrared (FTIR) imaging in transmission mode, employing a bidimensional focal plane array (FPA) detector, was applied for the detection and spatially resolved chemical characterisation of organic compounds or their degradation products within the stratigraphy of a critical group of fragments, originating from prehistoric and roman wall paintings, containing a very low concentration of subsisted organic matter or its alteration products. Past analyses using attenuated total reflection (ATR) or reflection FTIR on polished cross sections failed to provide any evidence of any organic material assignable as binding medium of the original painting. In order to improve the method's performance, in the present study, a new method of sample preparation in thin section was developed. The procedure is based on the use of cyclododecane C12H24 as embedding material and a subsequent double-side polishing of the specimen. Such procedure provides samples to be studied in FTIR transmission mode without losing the information on the spatial distribution of the detected materials in the paint stratigraphy. For comparison purposes, the same samples were also studied after opening their stratigraphy with a diamond anvil cell. Both preparation techniques offered high-quality chemical imaging of the decay products of an organic substance, giving clues to the painting technique. In addition, the thin sections resulting from the cyclododecane pre-treatment offered more layer-specific data, as the layer thickness and order remained unaffected, whereas the samples resulting from compression within the diamond cell were slightly deformed; however, since thinner and more homogenous, they provided higher spectral quality in terms of S/N ratio. In summary, the present study illustrates the appropriateness of FTIR imaging in transmission mode associated with a new thin section preparation strategy to detect and localise very low-concentrated organic matter subjected to deterioration processes, when the application of FTIR in reflection mode or FTIR-ATR fails to give any relevant information.

Identification and differentiation of food-related bacteria: A comparison of FTIR spectroscopy and MALDI-TOF mass spectrometry.

PubMed

Wenning, Mareike; Breitenwieser, Franziska; Konrad, Regina; Huber, Ingrid; Busch, Ulrich; Scherer, Siegfried

2014-08-01

The food industry requires easy, accurate, and cost-effective techniques for microbial identification to ensure safe products and identify microbial contaminations. In this work, FTIR spectroscopy and MALDI-TOF mass spectrometry were assessed for their suitability and applicability for routine microbial diagnostics of food-related microorganisms by analyzing their robustness according to changes in incubation time and medium, identification accuracy and their ability to differentiate isolates down to the strain level. Changes in the protocol lead to a significantly impaired performance of FTIR spectroscopy, whereas they had only little effects on MALDI-TOF MS. Identification accuracy was tested using 174 food-related bacteria (93 species) from an in-house strain collection and 40 fresh isolates from routine food analyses. For MALDI-TOF MS, weaknesses in the identification of bacilli and pseudomonads were observed; FTIR spectroscopy had most difficulties in identifying pseudomonads and enterobacteria. In general, MALDI-TOF MS obtained better results (52-85% correct at species level), since the analysis of mainly ribosomal proteins is more robust and seems to be more reliable. FTIR spectroscopy suffers from the fact that it generates a whole-cell fingerprint and intraspecies diversity may lead to overlapping species borders which complicates identification. In the present study values between 56% and 67% correct species identification were obtained. On the opposite, this high sensitivity offers the opportunity of typing below the species level which was not possible using MALDI-TOF MS. Using fresh isolates from routine diagnostics, both techniques performed well with 88% (MALDI-TOF) and 75% (FTIR) correct identifications at species level, respectively. Copyright © 2014 Elsevier B.V. All rights reserved.

Rapid investigation of α-glucosidase inhibitory activity of Phaleria macrocarpa extracts using FTIR-ATR based fingerprinting.

PubMed

Easmin, Sabina; Sarker, Md Zaidul Islam; Ghafoor, Kashif; Ferdosh, Sahena; Jaffri, Juliana; Ali, Md Eaqub; Mirhosseini, Hamed; Al-Juhaimi, Fahad Y; Perumal, Vikneswari; Khatib, Alfi

2017-04-01

Phaleria macrocarpa, known as "Mahkota Dewa", is a widely used medicinal plant in Malaysia. This study focused on the characterization of α-glucosidase inhibitory activity of P. macrocarpa extracts using Fourier transform infrared spectroscopy (FTIR)-based metabolomics. P. macrocarpa and its extracts contain thousands of compounds having synergistic effect. Generally, their variability exists, and there are many active components in meager amounts. Thus, the conventional measurement methods of a single component for the quality control are time consuming, laborious, expensive, and unreliable. It is of great interest to develop a rapid prediction method for herbal quality control to investigate the α-glucosidase inhibitory activity of P. macrocarpa by multicomponent analyses. In this study, a rapid and simple analytical method was developed using FTIR spectroscopy-based fingerprinting. A total of 36 extracts of different ethanol concentrations were prepared and tested on inhibitory potential and fingerprinted using FTIR spectroscopy, coupled with chemometrics of orthogonal partial least square (OPLS) at the 4000-400 cm -1 frequency region and resolution of 4 cm -1 . The OPLS model generated the highest regression coefficient with R 2 Y = 0.98 and Q 2 Y = 0.70, lowest root mean square error estimation = 17.17, and root mean square error of cross validation = 57.29. A five-component (1+4+0) predictive model was build up to correlate FTIR spectra with activity, and the responsible functional groups, such as -CH, -NH, -COOH, and -OH, were identified for the bioactivity. A successful multivariate model was constructed using FTIR-attenuated total reflection as a simple and rapid technique to predict the inhibitory activity. Copyright © 2016. Published by Elsevier B.V.

Water Retention and Rheology of Ti-doped, Synthetic Olivine

NASA Astrophysics Data System (ADS)

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

2012-12-01

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

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

Zhang Hui; Zou Kang; Guo Shaohuan

A nanostructural drug-inorganic clay composite involving a pharmaceutically active compound captopril (Cpl) intercalated Mg-Al-layered double hydroxides (Cpl-LDHs) with Mg/Al molar ratio of 2.06 has been assembled by coprecipitation method. Powder X-ray diffraction (XRD), Fourier transform infrared spectra (FT-IR) and Raman spectra analysis indicate a successful intercalation of Cpl between the layers with a vertical orientation of Cpl disulphide-containing S-S linkage. SEM photo indicates that as-synthesized Cpl-LDHs possess compact and non-porous structure with approximately and linked elliptical shape particles of ca. 50 nm. TG-DTA analyses suggest that the thermal stability of intercalated organic species is largely enhanced due to host-guest interactionmore » involving the hydrogen bond compared to pure form before intercalation. The in vitro release studies show that both the release rate and release percentages markedly decrease with increasing pH from 4.60 to 7.45 due to possible change of release mechanism during the release process. The kinetic simulation for the release data, and XRD and FT-IR analyses for samples recovered from release media indicate that the dissolution mechanism is mainly responsible for the release behaviour of Cpl-LDHs at pH 4.60, while the ion-exchange one is responsible for that at pH 7.45. - Graphical abstract: Based on XRD, FT-IR and Raman spectra analyses, it is suggested that captopril (Cpl) exists as its disulphide metabolites in the interlayer of Mg-Al-LDHs via hydrogen bonding between guest carboxylate function and hydroxyl group of the host layers. A schematic supramolecular structure of Cpl intercalates involving a vertical orientation of Cpl disulphide-containing S-S bond between the layers with carboxylate anions pointing to both hydroxide layers is presented.« less

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

PubMed

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

2018-01-01

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

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

PubMed

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

2018-08-15

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

A Portable FTIR Analyser for Field Measurements of Trace Gases and their Isotopologues: CO2, CH4, N2O, CO, del13C in CO2 and delD in water vapour

NASA Astrophysics Data System (ADS)

Griffith, D. W.; Bryant, G. R.; Deutscher, N. M.; Wilson, S. R.; Kettlewell, G.; Riggenbach, M.

2007-12-01

We describe a portable Fourier Transform InfraRed (FTIR) analyser capable of simultaneous high precision analysis of CO2, CH4, N2O and CO in air, as well as δ13C in CO2 and δD in water vapour. The instrument is based on a commercial 1 cm-1 resolution FTIR spectrometer fitted with a mid-IR globar source, 26 m multipass White cell and thermoelectrically-cooled MCT detector operating between 2000 and 7500 cm-1. Air is passed through the cell and analysed in real time without any pre-treatment except for (optional) drying. An inlet selection manifold allows automated sequential analysis of samples from one or more inlet lines, with typical measurement times of 1-10 minutes per sample. The spectrometer, inlet sampling sequence, real-time quantitative spectrum analysis, data logging and display are all under the control of a single program running on a laptop PC, and can be left unattended for continuous measurements over periods of weeks to months. Selected spectral regions of typically 100-200 cm-1 width are analysed by a least squares fitting technique to retrieve concentrations of trace gases, 13CO2 and HDO. Typical precision is better than 0.1% without the need for calibration gases. Accuracy is similar if measurements are referenced to calibration standard gases. δ13C precision is typically around 0.1‰, and for δD it is 1‰. Applications of the analyser include clean and polluted air monitoring, tower-based flux measurements such as flux gradient or integrated horizontal flux measurements, automated soil chambers, and field-based measurements of isotopic fractionation in soil-plant-atmosphere systems. The simultaneous multi-component advantages can be exploited in tracer-type emission measurements, for example of CH4 from livestock using a co-released tracer gas and downwind measurement. We have also developed an open path variant especially suited to tracer release studies and measurements of NH3 emissions from agricultural sources. An illustrative selection of applications will be presented.

Solution chemistry of carbonate minerals and its effects on the flotation of hematite with sodium oleate

NASA Astrophysics Data System (ADS)

Li, Dong; Yin, Wan-zhong; Xue, Ji-wei; Yao, Jin; Fu, Ya-feng; Liu, Qi

2017-07-01

The effects of carbonate minerals (dolomite and siderite) on the flotation of hematite using sodium oleate as a collector were investigated through flotation tests, supplemented by dissolution measurements, solution chemistry calculations, zeta-potential measurements, Fourier transform infrared (FTIR) spectroscopic studies, and X-ray photoelectron spectroscopy (XPS) analyses. The results of flotation tests show that the presence of siderite or dolomite reduced the recovery of hematite and that the inhibiting effects of dolomite were stronger. Dissolution measurements, solution chemistry calculations, and flotation tests confirmed that both the cations (Ca2+ and Mg2+) and CO3 2- ions dissolved from dolomite depressed hematite flotation, whereas only the CO3 2- ions dissolved from siderite were responsible for hematite depression. The zeta-potential, FTIR spectroscopic, and XPS analyses indicated that Ca2+, Mg2+, and CO3 2- (HCO3 -) could adsorb onto the hematite surface, thereby hindering the adsorption of sodium oleate, which was the main reason for the inhibiting effects of carbonate minerals on hematite flotation.

Characterization of lignin during oxidative and hydrothermal pre-treatment processes of wheat straw and corn stover.

PubMed

Kaparaju, Prasad; Felby, Claus

2010-05-01

The objective of the study was to characterize and map changes in lignin during hydrothermal and wet explosion pre-treatments of wheat straw and corn stover. Chemical composition, microscopic (atomic force microscopy and scanning electron microscopy) and spectroscopic (attenuated total reflectance Fourier transform infrared spectroscopy, ATR-FTIR) analyses were performed. Results showed that both pre-treatments improved the cellulose and lignin content with substantial removal of hemicellulose in the pre-treated biomasses. These values were slightly higher for hydrothermal compared to wet explosion pre-treatment. ATR-FTIR analyses also confirmed these results. Microscopic analysis showed that pre-treatments affected the biomass by partial difibration. Lignin deposition on the surface of the hydrothermally pre-treated fibre was very distinct while severe loss of fibril integrity was noticed with wet exploded fibre. The present study thus revealed that the lignin cannot be removed by the studied pre-treatments. However, both pre-treatments improved the accessibility of the biomass towards enzymatic hydrolysis. Copyright 2009 Elsevier Ltd. All rights reserved.

Multiple fingerprinting analyses in quality control of Cassiae Semen polysaccharides.

PubMed

Cheng, Jing; He, Siyu; Wan, Qiang; Jing, Pu

2018-03-01

Quality control issue overshadows potential health benefits of Cassiae Semen due to the analytic limitations. In this study, multiple-fingerprint analysis integrated with several chemometrics was performed to assess the polysaccharide quality of Cassiae Semen harvested from different locations. FT-IR, HPLC, and GC fingerprints of polysaccharide extracts from the authentic source were established as standard profiles, applying to assess the quality of foreign sources. Analyses of FT-IR fingerprints of polysaccharide extracts using either Pearson correlation analysis or principal component analysis (PCA), or HPLC fingerprints of partially hydrolyzed polysaccharides with PCA, distinguished the foreign sources from the authentic source. However, HPLC or GC fingerprints of completely hydrolyzed polysaccharides couldn't identify all foreign sources and the methodology using GC is quite limited in determining the monosaccharide composition. This indicates that FT-IR/HPLC fingerprints of non/partially-hydrolyzed polysaccharides, respectively, accompanied by multiple chemometrics methods, might be potentially applied in detecting and differentiating sources of Cassiae Semen. Copyright © 2018 Elsevier B.V. All rights reserved.

The analysis of scalp irritation by coacervates produced in hair shampoo via FTIR with focal plane array detector, X-ray photoelectron microscopy and HaCaT cells.

PubMed

Jung, I K; Park, S C; Kim, S H; Kim, J H; Cha, N R; Bae, W R; Kim, H N; Cho, S A; Yoo, J W; Kim, B M; Lee, J H

2017-04-01

Coacervates are inevitably formed on scalp on using hair washing products. Our goal was to analyse the coacervates in detail to identify the part responsible for scalp stimulation. Shampoo that increases coacervate formation was applied to in vitro skin and was washed. The residue was then analysed using Fourier transform infrared spectroscopy-focal plane array (FTIR-FPA) and X-ray photoelectron microscopy (XPS). And HaCaT cells were used for irritant test of coacervate. Through this research, it was confirmed that the coacervate was a macromolecule structurally similar to a cationic polymer and contains an anionic surfactant. Its anionic surfactant was structurally semi-stable so that it released onto scalp when it absorbs moisture. Coacervate releases sulphate bonding into the matrix when it is exposed to water. Thus, the scalp stimulation would be expected. © 2016 Society of Cosmetic Scientists and the Société Française de Cosmétologie.

Primidone--an antiepileptic drug--characterisation by quantum chemical and spectroscopic (FTIR, FT-Raman, 1H, 13C NMR and UV-Visible) investigations.

PubMed

Arjunan, V; Santhanam, R; Subramanian, S; Mohan, S

2013-05-15

The solid phase FTIR and FT-Raman spectra of primidone were recorded in the regions 4000-400 cm(-1) and 4000-100 cm(-1), respectively. The vibrational spectra were analysed and the observed fundamentals were assigned and analysed. The experimental wavenumbers were compared with the theoretical scaled vibrational wavenumbers determined by DFT methods. The Raman intensities were also determined with B3LYP/6-31G(d,p) method. The total electron density and molecular electrostatic potential surface of the molecule were constructed by using B3LYP/6-311++G(d,p) method to display electrostatic potential (electron+nuclei) distribution. The HOMO and LUMO energies were measured. Natural bond orbital analysis of primidone has been performed to indicate the presence of intramolecular charge transfer. The (1)H and (13)C NMR spectra were recorded and the chemical shifts of the molecule were calculated. Copyright © 2013 Elsevier B.V. All rights reserved.

Rapid Biosynthesis of AgNPs Using Soil Bacterium Azotobacter vinelandii With Promising Antioxidant and Antibacterial Activities for Biomedical Applications

NASA Astrophysics Data System (ADS)

Karunakaran, Gopalu; Jagathambal, Matheswaran; Gusev, Alexander; Torres, Juan Antonio Lopez; Kolesnikov, Evgeny; Kuznetsov, Denis

2017-07-01

Silver nanoparticles (AgNPs) are applied in various fields from electronics to biomedical applications as a result of their high surface-to-volume ratio. Even though different approaches are available for synthesis of AgNPs, a nontoxic method for the synthesis has not yet been developed. Thus, this study focused on developing an easy and ecofriendly approach to synthesize AgNPs using Azotobacter vinelandii culture extracts. The biosynthesized nanoparticles were further characterized by ultraviolet-visible (UV-Vis) spectroscopy, x-ray diffraction (XRD), Fourier transform infrared (FTIR), energy-dispersive spectrum, particle size distribution (PSD), and transmission electron microscopy (TEM). UV absorption noticed at 435 nm showed formation of AgNPs. The XRD pattern showed a face-centered cubic structure with broad peaks of 28.2°, 32.6°, 46.6°, 55.2°, 57.9°, and 67.8°. The FTIR confirmed the involvement of various functional groups in the biosynthesis of AgNPs. The PSD and TEM analyses showed spherical, well-distributed nanoparticles with an average size of 20-70 nm. The elemental studies confirmed the existence of pure AgNPs. The bacterial extract containing extracellular enzyme nitrate reductase converted silver nitrate into AgNPs. AgNPs significantly inhibited the growth of pathogenic bacteria such as Streptomyces fradiae (National Collection of Industrial Microorganisms (NCIM) 2419), Staphylococcus aureus (NCIM 2127), Escherichia coli (NCIM 2065), and Serratia marcescens (NCIM 2919). In addition, biosynthesized AgNPs were found to possess strong antioxidant activity. Thus, the results of this study revealed that biosynthesized AgNPs could serve as a lead in the development of nanomedicine.

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

NASA Astrophysics Data System (ADS)

Singh, Ravindra Kumar; Singh, Ashok Kumar

2017-02-01

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

Black painted pottery, Kildehuse II, Odense County, Denmark.

PubMed

Trąbska, Joanna; Wesełucha-Birczyńska, Aleksandra; Zięba-Palus, Janina; Runge, Mads Thagård

2011-08-15

This work aimed at characterization of a black layer covering a Bronze Age (period VI) pot surface. To solve research problems plane polarized light microscopy (PLM), scanning microscopy with X-ray microanalyser (SEM/EDS), Raman and FTIR microspectroscopies were applied. Observation of the black layer under the PLM suggests that we deal with an opaque, isotropic layer, purposely put on leather-hard, burnished surface of a pot. No traces of organic substances that might have modified a pot surface before painting were detected. The black layer coats the pot with a continuous 0.2-0.4 μm thick layer. The black layer must have been applied while warm or hot. It is recognized that the black layer is a true painting layer. Spectroscopic analyses (Raman and FTIR) point that birch tar or a birch-pine tar had been applied. Carbon black should be definitely excluded. The analyzed organic substance is structurally ordered in various degrees, due to varying temperature influence. Some Raman spectra reveal, in second-order region of the spectrum (>2000 cm(-1)), the graphite presence. Scarce points reveal the presence of inorganic admixtures: clay minerals, feldspars and quartz. The next question is: Is it an organic paint or a carbon-based, "mixed" paint? Inorganic admixtures are only casual. Relatively high concentration of alumina is expected to have appeared due to aluminum mobility in acidic environment and this was provided by organic tar/pitch substances. Phosphorus (usually with calcium) mostly concentrates together with clay minerals. Thus, hypothesis on bone powder or ash addition to tar/pitch should be excluded. Some elements may originate not only from inorganic substances but also from wood ashes. Copyright © 2010 Elsevier B.V. All rights reserved.

Black painted pottery, Kildehuse II, Odense County, Denmark

NASA Astrophysics Data System (ADS)

Trąbska, Joanna; Wesełucha-Birczyńska, Aleksandra; Zięba-Palus, Janina; Runge, Mads Thagård

2011-08-01

This work aimed at characterization of a black layer covering a Bronze Age (period VI) pot surface. To solve research problems plane polarized light microscopy (PLM), scanning microscopy with X-ray microanalyser (SEM/EDS), Raman and FTIR microspectroscopies were applied. Observation of the black layer under the PLM suggests that we deal with an opaque, isotropic layer, purposely put on leather-hard, burnished surface of a pot. No traces of organic substances that might have modified a pot surface before painting were detected. The black layer coats the pot with a continuous 0.2-0.4 μm thick layer. The black layer must have been applied while warm or hot. It is recognized that the black layer is a true painting layer. Spectroscopic analyses (Raman and FTIR) point that birch tar or a birch-pine tar had been applied. Carbon black should be definitely excluded. The analyzed organic substance is structurally ordered in various degrees, due to varying temperature influence. Some Raman spectra reveal, in second-order region of the spectrum (>2000 cm -1), the graphite presence. Scarce points reveal the presence of inorganic admixtures: clay minerals, feldspars and quartz. The next question is: Is it an organic paint or a carbon-based, "mixed" paint? Inorganic admixtures are only casual. Relatively high concentration of alumina is expected to have appeared due to aluminum mobility in acidic environment and this was provided by organic tar/pitch substances. Phosphorus (usually with calcium) mostly concentrates together with clay minerals. Thus, hypothesis on bone powder or ash addition to tar/pitch should be excluded. Some elements may originate not only from inorganic substances but also from wood ashes.

Dynamic Multivariate Accelerated Corrosion Test Protocol

DTIC Science & Technology

2014-10-01

atmospheric, accelerated, AA2024-T3, AA6061-T6, AA7075-T3, 1010 steel, AgCl, rare earth conversion coat, magnesium rich primer, polyurethane , Eyring, Monte...morphology and elemental analysis by scanning electron microscopy-energy dispersive spectroscopy (SEM-EDS) and electrochemical determinations of...in the FT-IR analysis; degradation of the components of the high performance polyurethane coatings exposed in the UV/ozone chamber were more

In-situ ATR-FTIR and surface complexation modeling studies on the adsorption of dimethylarsenic acid and p-arsanilic acid on iron-(oxyhydr)oxides

USDA-ARS?s Scientific Manuscript database

Arsenic is an element that exists naturally in many rocks and minerals around the world. It also accumulates in petroleum, shale, oil sands and coal deposits as a result of biogeochemical processes, and it has been found in fly ash from the combustion of solid biofuels. Arsenic compounds in their o...

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.

Surveillance system for air pollutants by combination of the decision support system COMPAS and optical remote sensing systems

NASA Astrophysics Data System (ADS)

Flassak, Thomas; de Witt, Helmut; Hahnfeld, Peter; Knaup, Andreas; Kramer, Lothar

1995-09-01

COMPAS is a decision support system designed to assist in the assessment of the consequences of accidental releases of toxic and flammable substances. One of the key elements of COMPAS is a feedback algorithm which allows us to calculate the source term with the aid of concentration measurements. Up to now the feedback technique is applied to concentration measurements done with test tubes or conventional point sensors. In this paper the extension of the actual method is presented which is the combination of COMPAS and an optical remote sensing system like the KAYSER-THREDE K300 FTIR system. Active remote sensing methods based on FTIR are, among other applications, ideal for the so-called fence line monitoring of the diffuse emissions and accidental releases from industrial facilities, since from the FTIR spectra averaged concentration levels along the measurement path can be achieved. The line-averaged concentrations are ideally suited as on-line input for COMPAS' feedback technique. Uncertainties in the assessment of the source term related with both shortcomings of the dispersion model itself and also problems of a feedback strategy based on point measurements are reduced.

Label-Free Determination of Protein Binding in Aqueous Solution using Overlayer Enhanced Attenuated Total Reflectance Fourier Transform Infrared Spectroscopy (OE-ATR-FTIR)

NASA Astrophysics Data System (ADS)

Ruthenburg, Travis; Aweda, Tolulope; Park, Simon; Meares, Claude; Land, Donald

2009-03-01

Protein binding/affinity studies are often performed using Surface Plasmon Resonance techniques that don't produce much spectral information. Measurement of protein binding affinity using FTIR is traditionally performed using high protein concentration or deuterated solvent. By immobilizing a protein near the surface of a gold-coated germanium internal reflection element interactions can be measured between an immobilized protein and free proteins or small molecules in aqueous solution. By monitoring the on and off rates of these interactions, the dissociation constant for the system can be determined. The dissociation constant for the molecule Yttrium-DOTA binding to the antibody 2D12.5 system was determined to be 100nM. Results will also be presented from our measurements of Bovine Serum Albumin (BSA) binding to anti-BSA.

Characterization of cellulosic wastes and gasification products from chicken farms

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

Joseph, Paul, E-mail: p.joseph@ulster.ac.uk; Tretsiakova-McNally, Svetlana; McKenna, Siobhan

Highlights: Black-Right-Pointing-Pointer The gas chromatography indicated the variable quality of the producer gas. Black-Right-Pointing-Pointer The char had appreciable NPK values, and can be used as a fertiliser. Black-Right-Pointing-Pointer The bio-oil produced was of poor quality, having high moisture content and low pH. Black-Right-Pointing-Pointer Mass and energy balances showed inadequate level energy recovery from the process. Black-Right-Pointing-Pointer Future work includes changing the operating parameters of the gasification unit. - Abstract: The current article focuses on gasification as a primary disposal solution for cellulosic wastes derived from chicken farms, and the possibility to recover energy from this process. Wood shavings and chickenmore » litter were characterized with a view to establishing their thermal parameters, compositional natures and calorific values. The main products obtained from the gasification of chicken litter, namely, producer gas, bio-oil and char, were also analysed in order to establish their potential as energy sources. The experimental protocol included bomb calorimetry, pyrolysis combustion flow calorimetry (PCFC), thermo-gravimetric analyses (TGA), differential scanning calorimetry (DSC), Fourier transform infrared (FT-IR) spectroscopy, Raman spectroscopy, elemental analyses, X-ray diffraction (XRD), mineral content analyses and gas chromatography. The mass and energy balances of the gasification unit were also estimated. The results obtained confirmed that gasification is a viable method of chicken litter disposal. In addition to this, it is also possible to recover some energy from the process. However, energy content in the gas-phase was relatively low. This might be due to the low energy efficiency (19.6%) of the gasification unit, which could be improved by changing the operation parameters.« less

Calcium-rich biochar from the pyrolysis of crab shell for phosphorus removal.

PubMed

Dai, Lichun; Tan, Furong; Li, Hong; Zhu, Nengmin; He, Mingxiong; Zhu, Qili; Hu, Guoquan; Wang, Li; Zhao, Jie

2017-08-01

Calcium-rich biochars (CRB) prepared through pyrolysis of crab shell at various temperatures were characterized for physicochemical properties and P removal potential. Elemental analysis showed that CRB was rich in calcium (22.91%-36.14%), while poor in carbon (25.21%-9.08%). FTIR, XRD and TG analyses showed that calcite-based CRB was prepared at temperature ≤600 °C, while lime-based CRB was prepared at temperature ≥700 °C. Phosphorus removal experiment showed that P removal efficiencies in 80 mg P/L phosphate solution and biogas effluent ranged from 26% to 11%, respectively, to about 100% and 63%, respectively, depending on the pyrolysis temperature of the resulting biochar. Specifically, compared to common used CaCO 3 and Ca(OH) 2 , P removal potential of calcite-based CRB was much higher than that of CaCO 3 ; while that of lime-based CRB was close to that of Ca(OH) 2 . These results suggested that CRB was competent for P removal/recovery from wastewater. Copyright © 2017 Elsevier Ltd. All rights reserved.

Structural, spectral, DFT and biological studies on macrocyclic mononuclear ruthenium (II) complexes

NASA Astrophysics Data System (ADS)

Muthukkumar, M.; Kamal, C.; Venkatesh, G.; Kaya, C.; Kaya, S.; Enoch, Israel V. M. V.; Vennila, P.; Rajavel, R.

2017-11-01

Macrocyclic mononuclear ruthenium (II) complexes have been synthesized by condensation method [Ru (L1, L2, L3) Cl2] L1 = (C36 H31 N9), L2= (C42H36N8), L3= (C32H32 N8)]. These ruthenium complexes have been established by elemental analyses and spectroscopic techniques (Fourier transform infrared spectroscopy (FT-IR), 1H- nuclear magnetic resonance (NMR), 13C- NMR and Electrospray ionization mass spectrometry (ESI-MS)). The coordination mode of the ligand has been confirmed and the octahedral geometry around the ruthenium ion has been revealed. Binding affinity and binding mode of ruthenium (II) complexes with Bovine serum Albumin (BSA) have been characterized by Emission spectra analysis. UV-Visible and fluorescence spectroscopic techniques have also been utilized to examine the interaction between ligand and its complexes L1, L2, & L3 with BSA. Chemical parameters and molecular structure of Ru (II) complexes L1H, L2H, & L3H have been determined by DFT coupled with B3LYP/6-311G** functional in both the gaseous and aqueous phases.

Thiolated citrus low-methoxyl pectin: Synthesis, characterization and rheological and oxidation-responsive gelling properties.

PubMed

Chen, Jinfeng; Ye, Fayin; Zhou, Yun; Zhao, Guohua

2018-02-01

In the present study, citrus low-methoxyl pectin was modified by conjugating cysteine via amide bonds, and the resultant polymer (CYS-PEC) was characterized. CYS-PEC conjugates with thiol contents varying from 77.8μmol/g to 296μmol/g were synthesized, and the successful conjugation was evidenced by elemental, and FT-IR analyses. The sulfur in CYS-PEC is predominately in the thiol form, with a minor fraction forming disulfide bonds (∼15%), which occur when thiol/disulfide interchange interrupts the intended thiolation. Both native and modified pectin dispersions exhibited strong pseudoplastic properties, and the frequency sweeps revealed them to be dispersions containing microgel particles. Dynamic viscoelastic analysis was used to determine the oxidation-response gelling capacities of polymer dispersions containing H 2 O 2 , especially those that are highly thiolated and have cross-linked gel properties. For oxidation-induced CYS-PEC gels, their gelation time, hardness, viscosity and elastic moduli and swelling-disintegration ratio are dependent on the thiol group content, H 2 O 2 concentration and polymer concentration. Copyright © 2017 Elsevier Ltd. All rights reserved.

Nano-sized, quaternary titanium(IV) metal-organic frameworks with multidentate ligands.

PubMed

Baranwal, Balram Prasad; Singh, Alok Kumar

2010-12-01

Some mononuclear nano-sized, quaternary titanium(IV) complexes having the general formula [Ti(acac)(OOCR)2(SB)] (where Hacac=acetylacetone, R=C15H31 or C17H35, HSB=Schiff bases) have been synthesized using different multidentate ligands. These were characterized by elemental analyses, molecular weight determinations and spectral (FTIR, 1H NMR and powder XRD) studies. Conductance measurement indicated their non-conducting nature which may behave like insulators. Structural parameters like the values of limiting indices h, k, l, cell constants a, b, c, angles α, β, γ and particle size are calculated from powder XRD data for complex 1 which indicated nano-sized triclinic system in them. Bidentate chelating nature of acetylacetone, carboxylate and Schiff base anions in the complexes was established by their infrared spectra. Molecular weight determinations confirmed mononuclear nature of the complexes. On the basis of physico-chemical studies, coordination number 8 was assigned for titanium(IV) in the complexes. Transmission electron microscopy (TEM) and the selected area electron diffraction (SAED) studies indicated spherical particles with poor crystallinity. Copyright © 2010 Elsevier B.V. All rights reserved.

Synthesis, spectroscopic, thermal and structural properties of 4-(2-aminoethyl)pyridinium tetracyanometallate(II) complexes

NASA Astrophysics Data System (ADS)

Karaağaç, Dursun; Kürkçüoğlu, Güneş Süheyla; Şenyel, Mustafa; Şahin, Onur

2017-05-01

In this study, three new complexes (4aepyH)2[Ni(CN)4] (1), (4aepyH)2[Pd(CN)4] (2) and (4aepyH)2[Pt(CN)4] (3) [4aepy = 4-(2-aminoethyl)pyridine] have been synthesized and characterized by elemental, thermal, vibrational (FT-IR and Raman) and single-crystal X-ray diffraction techniques. The crystallographic analyses reveal that the complexes crystallize in the monoclinic system, space group C2/c. The asymmetric units of the complexes contain one M(II) ion, two cyanide ligands and one non-coordinated the 4aepy ligand. Each M(II) ion is four coordinated with four cyanide-carbon atoms in a square planar geometry and the [M(CN)4]2- anions act as a counter ion. The 4aepyH cations in the complexes compose of the protonation of the 4aepy. The vibrational spectral data also supported to the crystal structures of the complexes. Thermal stabilities and decomposition products of the complexes were investigated in the temperature range 40-700 °C in the static air atmosphere.

Acute Oral Toxicity Evaluations of Some Zinc(II) Complexes Derived from 1-(2-Salicylaldiminoethyl)piperazine Schiff Bases in Rats

PubMed Central

Salga, Muhammad Saleh; Ali, Hapipah Mohd; Abdulla, Mahmood Ameen; Abdelwahab, Siddig Ibrahim

2012-01-01

The current study described the synthesis and the in vivo acute oral toxicity evaluations in Sprague Dawley rats. The compounds were characterized by elemental analyses, LC-MS, FTIR, 1H NMR, 13C NMR and UV-visible spectroscopy. In the acute toxicity study, a single administration of the compounds was performed orally to the rats at the single doses of 2000 mg/kg and they were then monitored for possible side effects, mortality or behavioral changes up to 14 days. The serum level of aspartate (AST), alanine aminotransferases (ALT), alkaline phosphate (ALP), triglyceride, high density lipoprotein (HDL), immunoglobulins (GAM) and the C-reactive proteins did not significantly change. The hematological indices white blood cells (WBC), haematocrit (HCT), red blood cells (RBC), mean corpuscular volume (MCV), mean corpuscular haemoglobin concentration (MCHC), and mean corpuscular hemoglobin (MCH) were within the normal range. The renal function indices examined were also within the reference range. Generally, the compounds exhibited low toxic effects as required for further in vivo therapeutic studies. PMID:22408397

Effect of operating parameters on bio-fuel production from waste furniture sawdust.

PubMed

Uzun, Basak Burcu; Kanmaz, Gülin

2013-04-01

Fast pyrolysis is an effective technology for conversion of biomass into energy and value-added chemicals instead of burning them directly. In this study, fast pyrolysis of waste furniture sawdust (pine sawdust) was investigated under various reaction conditions (reaction time, pyrolysis temperature, heating rate, residence time and particle size) in a tubular reactor. The optimum reaction conditions for bio-oil production was found as reaction time of 5 min, pyrolysis temperature of 500 °C, heating rate of 300 °C min(-1) under nitrogen flow rate of 400 cm(3) min(-1). At these conditions, maximum bio-oil yield was obtained as 42.09%. Pyrolysis oils were characterized by using various elemental analyses, fourier - transformation infrared (FT-IR) spectrometry and gas chromatography-mass spectrometry (GC-MS). The results of the GC-MS showed that cracking of large molecular phenolics was followed by partial conversion into phenol and alkylated phenols (45%) during the pyrolysis. According to the experimental and characterization results; the liquid product could be used as feedstock for the chemical industry or petroleum crude for refinery.

Investigating the origins of rhythmic major-element zoning in HP/LT garnets from worldwide subduction mélanges

NASA Astrophysics Data System (ADS)

Viete, D. R.; Hacker, B. R.; Seward, G.; Allen, M. B.

2016-12-01

Rhythmic major-element zoning has been documented in garnets from high pressure/low temperature (HP/LT) lenses within a number of worldwide subduction mélanges (e.g. California, Chinese Tianshan, Cuba, Greek Cyclades, Guatemala, Japan, Venezuela). The origin of these features has implications for the nature of subduction-zone processes. Conditions of rhythmic zoning acquirement in HP/LT garnets of California and Venezuela were investigated by use of Raman and FTIR microspectroscopy, and thermodynamic modelling of phase equilibria. Quartz-in-garnet Raman barometry reveals varying P—on the order of 100­-300 MPa, over radial distances of 10s of µm—in association with the high-Mn (and low-Mg) bands that define the fine-scale rhythmic zoning. Results from FTIR microspectroscopy demonstrate association between the high-Mn bands and locally depressed (structural) OH and elevated (molecular) H2O concentrations. The microspectroscopy results suggest changes in P and fluid activity attended development of the cryptic rhythmic zoning. Perple_X modelling of phase equilibria shows that, for specific rock chemistry and subduction P-T conditions, garnet modal abundance is extremely sensitive to changes in P (e.g. 10-20 vol.% growth/dissolution for ΔP = 200 MPa). Rhythmic major-element zoning may reflect P- and/or fluid-driven cycles of garnet stability-instability and/or varying reaction progress/kinetics during subduction. Steep compositional gradients that define the rhythmic major-element zoning limit time scales at subduction T, requiring that such individual stability-instability and/or accelerated reaction cycles were extremely brief. Seismic cycles or porosity waves represent ephemeral phenomena capable of accounting for development of rhythmic major-element zoning in HP/LT garnet, during subduction, as a result of fluctuations in both P and fluids. Metamorphic rocks may well carry detailed records of the catastrophism that punctuates longer-term tectonometamorphic processes.

Rapid authentication of edible bird's nest by FTIR spectroscopy combined with chemometrics.

PubMed

Guo, Lili; Wu, Yajun; Liu, Mingchang; Ge, Yiqiang; Chen, Ying

2018-06-01

Edible bird's nests (EBNs) have been traditionally regarded as a kind of medicinal and healthy food in China. For economic reasons, they are frequently subjected to adulteration with some cheaper substitutes, such as Tremella fungus, agar, fried pigskin, and egg white. As a kind of precious and functional product, it is necessary to establish a robust method for the rapid authentication of EBNs with small amounts of samples by simple processes. In this study, the Fourier transform infrared spectroscopy (FTIR) system was utilized and its feasibility for identification of EBNs was verified. FTIR spectra data of authentic and adulterated EBNs were analyzed by chemometrics analyses including principal component analysis, linear discriminant analysis (LDA), support vector machine (SVM) and one-class partial least squares (OCPLS). The results showed that the established LDA and SVM models performed well and had satisfactory classification ability, with the former 94.12% and the latter 100%. The OCPLS model was developed with prediction sensitivity of 0.937 and specificity of 0.886. Further detection of commercial EBN samples confirmed these results. FTIR is applicable in the scene of rapid authentication of EBNs, especially for quality supervision departments, entry-exit inspection and quarantine, and customs administration. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

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

PubMed

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

2018-01-15

Leaves of Urtica dioica collected from two areas of different environmental pollution were analysed by fourier transform infrared spectroscopy (FTIR) and electron paramagnetic resonance (EPR) spectroscopy. Analysis of FTIR spectra allows to describe main component of plant like proteins, lipids and carbohydrates. Although the FTIR spectra of plants from these two geographical locations of different environmental pollution appear to be relatively similar, 2D correlation shows completely different patterns. Synchronous and asynchronous correlation maps showed sequences of changes occurring during development of plant, manly in Amide I and Amide II, lignin, lipids and cellulose. In addition, 2D analysis revealed another sequence of changes as the function of plant growth depending on the degree of the environmental pollution. Two various kinds of paramagnetic species, transition metal ions (Mn(II), Fe(III)) and stable organic radicals (chlorophyll, semiquinone, tyrosyl and carbon centered) were found in leaves of nettle collected at different stages of development and growing in clean and polluted environment. In plants growing in polluted area the injuries of protein molecules bonding metal ions and the disturbances of photosynthesis and redox equilibrium in cells, as well as instability of polysaccharide structure of cell walls were observed. Copyright © 2017 Elsevier B.V. All rights reserved.

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.

Emission FTIR analyses of thin microscopic patches of jet fuel residue deposited on heated metal surface

NASA Technical Reports Server (NTRS)

Lauer, J. L.; Vogel, P.

1984-01-01

Deposits laid down in patches on metal strips in a high pressure/high temperature fuel system simulator operated with aerated fuel at varying flow rates were analyzed by emission FTIR in terms of functional groups. Significant differences were found in the spectra and amounts of deposits derived from fuels to which small concentrations of oxygen-, nitrogen-, or sulfur-containing heterocyclics or metal naphthenates were added. The spectra of deposits generated on strips by heating fuels and air in a closed container were very different from those of the flowing fluid deposits. One such closed-container dodecane deposit on silver gave a strong surface-enhanced Raman spectrum.

Synthesis, crystal structure and antimicrobial activities of two isomeric gold(I) complexes with nitrogen-containing heterocycle and triphenylphosphine ligands, [Au(L)(PPh3)] (HL = pyrazole and imidazole).

PubMed

Nomiya, K; Noguchi, R; Ohsawa, K; Tsuda, K; Oda, M

2000-03-01

Two isomeric gold(I)-triphenylphosphine complexes with nitrogen-containing heterocycles, [Au(L)(PPh3) (HL = pyrazole (1), imidazole (2)) were isolated as colorless cubic crystals for 1 and colorless plate crystals for 2, respectively. The crystal structures of 1 and 2 were determined by single-crystal X-ray diffraction. These complexes were also fully characterized by complete elemental analyses, thermogravimetric/differential thermal analyses (TG/DTA) and FT-IR in the solid state and by solution NMR (31P, 1H and 13C) spectroscopy and molecular weight measurements in acetone solution. These complexes consisted of a monomeric 2-coordinate AuNP core both in the solid state and in solution. The molecular structures of 1 and 2 were compared with those of related gold(I) complexes, [Au(1,2,3-triz)(PPh3)] (3, Htriz = triazole), [Au(1,2,4-triz)(PPh3)]2 (4) as a dimer through a gold(I)-gold(I) bond in the solid state, and [Au(tetz)(PPh3)] (5, Htetz = tetrazole). Selective and effective antimicrobial activities against two gram-positive bacteria (B. subtilis, S. aureus) and modest activities against one yeast (C. albicans) found in these gold(I) complexes 1-4 are noteworthy, in contrast to poor activities observed in the corresponding silver(I) complexes.

From synthetic to biogenic Mg-containing calcites: a comparative study using FTIR microspectroscopy.

PubMed

Long, Xia; Nasse, Michael J; Ma, Yurong; Qi, Limin

2012-02-21

The formation mechanism of the thermodynamically unstable calcite phase, very high Mg calcite, in biological organisms such as sea urchin or corallina algae has been an enigma for a very long time. In contrast to conventional methods such as KBr pellet Fourier Transform infrared (FTIR) spectroscopy and X-ray diffraction (XRD), FTIR microspectroscopy (FTIRM) provides additional information about a local disorder such as an amorphous phase or the occlusion of Mg ions in the calcite lattice. In this work, we characterise for the first time systematically synthetic and biogenic Mg-containing calcium carbonate samples (especially sea urchin teeth--SUT) in detail by using two FTIRM instruments and compare these samples with KBr pellet FTIR measurements. Furthermore, we present spectra from geogenic calcite and dolomite minerals, recorded with both FTIRM systems, as well as KBr pellet FTIR spectra as references. We analyse the spectra by applying multi-peak curve fitting on the in-plane-bending (ν(4)) and out-of-plane (ν(2)) bands. Based on the obtained results we attribute the two singlet bands at ∼860-865 cm(-1) and ∼695-704 cm(-1) observed in the SUT FTIRM spectra to the existence of amorphous calcium carbonate (ACC), and report for the first time the existence of ACC at the mature end of SUT. In the other three studied biominerals, however, we did not find any ACC. Also, based on the FTIRM results, we observe that not only ν(4), but also ν(2) shifts to higher wavenumbers if more calcium ions are replaced by magnesium ions in the calcite lattices.

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

PubMed

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

2013-05-15

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

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

PubMed

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

2010-03-01

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

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

PubMed

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

2017-04-01

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

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

NASA Astrophysics Data System (ADS)

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

2015-10-01

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

Synthesis of nanocrystalline CdS thin film by SILAR and their characterization

NASA Astrophysics Data System (ADS)

Mukherjee, A.; Satpati, B.; Bhattacharyya, S. R.; Ghosh, R.; Mitra, P.

2015-01-01

Cadmium sulphide (CdS) thin film was prepared by successive ion layer adsorption and reaction (SILAR) technique using ammonium sulphide as anionic precursor. Characterization techniques of XRD, SEM, TEM, FTIR and EDX were utilized to study the microstructure of the films. Structural characterization by x-ray diffraction reveals the polycrystalline nature of the films. Cubic structure is revealed from X-ray diffraction and selected area diffraction (SAD) patterns. The particle size estimated using X-ray line broadening method is approximately 7 nm. Instrumental broadening was taken into account while particle size estimation. TEM shows CdS nanoparticles in the range 5-15 nm. Elemental mapping using EFTEM reveals good stoichiometric composition of CdS. Characteristic stretching vibration mode of CdS was observed in the absorption band of FTIR spectrum. Optical absorption study exhibits a distinct blue shift in band gap energy value of about 2.56 eV which confirms the size quantization.

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

PubMed

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

2013-02-15

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

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

PubMed

Gökce, Halil; Bahçeli, Semiha

2013-12-01

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

Influence of Hemostatic Solution on Bond Strength and Physicochemical Properties of Resin Cement.

PubMed

Araújo, Isabela Sousa de; Prado, Célio Jesus do; Raposo, Luís Henrique Araújo; Soares, Carlos José; Zanatta, Rayssa Ferreira; Torres, Carlos Rocha Gomes; Ruggiero, Reinaldo; Silva, Gisele Rodrigues da

2017-01-01

The aim of this study was to evaluate the degree of conversion, color stability, chemical composition, and bond strength of a light-cured resin cement contaminated with three different hemostatic solutions. Specimens were prepared for the control (uncontaminated resin cement) and experimental groups (resin cement contaminated with one of the hemostatic solutions) according to the tests. For degree of conversion, DC (n = 5) and color analyses (n = 10), specimens (3 mm in diameter and 2 mm thick) were evaluated by Fourier transform infrared spectroscopy (FTIR) and CIELAB spectrophotometry (L*, a*, b*), respectively. For elemental chemical analysis (n = 1), specimens (2 mm thick and 6 mm in diameter) were evaluated by x-ray energy-dispersive spectroscopy (EDS). The bond strengths of the groups were assessed by the microshear test (n = 20) in a leucite-reinforced glass ceramic substrate, followed by failure mode analysis by scanning electron microscopy (SEM). The mean values, except for the elemental chemical evaluation and failure mode, were evaluated by ANOVA and Tukey's HSD test. The color stability was influenced by storage time (p<0.001) and interaction between contamination and storage time (p<0.001). Hemostop and Viscostat Clear contamination did not affect the DC, however Viscostat increased the DC. Bond strength of the resin cement to ceramic was negatively affected by the contaminants (p<0.001). Contamination by hemostatic agents affected the bond strength, degree of conversion, and color stability of the light-cured resin cement tested.

Membrane fouling of forward osmosis (FO) membrane for municipal wastewater treatment: A comparison between direct FO and OMBR.

PubMed

Sun, Yan; Tian, Jiayu; Zhao, Zhiwei; Shi, Wenxin; Liu, Dongmei; Cui, Fuyi

2016-11-01

In this work, membrane fouling behavior in a direct forward osmosis (FO) and an osmotic membrane bioreactor (OMBR) for municipal wastewater treatment was systematically investigated and compared. During the long-term operation, much severer flux decline was observed for the direct FO than that for the OMBR. The cake layer was found to be much thicker, together with large amounts of microorganisms growing on the membrane surface in direct FO. Interestingly, no obvious attachment of microorganisms on the membrane surface was observed in the OMBR. The fourier transform infrared spectroscopy (FTIR) and excitation emission matrices (EEM) analyses showed the polysaccharides and proteins were the dominant organic foulants in the fouling layer, and the quantity of the organic substances was also higher in direct FO than that in OMBR. Energy-dispersive X-ray (EDX) results indicated the main inorganic elements in the fouling layer were Ca, Mg, Fe and P, all of which exhibited higher relative percentages in direct FO than that in OMBR. The occurrence of higher contents of microorganisms, organic foulants and inorganic elements in the cake layer caused a higher filtration resistance for the FO membrane in the direct FO. Although more severe membrane fouling was identified in direct FO, the hydraulic and chemical cleaning was more effective on recovering the water permeability of the membrane in direct FO than that in OMBR. Copyright © 2016 Elsevier Ltd. All rights reserved.

Chemical modification of magnetite nanoparticles and preparation of acrylic-base magnetic nanocomposite particles via miniemulsion polymerization

NASA Astrophysics Data System (ADS)

Mahdieh, Athar; Mahdavian, Ali Reza; Salehi-Mobarakeh, Hamid

2017-03-01

Nowadays, magnetic nanocomposite particles have attracted many interests because of their versatile applications. A new method for chemical modification of Fe3O4 nanoparticles with polymerizable groups is presented here. After synthesis of Fe3O4 nanoparticles by co-precipitation method, they were modified sequentially with 3-aminopropyl triethoxysilane (APTES), acryloyl chloride (AC) and benzoyl chloride (BC) and all were characterized by FTIR, XRD, SEM and TGA analyses. Then the modified magnetite nanoparticles with unsaturated acrylic groups were copolymerized with methyl methacrylate (MMA), butyl acrylate (BA) and acrylic acid (AA) through miniemulsion polymerization. Although several reports exist on preparation of magnetite-base polymer particles, but the efficiency of magnetite encapsulationwith reasonable content and obtaining final stable latexes with limited aggregation ofFe3O4 are still important issues. These were considered here by controlling reaction parameters. Hence, a seriesofmagneticnanocomposites latex particlescontaining different amounts of Fe3O4 nanoparticles (0-10 wt%) were prepared with core-shell morphology and diameter below 200 nm and were characterized by FT-IR, DSC and TGA analyses. Their morphology and size distribution were studied by SEM, TEM and DLS analyses too. Magnetic properties of all products were also measuredby VSM analysis and the results revealed almost superparamagnetic properties for the obtained nanocomposite particles.

Investigation on the effect of RF air plasma and neem leaf extract treatment on the surface modification and antimicrobial activity of cotton fabric

NASA Astrophysics Data System (ADS)

Vaideki, K.; Jayakumar, S.; Rajendran, R.; Thilagavathi, G.

2008-02-01

A thorough investigation on the antimicrobial activity of RF air plasma and azadirachtin (neem leaf extract) treated cotton fabric has been dealt with in this paper. The cotton fabric was given a RF air plasma treatment to improve its hydrophilicity. The process parameters such as electrode gap, time of exposure and RF power have been varied to study their effect in improving the hydrophilicity of the cotton fabric and they were optimized based on the static immersion test results. The neem leaf extract (azadirachtin) was applied on fabric samples to impart antimicrobial activity. The antimicrobial efficacy of the samples have been analysed and compared with the efficacy of the cotton fabric treated with the antimicrobial finish alone. The investigation reveals that the RF air plasma has modified the surface of the fabric, which in turn increased the antimicrobial activity of the fabric when treated with azadirachtin. The surface modification due to RF air plasma treatment has been analysed by comparing the FTIR spectra of the untreated and plasma treated samples. The molecular interaction between the fabric, azadirachtin and citric acid which was used as a cross linking agent to increase the durability of the antimicrobial finish has also been analysed using FTIR spectra.

O-6 Optical Property Degradation of the Hubble Space Telescope's Wide Field Camera-2 Pick Off Mirror

NASA Technical Reports Server (NTRS)

McNamara, Karen M.; Hughes, D. W.; Lauer, H. V.; Burkett, P. J.; Reed, B. B.

2011-01-01

Degradation in the performance of optical components can be greatly affected by exposure to the space environment. Many factors can contribute to such degradation including surface contaminants; outgassing; vacuum, UV, and atomic oxygen exposure; temperature cycling; or combinations of parameters. In-situ observations give important clues to degradation processes, but there are relatively few opportunities to correlate those observations with post-flight ground analyses. The return of instruments from the Hubble Space Telescope (HST) after its final servicing mission in May 2009 provided such an opportunity. Among the instruments returned from HST was the Wide-Field Planetary Camera-2 (WFPC-2), which had been exposed to the space environment for 16 years. This work focuses on the identifying the sources of degradation in the performance of the Pick-off mirror (POM) from WFPC-2. Techniques including surface reflectivity measurements, spectroscopic ellipsometry, FTIR (and ATR-FTIR) analyses, SEM/EDS, X-ray photoelectron spectroscopy (XPS) with and without ion milling, and wet and dry physical surface sampling were performed. Destructive and contact analyses took place only after completion of the non-destructive measurements. Spectroscopic ellipsometry was then repeated to determine the extent of contaminant removal by the destructive techniques, providing insight into the nature and extent of polymerization of the contaminant layer.

Trace gas emissions from biomass burning in tropical Australian savannas

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

Hurst, D.F.; Griffith, D.W.T.; Cook, G.D.

1994-08-20

The trace gas emissions of biomass burning was measured during the 1991 and 1992 dry seasons (April through October) at the Kapalga Research Station in Kakadu National Park, Northern Territory, Australia. Over 100 smoke samples from savannah fires were collected, from the ground and from aircraft flying at 50 to 700 meters above the fires. The samples were analyzed for carbon dioxide, carbon monoxide, nitrous oxides, and other carbon and nitrogen compounds using gas phase Fourier transform infrared (FTIR) spectroscopy, matrix isolation FTIR spectroscopy, and chemiluminescence techniques. This paper describes the results of the gas analyses and discusses the potentialmore » impacts of these gases on regional atmospheric chemistry.49 refs., 4 figs., 7 tabs.« less

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

PubMed

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

2017-10-01

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

Effect of ingested tungsten oxide (WOx) nanofibers on digestive gland tissue of Porcellio scaber (Isopoda, Crustacea): fourier transform infrared (FTIR) imaging.

PubMed

Novak, Sara; Drobne, Damjana; Vaccari, Lisa; Kiskinova, Maya; Ferraris, Paolo; Birarda, Giovanni; Remškar, Maja; Hočevar, Matej

2013-10-01

Tungsten nanofibers are recognized as biologically potent. We study deviations in molecular composition between normal and digestive gland tissue of WOx nanofibers (nano-WOx) fed invertebrate Porcellio scaber (Iosopda, Crustacea) and revealed mechanisms of nano-WOx effect in vivo. Fourier Transform Infrared (FTIR) imaging performed on digestive gland epithelium was supplemented by toxicity and cytotoxicity analyses as well as scanning electron microscopy (SEM) of the surface of the epithelium. The difference in the spectra of the Nano-WOx treated and control cells showed up in the central region of the cells and were related to lipid peroxidation, and structural changes of nucleic acids. The conventional toxicity parameters failed to show toxic effects of nano-WOx, whereas the cytotoxicity biomarkers and SEM investigation of digestive gland epithelium indicated sporadic effects of nanofibers. Since toxicological and cytological measurements did not highlight severe effects, the biochemical alterations evidenced by FTIR imaging have been explained as the result of cell protection (acclimation) mechanisms to unfavorable conditions and indication of a nonhomeostatic state, which can lead to toxic effects.

FTIR gas analysis with improved sensitivity and selectivity for CWA and TIC detection

NASA Astrophysics Data System (ADS)

Phillips, Charles M.; Tan, Huwei

2010-04-01

This presentation describes the use of an FTIR (Fourier Transform Infrared)-based spectrometer designed to continuously monitor ambient air for the presence of chemical warfare agents (CWAs) and toxic industrial chemicals (TICs). The necessity of a reliable system capable of quickly and accurately detecting very low levels of CWAs and TICs while simultaneously retaining a negligible false alarm rate will be explored. Technological advancements in FTIR sensing have reduced noise while increasing selectivity and speed of detection. These novel analyzer design characteristics are discussed in detail and descriptions are provided which show how optical throughput, gas cell form factor, and detector response are optimized. The hardware and algorithms described here will explain why this FTIR system is very effective for the simultaneous detection and speciation of a wide variety of toxic compounds at ppb concentrations. Analytical test data will be reviewed demonstrating the system's sensitivity to and selectivity for specific CWAs and TICs; this will include recent data acquired as part of the DHS ARFCAM (Autonomous Rapid Facility Chemical Agent Monitor) project. These results include analyses of the data from live agent testing for the determination of CWA detection limits, immunity to interferences, detection times, residual noise analysis and false alarm rates. Sensing systems such as this are critical for effective chemical hazard identification which is directly relevant to the CBRNE community.

Reconnaissance gas measurements on the East Rift Zone of Kilauea Volcano, Hawai'i by Fourier transform infrared spectroscopy

USGS Publications Warehouse

McGee, Kenneth A.; Elias, Tamar; Sutton, A. Jefferson; Doukas, Michael P.; Zemek, Peter G.; Gerlach, Terrence M.

2005-01-01

We report the results of a set of measurements of volcanic gases on two small ground level plumes in the vicinity of Pu`u `O`o cone on the middle East Rift Zone (ERZ) of Kilauea volcano, Hawai`i on 15 June 2001 using open-path Fourier transform infrared (FTIR) spectroscopy. The work was carried out as a reconnaissance survey to assess the monitoring and research value of FTIR measurements at this volcano. Despite representing emissions of residual volatiles from lava that has undergone prior degassing, the plumes contained detectable amounts of CO2, CO, SO2, HCl, HF and SiF4. Various processes, including subsurface cooling, condensation of water in the atmospheric plume, oxidation, dissolution in water, and reactions with wall rocks at plume vents affect the abundance of these gases. Low concentrations of volcanic CO2 measured against a high ambient background are not well constrained by FTIR spectroscopy. Although there appear to be some differences between these gases and Pu`u `O`o source gases, ratios of HCl/SO2, HF/SO2 and CO/SO2 determined by FTIR measurements of these two small plumes compare reasonably well with earlier published analyses of ERZ vent samples. The measurements yielded emission rate estimates of 4, 11 and 4 t d-1

ATR-FTIR microscopy in mapping mode for the study of verdigris and its secondary products

NASA Astrophysics Data System (ADS)

Prati, S.; Bonacini, I.; Sciutto, G.; Genty-Vincent, A.; Cotte, M.; Eveno, M.; Menu, M.; Mazzeo, R.

2016-01-01

To study degradation processes occurring on painting materials, the use of high-resolution micro-analytical techniques is highly requested since it provides a detailed identification and localisation of both the original and deteriorated ingredients. Among the various pigments recently studied, the characterisation of verdigris has received a major interest. This pigment has not a unique chemical formula, but its composition depends on the recipe employed for its manufacturing. Moreover, verdigris paints are not stable and are subject to a colour change from blue-green to green, which occurs in the first few months after the application. In this paper, we focused our attention on the use of ATR-FTIR mapping as a useful method to identify verdigris secondary products and pathways. Several mock-ups and real samples have been analysed, and the correlation among the detected compounds and their spatial location, obtained by the application of ATR-FTIR microscopy in mapping mode, allowed formulating some hypotheses on the degradation pattern of verdigris, which may feed the discussion on the transformation and stability of this pigment. From an analytical point of view, we showed how FTIR mapping approaches may be extremely useful both for the identification of compounds in complex matrix in which single spectra may limit the exhaustive characterisations due to bands overlapping and for the study of degradation pathways by taking into consideration the relative distribution of degradation products.

Characterization of liquefied wood residues from different liquefaction conditions

Treesearch

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

2007-01-01

The amount of wood residue is used as a measurement of the extent of wood liquefaction. Characterization of the residue from wood liquefaction provides a new approach to understand some fundamental aspects of the liquefaction reaction. Residues were characterized by wet chemical analyses, Fourier transform infrared (FTIR) spectroscopy, X-ray diffraction (XRD), and...

Using FTIR-ATR Spectroscopy to Teach the Internal Standard Method

ERIC Educational Resources Information Center

Bellamy, Michael K.

2010-01-01

The internal standard method is widely applied in quantitative analyses. However, most analytical chemistry textbooks either omit this topic or only provide examples of a single-point internal standardization. An experiment designed to teach students how to prepare an internal standard calibration curve is described. The experiment is a modified…

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

PubMed

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

2013-04-07

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

Acetone sensor based on zinc oxide hexagonal tubes

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

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

2014-04-24

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

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

NASA Astrophysics Data System (ADS)

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

2002-10-01

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

Modification of surface characteristic and tribo-electric properties of polymers by DBD plasma in atmospheric air

NASA Astrophysics Data System (ADS)

Bekkara, Mohammed Fethi; Dascalescu, Lucien; Benmimoun, Youcef; Zeghloul, Thami; Tilmatine, Amar; Zouzou, Noureddine

2018-01-01

The aim of this paper is to quantify the effects of dielectric barrier discharge (DBD) exposure on the physico-chemical and tribo-electric properties of polymers. The study was conducted in atmospheric air on polypropylene, polyethylene and polyvinyl-chloride. These three types of polymers are widely used in industry. The polymers were characterized by means of an optical profilometer, a fourier-transform infrared (FTIR) spectrometer and an electric charge measurement system. The latter is composed of a Faraday pail connected to an electrometer. The profilometer analyses showed that the DBD plasma treatment has increased the surface roughness of the three polymers. FTIR revealed that oxygen atoms and polar groups were grafted on their surfaces, thereby conferring them a hydrophilic character. The short (2 sec) DBD plasma treatment has considerably improved the electrostatic charge acquired by the polymers during electrostatic tribo-charging, while longer exposures conferred the polymer anti-static properties and decreased its tribo-charging capability. The correlation between the results of the physico-chemical analyses and the tribo-electric behavior has been discussed.

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

PubMed

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

2008-06-01

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

UV–Vis and ATR–FTIR spectroscopic investigations of postmortem interval based on the changes in rabbit plasma

PubMed Central

Wang, Qi; He, Haijun; Li, Bing; Lin, Hancheng; Zhang, Yinming; Zhang, Ji

2017-01-01

Estimating PMI is of great importance in forensic investigations. Although many methods are used to estimate the PMI, a few investigations focus on the postmortem redistribution. In this study, ultraviolet–visible (UV–Vis) measurement combined with visual inspection indicated a regular diffusion of hemoglobin into plasma after death showing the redistribution of postmortem components in blood. Thereafter, attenuated total reflection–Fourier transform infrared (ATR–FTIR) spectroscopy was used to confirm the variations caused by this phenomenon. First, full-spectrum partial least-squares (PLS) and genetic algorithm combined with PLS (GA-PLS) models were constructed to predict the PMI. The performance of GA-PLS model was better than that of full-spectrum PLS model based on its root mean square error (RMSE) of cross-validation of 3.46 h (R2 = 0.95) and the RMSE of prediction of 3.46 h (R2 = 0.94). The investigation on the similarity of spectra between blood plasma and formed elements also supported the role of redistribution of components in spectral changes in postmortem plasma. These results demonstrated that ATR-FTIR spectroscopy coupled with the advanced mathematical methods could serve as a convenient and reliable tool to study the redistribution of postmortem components and estimate the PMI. PMID:28753641

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.

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

PubMed Central

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

2017-01-01

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

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.

Finite element analysis of structural engineering problems using a viscoplastic model incorporating two back stresses

NASA Technical Reports Server (NTRS)

Arya, Vinod K.; Halford, Gary R.

1993-01-01

The feasibility of a viscoplastic model incorporating two back stresses and a drag strength is investigated for performing nonlinear finite element analyses of structural engineering problems. To demonstrate suitability for nonlinear structural analyses, the model is implemented into a finite element program and analyses for several uniaxial and multiaxial problems are performed. Good agreement is shown between the results obtained using the finite element implementation and those obtained experimentally. The advantages of using advanced viscoplastic models for performing nonlinear finite element analyses of structural components are indicated.

H2o Quantitative Analysis of Transition Zone Minerals Wadsleyite and Ringwoodite By Raman Spectroscopy

NASA Astrophysics Data System (ADS)

Novella, D.; Bolfan-Casanova, N.; Bureau, H.; Raepsaet, C.; Montagnac, G.

2014-12-01

Liquid H2O covers approximately 70% of the Earth's surface but it can also be incorporated as OH- groups in nominally anhydrous minerals (NAMs) that constitute the Earth's mantle, as observed in peridotitic xenoliths. The presence of even trace amounts (ppm wt) of hydrogen in mantle minerals strongly affect the physical, chemical and rheological properties of the mantle. The Earth's transition zone (410 to 660 km depth) is particularly important in this regard since it can store large amounts of H2O (wt%) as shown by experiments and recently by a natural sample. Addressing the behavior of H2O at high depths and its potential concentration in mantle NAMs is therefore fundamental to fully comprehend global-scale processes such as plate tectonics and magmatism. We developed an innovative technique to measure the H2O content of main transition zone NAMs wadsleyite and ringwoodite by Raman spectroscopy. This technique allows to use a beam of 1-3 µm size to measure small samples that are typical for high pressure natural and synthetic specimens. High pressure polyphasic samples are indeed very challenging to be measured in terms of H2O content by the routinely used Fourier transform infra-red (FTIR) spectroscopy and ion probe mass spectroscopy analyses, making the Raman approach a valid alternative. High quality crystals of wadsleyite and ringwoodite were synthesized at high pressure and temperature in a multi-anvil press and analyzed by Raman and FTIR spectroscopy as well as elastic recoil detection analyses (ERDA) which is an absolute, standard-free technique. We will present experimental data that allow to apply Raman spectroscopy to the determination of H2O content of the most abundant minerals in the transition zone. The data gathered in this study will also permit to investigate the absorption coefficients of wadsleyite and ringwoodite that are employed in FTIR quantitative analyses.

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

NASA Astrophysics Data System (ADS)

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

2016-11-01

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

Assessment of Ethylene Vinyl-Acetato Copolymer (EVA) Samples Bombarded by Gamma Radiation via Linearity Analyses

NASA Astrophysics Data System (ADS)

de Oliveira, L. N.; do Nascimento, E. O.; Schimidt, F.; Antonio, P. L.; Caldas, L. V. E.

2018-03-01

Materials with the potential to become dosimeters are of interest in radiation physics. In this research, the materials were analyzed and compared in relation to their linearity ranges. Samples of ethylene vinyl-acetate copolymer (EVA) were irradiated with doses from 10 Gy to 10 kGy using a 60Co Gamma-Cell system 220 and evaluated with the FTIR technique. The linearity analyses were applied through two methodologies, searching for linear regions in their response. The results show that both applied analyses indicate linear regions in defined dose interval. The radiation detectors EVA can be useful for radiation dosimetry in intermediate and high doses.

Organic geochemistry of resins from modern Agathis australis and Eocene resins from New Zealand: Diagenetic and taxonomic implications

USGS Publications Warehouse

Lyons, P.C.; Mastalerz, Maria; Orem, W.H.

2009-01-01

A maturation series of resins and fossil resins from New Zealand, ranging in age from Modern to Eocene and ranging from uncoalified to high volatile C bituminous coal, were analyzed by elemental, pyrolysis-gas chromatography (Py-GC), Fourier Transform infrared (FTir), and solid-state 13C nuclear magnetic resonance (13C NMR) techniques. For comparison, four resin samples from the Latrobe Valley, Australia, were analyzed. All of the resins and fossil resins of this study show very high H/C atomic ratios, and are characterized by dominant peaks in the 10-60??ppm range of solid-state 13C NMR spectra and prominent bands in the aliphatic stretching region (2800-3000??cm- 1) of FTir spectra, all indicating a highly aliphatic molecular structure. The 13C NMR and FTir data indicate a diterpenoid structure for these resins. There is an abrupt loss of oxygen that occurs at the Lignite A/Subbituminous C stage, which is attributed to a dramatic loss of carboxyl (COOH) from the diterpenoid molecule. This is a new finding in the diagenesis of resins. This important loss in oxygenated functional groups is attributed to a maturation change. Also, there is a progressive loss of exomethylene (CH2) groups with increasing degree of maturation, as shown by both 13C NMR and FTir data. This change has been noted by previous investigators. Exomethylene is absent in the fossil resins from the Eocene high volatile C bituminous coals. This progressive loss is characteristic of Class I resinites. FTir data indicate that the oxygenated functional groups are strong in all the resin samples except the fossil resin from high volatile C bituminous coal. This important change in oxygenated functional groups is attributed to maturation changes. The 13C NMR and FTir data indicate there are minor changes in the Agathis australis resin from the living tree and soil, which suggests that alteration of A. australis resins begins shortly after deposition in the soil for as little as 1000??years. The Morwell and Yallourn fossil resins from brown coal (lignite B) Australia do not have some of the FTir characteristics of the New Zealand resins, which most likely indicates they have a different plant source because different degrees of oxidation and weathering and changes due to fires (i.e., charring) can be ruled out. Our results have implications for studies of the maturation, provenance, and botanical sources of fossil resins and resinites in Eocene and Miocene coals and sediments of New Zealand and Australia. ?? 2009 Elsevier B.V. All rights reserved.

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

PubMed Central

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

2015-01-01

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

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

PubMed

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

2014-10-15

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

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

PubMed

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

2018-02-01

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

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

PubMed Central

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

2013-01-01

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

Optical, thermal and morphological study of ZnS doped PVA polymer nano composites

NASA Astrophysics Data System (ADS)

Guruswamy, B.; Ravindrachary, V.; Shruthi, C.; Sagar, Rohan N.; Hegde, Shreedatta

2018-05-01

The effect of ZnS nano particle doping on optical, thermal properties and morphological study of the PVA polymer has been investigated using FTIR, UV-Visible and TGA, FESEM techniques. Nano sized ZnS particles were synthesized by a simple wet chemical route. Pure and ZnS/PVA nano composites were prepared using solution casting technique. The FTIR study confirms that the ZnS nano particles interacts with the OH group of PVA polymer and forms the complex. The formation of these complexes affects the optical and thermal properties of the composite. The changes in optical properties were studied using UV-Vis absorption method. The variation in thermal property was analysed using TGA results. The modified surface morphology analysis was carried out using FESEM.

Fabrication and characterization of nickel oxide nanoparticles/silicon NiO NPS/Si

NASA Astrophysics Data System (ADS)

Shuihab, Aliyah; Khalf, Surour

2018-05-01

In this study, (NiO) thin film which prepared by chemical method and deposited by drop casting technique on glass. The structural, optical and chemical analyses have been investigated. X-ray diffraction (XRD) measurements relieve that the (NiO) thin film was polycrystalline, cubic structure and there is no trace of the other material. UV-Vis measurements reveal that the energy gap of (NiO) thin film was found 1.8 eV. The Fourier Transform Infrared Spectroscopy (FTIR) spectrum of (NiO) thin film shows NiO nanoparticles had its IR peak of Ni-O stretching vibration and shifted to blue direction. Due to their quantum size effect and spherical nanostructures, the FTIR absorption of NiO nanoparticles is blue-shifted compared to that of the bulk form.

Pectin functionalised by fatty acids: Diffuse reflectance infrared Fourier transform (DRIFT) spectroscopic characterisation

NASA Astrophysics Data System (ADS)

Kamnev, Alexander A.; Calce, Enrica; Tarantilis, Petros A.; Tugarova, Anna V.; De Luca, Stefania

2015-01-01

Chemically modified pectin derivatives obtained by partial esterification of its hydroxyl moieties with fatty acids (FA; oleic, linoleic and palmitic acids), as well as the initial apple peel pectin were comparatively characterised using diffuse reflectance infrared Fourier transform (DRIFT) spectroscopy. Characteristic changes observed in DRIFT spectra in going from pectin to its FA esters are related to the corresponding chemical modifications. Comparing the DRIFT spectra with some reported data on FTIR spectra of the same materials measured in KBr or NaCl matrices has revealed noticeable shifts of several polar functional groups both in pectin and in its FA-esterified products induced by the halide salts. The results obtained have implications for careful structural analyses of biopolymers with hydrophilic functional groups by means of different FTIR spectroscopic methodologies.

Ultrasound-assisted facile synthesis of a new tantalum(V) metal-organic framework nanostructure: Design, characterization, systematic study, and CO{sub 2} adsorption performance

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

Sargazi, Ghasem, E-mail: g.sargazi@gmail.com; Young Researchers Society, Shahid Bahonar University of Kerman, Kerman, Iran; Afzali, Daryoush, E-mail: daryoush_afzali@yahoo.com

2017-06-15

This work presents a fast route for the preparation of a new Ta(V) metal-organic framework nanostructure with high surface area, significant porosity, and small size distribution. X-ray diffraction (XRD), scanning electron microscopy (SEM), Transition electron microscopy (TEM), energy dispersive spectrometer (EDS), thermo-gravimetric analysis (TGA), differential scanning calorimetry (DSC), fourier transform infrared spectroscopy (FTIR), CHNS/O elemental analyser, and Brunauer-Emmett-Teller (BET) surface area analysis were applied to characterize the synthesized product. Moreover, the influences of ultrasonic irradiation including temperature, time, and power on different features of the final products were systematically studied using 2{sup k-1} factorial design experiments, and the response surfacemore » optimization was used for determining the best welding parameter combination. The results obtained from analyses of variances showed that ultrasonic parameters affected the size distribution, thermal behaviour, and surface area of Ta-MOF samples. Based on response surface methodology, Ta-MOF could be obtained with mean diameter of 55 nm, thermal stability of 228 °C, and high surface area of 2100 m{sup 2}/g. The results revealed that the synthesized products could be utilized in various applications such as a novel candidate for CO{sub 2} adsorption. - Graphical abstract: A facile route was used for fabrication of a new metal -organic framework based on tantalum nanostructures that have high surface area, considerable porosity, homogenous morphology, and small size distribution.« less

Electrophoretic Deposition of Chitosan/45S5 Bioactive Glass Composite Coatings Doped with Zn and Sr

PubMed Central

Miola, Marta; Verné, Enrica; Ciraldo, Francesca Elisa; Cordero-Arias, Luis; Boccaccini, Aldo R.

2015-01-01

In this research work, the original 45S5 bioactive glass was modified by introducing zinc and/or strontium oxide (6 mol%) in place of calcium oxide. Sr was added for its ability to stimulate bone formation and Zn for its role in bone metabolism, antibacterial properties, and anti-inflammatory effect. The glasses were produced by means of melting and quenching process. SEM and XRD analyses evidenced that Zr and Sr introduction did not modify the glass structure and morphology while compositional analysis (EDS) demonstrated the effective incorporation of these elements in the glass network. Bioactivity test in simulated body fluid (SBF) up to 1 month evidenced a reduced bioactivity kinetics for Zn-doped glasses. Doped glasses were combined with chitosan to produce organic/inorganic composite coatings on stainless steel AISI 316L by electrophoretic deposition (EPD). Two EPD processes were considered for coating development, namely direct current EPD (DC-EPD) and alternating current EPD (AC-EPD). The stability of the suspension was analyzed and the deposition parameters were optimized. Tape and bending tests demonstrated a good coating-substrate adhesion for coatings containing 45S5-Sr and 45S5-ZnSr glasses, whereas the adhesion to the substrate decreased by using 45S5-Zn glass. FTIR analyses demonstrated the composite nature of coatings and SEM observations indicated that glass particles were well integrated in the polymeric matrix, the coatings were fairly homogeneous and free of cracks; moreover, the AC-EPD technique provided better results than DC-EPD in terms of coating quality. SEM, XRD analyses, and Raman spectroscopy, performed after bioactivity test in SBF solution, confirmed the bioactive behavior of 45S5-Sr-containing coating while coatings containing Zn exhibited no hydroxyapatite formation. PMID:26539431

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

PubMed

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

2016-06-15

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

Synthesis, characterization, spectrophotometric, structural and antimicrobial studies of the newly charge transfer complex of p-phenylenediamine with π acceptor picric acid

NASA Astrophysics Data System (ADS)

Khan, Ishaat M.; Ahmad, Afaq; Oves, M.

2010-12-01

Charge transfer complex (CTC) of donor, p-phenylenediamine (PPD) and acceptor, 2,4,6-trinitrophenol (picric acid) has been studied in methanol at room temperature. The CT complex was synthesized and characterized by elemental analysis, FTIR spectra, 1H NMR spectroscopy and electronic absorption spectra which indicate the CT interaction associated with proton migration from the acceptor to the donor followed by hydrogen bonding via N +-H⋯O -. The thermal stability of CT complex was studied using TGA and DTA analyses techniques. The CT complex was screened for its antifungal activity against Aspergillus niger (Laboratory isolate), Candida albicans (IQA-109) and Penicillium sp. (Laboratory isolate) and antibacterial activity against two Gram-positive bacteria Staphylococcus aureus (MSSA 22) and Bacillus subtilis (ATCC 6051) and two Gram-negative bacteria Escherichia coli (K 12) and Pseudomonas aeruginosa (MTCC 2488). It gives good antimicrobial activity. The stoichiometry of the CT complex was found to be 1:1. The physical parameters of CT complex were evaluated by the Benesi-Hildebrand equation. On the basis of the studies, the structure of CT complex is [(PPDH) +(PA) -], and a general mechanism for its formation is proposed.

Rod shaped oxovanadium(IV) Schiff base complexes: Synthesis, mesomorphism and influence of flexible alkoxy chain lengths

NASA Astrophysics Data System (ADS)

Gupta, Bishop Dev; Datta, Chitraniva; Das, Gobinda; Bhattacharjee, Chira R.

2014-06-01

A series of oxovanadium(IV) complexes of bidentate [N,O] donor Schiff-base ligands of the type [VO(L)2], [L = N-(4-n-alkoxysalicylaldimine)-4‧-octadecyloxyaniline, n = 8, 10, 12, 14, 16 and 18] have been synthesized. The compounds were characterized by elemental analyses, Fourier transform infrared spectroscopy (FTIR), 1H, 13C nuclear magnetic resonance (NMR), ultraviolet-visible spectroscopy (UV-Vis), and fast atom bombardment (FAB) mass spectrometry. The mesomorphic behavior of the compounds was studied by polarized optical microscopy (POM) and differential scanning calorimetry (DSC). The ligands and complexes are all thermally stable exhibiting smectic mesomorphism. The ligands 8-OR to16-OR show SmC phase at ∼113-118 °C and an unidentified SmX phase reminiscent of soft crystal at ∼77-91 °C whereas the complexes all showed SmA phases. Interestingly the complexes with C10 and C12 alkoxy chain length exhibited additionally SmC phases also. The melting points of the ligands linearly increases whereas mesophase to isotropic transition temperature decreases as a function of increasing carbon chain length of alkoxy arm while no trend was apparently noticeable for the complexes.

Two new Ni(II) supramolecular complexes based on ethyl isonicotinate and ethyl nicotinate for removal of acid blue 92 dye

NASA Astrophysics Data System (ADS)

Etaiw, Safaa El-din H.; Marie, Hassan

2018-03-01

Two new luminescent supramolecular complexes (SC); [Ni(EIN)4(NCS)2] SC1 and [Ni2(EN)8(NCS)4] SC2, (EIN = ethyl isonicotinate, EN = ethyl nicotinate), have been synthesized by self-assembly method and structurally characterized by X-ray single crystal, FT-IR and UV-Vis spectra, PXRD, elemental and thermogravimetric analyses. Both SC1 and SC2 are monoclinic crystals however, they have different asymmetric units. Ni(II) atoms in both SC are isostructural and have similar hexa-coordinate environment. The structures of SC1 and SC2 consist of parallel polymeric 1D-chains, extended in two and three dimensional supramolecular frameworks by intermolecular hydrogen bonding interactions. SC1 and SC2 are luminescent materials which can be used in applications as molecular sensing systems. SC1 and SC2 were used as heterogeneous catalysts for degradation of acid blue 92 (AB-92) under sun light irradiation. The fluorescence measurements of terephthalic acid technique as a probe molecule were used to determine the •OH radicals. Also the radicals trapping experiments using isopropanol alcohol (IPA) as radical scavenger were discussed. In addition a mechanism of degradation was proposed and discussed.

The preparation and antioxidant activity of the sulfanilamide derivatives of chitosan and chitosan sulfates.

PubMed

Zhong, Zhimei; Ji, Xia; Xing, Ronge; Liu, Song; Guo, Zhanyong; Chen, Xiaolin; Li, Pengcheng

2007-06-01

Chitosan (CS) and chitosan sulfates (CSS) with different molecular weight (Mw) were reacted with 4-acetamidobenzene sulfonyl chloride to obtain sulfanilamide derivatives of chitosan and chitosan sulfates (LSACS, HSACS, LSACSS, HSACSS). The preparation conditions such as different reaction time, temperature, solvent, and the molar ratio of reaction materials are discussed in this paper. Their structures were characterized by FTIR spectroscopy and elemental analyses. The antioxidant activities of the derivatives were investigated employing various established in vitro systems, such as hydroxyl-radical ((*)OH) superoxide anion (O2(*-)) scavenging and reducing power. All kinds of the compounds (HCS, LCS, HCSS, LCSS, HSACS, LSACS, HSACSS, LSACSS) showed stronger scavenging activity on hydroxyl radical than ascorbic acid (Vc). The inhibitory activities of the derivatives toward superoxide radical by the PMS-NADH system were obvious. The experiment showed that the superoxide radical scavenging effect of sulfanilamide derivatives of chitosan and chitosan sulfates was stronger than that of original CS and CSS. All of the derivatives were efficient in the reducing power. The results indicated that the sulfanilamide group were grafted on CS and CSS increased the reducing power of them obviously.

Regular square planer bis-(4,4,4-trifluoro-1-(thiophen-2-yl)butane-1,3-dione)/copper(II) complex: Trans/cis-DFT isomerization, crystal structure, thermal, solvatochromism, hirshfeld surface and DNA-binding analysis

NASA Astrophysics Data System (ADS)

Hema, M. K.; Karthik, C. S.; Warad, Ismail; Lokanath, N. K.; Zarrouk, Abdelkader; Kumara, Karthik; Pampa, K. J.; Mallu, P.

2018-04-01

Trans-[Cu(O∩O)2] complex, O∩O = 4,4,4-trifluoro-1-(thiophen-2-yl)butane-1,3-dione was reported with high potential toward CT-DNA binder. The solved XRD-structure of complex indicated a perfect regular square-planer geometry around the Cu(II) center. The trans/cis-DFT-isomerization calculation supported the XRD seen in reflecting the trans-isomer as the kinetic-favor isomer. The desired complex structure was also characterized by conductivity measurement, CHN-elemental analyses, MS, EDX, SEM, UV-Vis., FT-IR, HAS and TG/DTG. The Solvatochromism behavior of the complex was evaluated using four different polar solvents. MPE and Hirshfeld surface analysis (HSA) come to an agreement that fluoride and thiophene protons atoms are with suitable electro-potential environment to form non-classical H-bonds of type CThsbnd H⋯F. The DNA-binding properties were investigated by viscosity tests and spectrometric titrations, the results revealed the complex as strong calf-thymus DNA binder. High intrinsic-binding constants value ∼1.8 × 105 was collected.

1D cyanide complexes with 2-pyridinemethanol: Synthesis, crystal structures and spectroscopic properties

NASA Astrophysics Data System (ADS)

Sayın, Elvan; Kürkçüoğlu, Güneş Süheyla; Yeşilel, Okan Zafer; Hökelek, Tuncer

2015-12-01

Two new one-dimensional coordination polymers, [Cu(hmpH)2Pd(μ-CN)2(CN)2]n (1) and [Cu(hmpH)2Pt(μ-CN)2(CN)2]n (2), (hmpH = 2-pyridinemethanol), have been synthesized and characterized by vibrational (FT-IR and Raman) spectroscopy, single crystal X-ray diffraction, thermal and elemental analyses techniques. Single crystal X-ray diffraction analysis indicates that complexes 1 and 2 are isomorphous and isostructural, and crystallize in the triclinic system and P-1 space group. The Pd(II) or Pt(II) ions are four coordinated with four cyanide-carbon atoms in a square planar geometry. Cu(II) ion displays a distorted octahedral coordination by two N-atoms and two O-atoms of hmpH ligands, two bridging cyanide groups. In one dimensional structure of the complexes, [M(CN)4]2- (M = Pd(II) or Pt(II)) anions and [Cu(hmpH)2]2+ cations are linked via bridging cyanide ligands. In the complexes, the presence of intramolecular C-H⋯M (M = Pd(II) or Pt(II)) interactions with distance values of 3.00-2.95 Å are established, respectively.

Quantum chemical study, spectroscopic investigations, NBO and HOMO-LUMO analyses of 3-aminoquinoline (3AQ) and [Ag(3AQ)2(TCA)] complex (TCA = Trichloroacetate)

NASA Astrophysics Data System (ADS)

Soliman, Saied M.; Kassem, Taher S.; Badr, Ahmed M. A.; Abu Youssef, Morsy A.; Assem, Rania

2014-09-01

The new [Ag(3AQ)2(TCA)]; (3AQ = 3-aminoquinoline and TCA = Trichloroacetate) complex is synthesized and characterized using elemental analysis, FTIR, NMR and mass spectroscopy. The molecular geometry, vibrational frequencies, gauge-including atomic orbital (GIAO) 1H chemical shift values of the free and coordinated 3AQ in the ground state have been calculated by using DFT/B3LYP method. The TD-DFT results of the [Ag(3AQ)2(TCA)] complex showed a π-π* transition band at 240.3-242.6 nm (f = 0.1334-0.1348) which has longer wavelength and lower absorption intensity than that for the free 3AQ (233.2 nm, f = 0.3958). Dipole moment, polarizability and HOMO-LUMO gap values predicted better nonlinear optical properties (NLO) for the [Ag(3AQ)2(TCA)] than the 3AQ ligand. NBO analysis has been used to predict the most accurate Lewis structure of the studied molecules. The energies of the different intramolecular charge transfer (ICT) interactions within the studied molecules were estimated using second order perturbation theory.

Synthesis, characterization and electrochemical investigations of mixed-ligand copper(II)-organic supramolecular frameworks

NASA Astrophysics Data System (ADS)

Singh, Sandeep K.; Srivastava, Ashish Kumar; Srivastava, Krishna; Banerjee, Rahul; Prasad, Jagdish

2017-11-01

Two mixed-ligand copper(II)-organic coordination compounds with 5,5‧-dimethyl-2,2‧-bipyridine (5,5‧-Me2bpy) as a primary ligand while aliphatic malonate (Hmal) and aromatic 2-hydroxynicotinate (2-OHNA) as secondary ligands, were synthesized. These complexes are formulated as: [Cu(Hmal)(5,5‧-Me2bpy)(H2O)](ClO4) 1 and [Cu2(2-OHNA)2(5,5‧-Me2bpy)2(NO3)](NO3) 2. These two complexes were structurally characterized by single crystal X-ray diffraction analysis. Characterization was further supported by powder X-ray diffraction analysis, elemental analyses, FT-IR, FAB-MASS and TGA, DSC studies. Cyclic voltammetric and UV-visible spectral studies of these two complexes have also been done. The electrochemical studies of complex 1 in DMSO and DMF have shown that this complex undergoes quasi-reversible diffusion-controlled one-electron transfer reaction without any chemical complication while complex 2 in DMSO undergoes quasi-reversible diffusion-controlled one electron transfer reaction, following EC mechanism. The electrochemical behaviour of complex 2 in DMF is complicated probably due to presence of more than one species in solution phase.

Structural, antimicrobial and computational characterization of 1-benzoyl-3-(5-chloro-2-hydroxyphenyl)thiourea.

PubMed

Atiş, Murat; Karipcin, Fatma; Sarıboğa, Bahtiyar; Taş, Murat; Çelik, Hasan

2012-12-01

A new thiourea derivative, 1-benzoyl-3-(5-chloro-2-hydroxyphenyl)thiourea (bcht) has been synthesized from the reaction of 2-amino-4-chlorophenol with benzoyl isothiocyanate. The title compound has been characterized by elemental analyses, FT-IR, (13)C, (1)H NMR spectroscopy and the single crystal X-ray diffraction analysis. The structure of bcht derived from X-ray diffraction of a single crystal has been presented. The structural and spectroscopic data of the molecule in the ground state were calculated by using density functional method using 6-311++G(d,p) basis set. The complete assignments of all vibrational modes were performed on the basis of the total energy distributions (TED). Isotropic chemical shifts ((13)C NMR and (1)H NMR) were calculated using the gauge-invariant atomic orbital (GIAO) method. Theoretical calculations of bond parameters, harmonic vibration frequencies and nuclear magnetic resonance are in good agreement with experimental results. The UV absorption spectra of the compound that dissolved in ACN and MeOH were recorded. Bcht was also screened for antimicrobial activity against pathogenic bacteria and fungi. Copyright © 2012 Elsevier B.V. All rights reserved.

Lysine-Grafted MCM-41 Silica as an Antibacterial Biomaterial.

PubMed

Villegas, María F; Garcia-Uriostegui, Lorena; Rodríguez, Ofelia; Izquierdo-Barba, Isabel; Salinas, Antonio J; Toriz, Guillermo; Vallet-Regí, María; Delgado, Ezequiel

2017-09-26

This paper proposes a facile strategy for the zwitterionization of bioceramics that is based on the direct incorporation of l-lysine amino acid via the ε-amino group onto mesoporous MCM-41 materials. Fourier transform infrared (FTIR) studies of lysine-grafted MCM-41 (MCM-LYS) simultaneously showed bands at 3080 and 1540 cm -1 and bands at 1625 and 1415 cm -1 corresponding to -NH 3+ /COO - pairs, which demonstrate the incorporation of the amino acid on the material surface keeping its zwitterionic character. Both elemental and thermogravimetric analyses showed that the amount of grafted lysine was 8 wt. % based on the bioceramic total weight. Moreover, MCM-LYS exhibited a reduction of adhesion of S. aureus and E. coli bacteria in 33% and 50%, respectively at physiological pH, as compared with pristine MCM-41. Biofilm studies onto surfaces showed that lysine functionalization elicited a reduction of the area covered by S. aureus biofilm from 42% to only 5% (88%). This research shows a simple and effective approach to chemically modify bioceramics using single amino acids that provides zwitterionic functionality, which is useful to develop new biomaterials that are able to resist bacterial adhesion.

Lysine-Grafted MCM-41 Silica as an Antibacterial Biomaterial

PubMed Central

Villegas, María F.; Garcia-Uriostegui, Lorena; Rodríguez, Ofelia; Izquierdo-Barba, Isabel; Salinas, Antonio J.; Toriz, Guillermo; Vallet-Regí, María; Delgado, Ezequiel

2017-01-01

This paper proposes a facile strategy for the zwitterionization of bioceramics that is based on the direct incorporation of l-lysine amino acid via the ε-amino group onto mesoporous MCM-41 materials. Fourier transform infrared (FTIR) studies of lysine-grafted MCM-41 (MCM-LYS) simultaneously showed bands at 3080 and 1540 cm−1 and bands at 1625 and 1415 cm−1 corresponding to -NH3+/COO− pairs, which demonstrate the incorporation of the amino acid on the material surface keeping its zwitterionic character. Both elemental and thermogravimetric analyses showed that the amount of grafted lysine was 8 wt. % based on the bioceramic total weight. Moreover, MCM-LYS exhibited a reduction of adhesion of S. aureus and E. coli bacteria in 33% and 50%, respectively at physiological pH, as compared with pristine MCM-41. Biofilm studies onto surfaces showed that lysine functionalization elicited a reduction of the area covered by S. aureus biofilm from 42% to only 5% (88%). This research shows a simple and effective approach to chemically modify bioceramics using single amino acids that provides zwitterionic functionality, which is useful to develop new biomaterials that are able to resist bacterial adhesion. PMID:28952559

Complexes of platinum and palladium with β-diketones and DMSO: Synthesis, characterization, molecular modeling, and biological studies

NASA Astrophysics Data System (ADS)

do Couto Almeida, J.; Marzano, I. M.; de Paula, F. C. Silva; Pivatto, M.; Lopes, N. P.; de Souza, P. C.; Pavan, F. R.; Formiga, A. L. B.; Pereira-Maia, E. C.; Guerra, W.

2014-10-01

This work reports on the synthesis and characterization of new complexes of the type [MCl(L)DMSO], where L = 4,4,4-trifluoro-1-phenyl-1,3-butanedione (HTPB) or 4,4,4-trifluoro-1-(2-thienyl)-1,3-butanedione (HTTA) and M = Pt2+ or Pd2+. These complexes were characterized by elemental analyses, conductivity measurements, FT-IR, UV-Vis, high-resolution mass spectra (HRESIMS) and TG/DTA. In the complexes, the metallic ions bind to β-diketone via the oxygen atoms and to DMSO molecule via sulfur atom. The structures of complexes were optimized and theoretical data showed good agreement with the experimental results. The cytotoxic activity of the compounds was evaluated in a chronic myelogenous leukemia cell line. The platinum complexes were more cytotoxic than the free ligands and carboplatin and are promising candidates for further investigations. As example, the compound [PtCl(TPB)(DMSO)] inhibits the growth of K562 cells with an IC50 value equal to 2.5 μM. Furthermore, microbiological assays against Mycobacterium tuberculosis showed that all complexes exhibit low cytotoxicity against this bacterial strain while the free ligands exhibited MIC values of approximately 10 μg mL-1.

In vitro testing of curcumin based composites coatings as antitumoral systems against osteosarcoma cells

NASA Astrophysics Data System (ADS)

Tirca, I.; Mitran, V.; Marascu, V.; Brajnicov, S.; Ion, V.; Stokker-Cheregi, F.; Popovici, I. A.; Cimpean, A.; Dinca, V.; Dinescu, M.

2017-12-01

In this work, we propose a new design for biodegradable composite coatings obtained by laser methods, which are aimed at evaluating the effects of active antitumoral elements on osteosarcoma cells. Our approach relies on embedding curcumin, which is a natural polyphenol having antitumoral properties, within biodegradable copolymer coatings (i.e. polyvinyl alcohol-polyethylene glycol - PVA-PEG) by using matrix assisted pulsed laser evaporation (MAPLE). The structural and morphological characteristics of the coatings were tailored by using different solvents (water, ethanol, benzene, dimethylsufoxide) as deposition matrix. The morphological characteristics of the resulting films were investigated by atomic force microscopy (AFM), whereas their chemical composition was characterized by Fourier transform infrared spectroscopy (FTIR). These characteristics were correlated with the degradation behavior by using ellipsometry (SE) and AFM measurements data. The in vitro study of the MG-63 osteosarcoma cell behavior indicates that the developed hybrid coatings significantly decreased osteosarcoma cell viability and proliferation potential. The physico-chemical characteristics of the thin films, along with the preliminary in vitro analyses, suggest that our developed polymeric hybrid coatings represent an efficient way to tackle the design of antitumoral surfaces, with applications in biomedicine.

Structure investigation of three hydrazones Schiff's bases by spectroscopic, thermal and molecular orbital calculations and their biological activities

NASA Astrophysics Data System (ADS)

Belal, Arafa A. M.; Zayed, M. A.; El-Desawy, M.; Rakha, Sh. M. A. H.

2015-03-01

Three Schiff's bases AI (2(1-hydrazonoethyl)phenol), AII (2, 4-dibromo 6-(hydrazonomethyl)phenol) and AIII (2(hydrazonomethyl)phenol) were prepared as new hydrazone compounds via condensation reactions with molar ratio (1:1) of reactants. Firstly by reaction of 2-hydroxy acetophenone solution and hydrazine hydrate; it gives AI. Secondly condensation between 3,5-dibromo-salicylaldehyde and hydrazine hydrate gives AII. Thirdly condensation between salicylaldehyde and hydrazine hydrate gives AIII. The structures of AI-AIII were characterized by elemental analysis (EA), mass (MS), FT-IR and 1H NMR spectra, and thermal analyses (TG, DTG, and DTA). The activation thermodynamic parameters, such as, ΔE∗, ΔH∗, ΔS∗ and ΔG∗ were calculated from the TG curves using Coats-Redfern method. It is important to investigate their molecular structures to know the active groups and weak bond responsible for their biological activities. Consequently in the present work, the obtained thermal (TA) and mass (MS) practical results are confirmed by semi-empirical MO-calculations (MOCS) using PM3 procedure. Their biological activities have been tested in vitro against Escherichia coli, Proteus vulgaris, Bacillissubtilies and Staphylococcus aurous bacteria in order to assess their anti-microbial potential.

Wood digestion in Pselactus spadix Herbst--a weevil attacking marine timber structures.

PubMed

Oevering, Pascal; Pitman, Andrew J; Pandey, Krishna K

2003-04-01

Pselactus spadix tunnels timber structures in the marine environment. Recent studies reported a cosmopolitan distribution for this weevil, which is frequently found in harbour and port areas. P. spadix feeds on timber (hardwood and softwood) in immature and adult life stages, but its digestion of wood components had not been investigated. Using dry weight analyses of tunnel walls and frass produced, P. spadix adults consumed Scots pine with soft rot decay at a rate of 1.59 +/- 0.37 mg d-1 and the digestibility of this substrate was 57.96 +/- 5.89 (i.e. for 100 mg consumed SR-pine, 58 mg was digested). Using gravimetric analysis to quantify structural wood components in tunnel walls and frass, P. spadix adults were found to digest cellulose, lignin and hemicellulose with digestibility coefficients of 82.2, 41.2 and 14.5 respectively. Fourier Transform Infrared (FTIR) spectroscopy analyses of tunnel walls and frass of adults and larvae from soft rotted pine also indicated digestion of all structural components, with larvae digesting cellulose and lignin more efficiently than adults. When FTIR was employed to analyse adult tunnel walls and frass from undecayed pine, cellulose and hemicellulose were digested, but no evidence of lignin digestion was found. This study shows that adults digest lignin when soft rot is present and suggests a symbiotic function of wood degrading microorganisms.

Characterisation of silica derived from rice husk (Muar, Johor, Malaysia) decomposition at different temperatures

NASA Astrophysics Data System (ADS)

Azmi, M. A.; Ismail, N. A. A.; Rizamarhaiza, M.; W. M. Hasif. A. A., K.; Taib, H.

2016-07-01

Rice husk was thermally decomposed to yield powder composed of silica (SiO2). Temperatures of 700°C and 1000°C were chosen as the decomposition temperatures. X-Ray Diffraction (XRD), X-Ray Florescence (XRF), Fourier Transform Infrared (FTIR), and Field Emission Scanning Electron Microscope (FESEM) analyses were conducted on a synthetic silica powder (SS-SiO2) and the rice husk ash as for the comparative characterisation study. XRD analyses clearly indicated that the decomposed rice husk yielded silica of different nature which are Crystalline Rice Husk Silica (C-RHSiO2) and Amorphous Rice Husk Silica (A-RHSiO2). Moreover, it was found that SS-SiO2 was of Quartz phase, C-RHSiO2 was of Trydimite and Cristobalite. Through XRF detection, the highest SiO2 purity was detected in SS-SiO2 followed by C-RHSiO2 and A-RHSiO2 with purity percentages of 99.60%, 82.30% and 86.30% respectively. FTIR results clearly indicated silica (SiO2) bonding 1056, 1064, 1047, 777, 790 and 798 cm-1) increased as the crystallinity silica increased. The Cristobalite phase was detected in C-RH SiO2 at the wavelength of 620 cm-1. Morphological features as observed by FESEM analyses confirmed that, SS-SiO2 and C-RH SiO2 showed prominent coarse granular morphology.

Experimental development of a new protocol for extraction and characterization of microplastics in fish tissues: First observations in commercial species from Adriatic Sea.

PubMed

Avio, Carlo Giacomo; Gorbi, Stefania; Regoli, Francesco

2015-10-01

The presence of microplastics in the marine environment has raised scientific interest during the last decade. Several organisms can ingest microplastics with potentially adverse effects on the digestive tract, respiratory system and locomotory appendages. However, a clear evidence of tissue accumulation and transfer of such microparticles in wild organisms is still lacking, partially hampered by technical difficulties in isolation and characterization protocols from biological samples. In this work, we compared the efficacy of some existing approaches and we optimized a new protocol allowing an extraction yield of microplastics from fish tissues ranging between 78% and 98%, depending on the polymer size. FT-IR analyses confirmed that the extraction procedure did not affect the particles characteristics. The method was further validated on the fish mullet, Mugil cephalus, exposed under laboratory conditions to polystyrene and polyethylene; the particles were isolated and quantified in stomach and liver, and their presence in the hepatic tissue was confirmed also by histological analyses. A preliminary characterization revealed the presence and distribution of microplastics in various fish species collected along the Adriatic Sea. FT-IR analyses indicated polyethylene as the predominant polymer (65%) in the stomach of fish. The overall results confirmed the newly developed method as a reliable approach to detect and quantify microplastics in the marine biota. Copyright © 2015 Elsevier Ltd. All rights reserved.

[Analysis of 14 elements for Jinhua bergamot by X-ray fluorescence spectrometry and elemental analyser].

PubMed

Wang, Zhi-gang; Yu, Hong-mei

2012-01-01

The content of the elements C, H, O and N in Jinhua bergamot was analysed by using Vario III elemental analyser, the bergamot sample was scanned by using X-ray fluorescence spectrometer with PW2400 wavelength dispersion, and the content of the elements Mg, Al, P, S, Cl, K, Ca, Mn, Fe and Sr was analysed by using IQ+ analytical method. It turned out that the result is more ideal if the content of the elements C, H, O and N is processed as fix phase, and the analytical result is more ideal if, to prevent the sample skin from coming off, the sample is wrapped with mylar film with the film coefficient adjusted.

High resolution analysis of the FTIR spectra of trifluoroamine NF3

NASA Astrophysics Data System (ADS)

Bolotova, I. B.; Ulenikov, O. N.; Bekhtereva, E. S.; Albert, S.; Bauerecker, S.; Hollenstein, H.; Lerch, Ph.; Quack, M.; Peter, T.; Seyfang, G.; Wokaun, A.

2018-06-01

We report high resolution Fourier Transform Infrared (FTIR) spectra of nitrogen trifluoride (trifluoroamine, NF3) measured with the Zürich Bruker prototype spectrometer (ZP 2001) and the SLS THz/FTIR setup (2009 prototype) in the range 20-3000 cm-1 at temperatures between 80 and 120 K using a collisional cooling cell designed with White cell multipath reflection optics and at room temperature (296 K). Except in the far-infrared with instrument limited resolution (Δν˜FWHM = 0.0008 cm-1) many of the spectra are nearly Doppler limited. Rovibrational transitions were assigned to 13 different vibrational bands and were used then in the fitting procedure. We re-investigated the bands 2ν4,ν1,ν2 +ν4,ν1 +ν4 , 2ν3 and ν1 +ν3 , which had been studied before, and we have analyzed the ν2 +ν3 , 2ν1,ν1 +ν2 +ν4,ν1 +ν2 +ν3,ν2 + 2ν3, 3ν3,ν1 + 2ν3 bands for the first time. All our analyses refer to the isotopomer 14 NF3.

Infrared Spectroscopy as a Tool to Study the Antioxidant Activity of Polyphenolic Compounds in Isolated Rat Enterocytes

PubMed Central

Barraza-Garza, Guillermo; Castillo-Michel, Hiram; de la Rosa, Laura A.; Martinez-Martinez, Alejandro; Pérez-León, Jorge A.; Cotte, Marine; Alvarez-Parrilla, Emilio

2016-01-01

The protective effect of different polyphenols, catechin (Cat), quercetin (Qc) (flavonoids), gallic acid (GA), caffeic acid (CfA), chlorogenic acid (ChA) (phenolic acids), and capsaicin (Cap), against H2O2-induced oxidative stress was evaluated in rat enterocytes using Attenuated Total Reflectance-Fourier Transform Infrared (ATR-FTIR) Spectroscopy and Fourier Transform Infrared Microspectroscopy (FTIRM), and results were compared to standard lipid peroxidation techniques: conjugated dienes (CD) and Thiobarbituric Acid Reactive Substances (TBARS). Analysis of ATR-FTIR and FTIRM spectral data allowed the simultaneous evaluation of the effects of H2O2 and polyphenols on lipid and protein oxidation. All polyphenols showed a protective effect against H2O2-induced oxidative stress in enterocytes, when administered before or after H2O2. Cat and capsaicin showed the highest protective effect, while phenolic acids had weaker effects and Qc presented a mild prooxidative effect (IR spectral profile of biomolecules between control and H2O2-treated cells) according to FTIR analyses. These results demonstrated the viability to use infrared spectroscopy to evaluate the oxidant and antioxidant effect of molecules in cell systems assays. PMID:27213031

A rapid ATR-FTIR spectroscopic method for detection of sibutramine adulteration in tea and coffee based on hierarchical cluster and principal component analyses.

PubMed

Cebi, Nur; Yilmaz, Mustafa Tahsin; Sagdic, Osman

2017-08-15

Sibutramine may be illicitly included in herbal slimming foods and supplements marketed as "100% natural" to enhance weight loss. Considering public health and legal regulations, there is an urgent need for effective, rapid and reliable techniques to detect sibutramine in dietetic herbal foods, teas and dietary supplements. This research comprehensively explored, for the first time, detection of sibutramine in green tea, green coffee and mixed herbal tea using ATR-FTIR spectroscopic technique combined with chemometrics. Hierarchical cluster analysis and PCA principle component analysis techniques were employed in spectral range (2746-2656cm -1 ) for classification and discrimination through Euclidian distance and Ward's algorithm. Unadulterated and adulterated samples were classified and discriminated with respect to their sibutramine contents with perfect accuracy without any false prediction. The results suggest that existence of the active substance could be successfully determined at the levels in the range of 0.375-12mg in totally 1.75g of green tea, green coffee and mixed herbal tea by using FTIR-ATR technique combined with chemometrics. Copyright © 2017 Elsevier Ltd. All rights reserved.

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

PubMed

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

2006-03-01

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

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

PubMed

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

2016-06-01

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

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

NASA Astrophysics Data System (ADS)

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

2018-01-01

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

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

NASA Astrophysics Data System (ADS)

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

2015-01-01

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

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

NASA Astrophysics Data System (ADS)

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

2015-02-01

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

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

NASA Astrophysics Data System (ADS)

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

2011-09-01

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

Sustainable conversion of agro-wastes into useful adsorbents

NASA Astrophysics Data System (ADS)

Bello, Olugbenga Solomon; Owojuyigbe, Emmanuel Seun; Babatunde, Monsurat Abiodun; Folaranmi, Folasayo Eunice

2017-11-01

Preparation and characterization of raw and activated carbon derived from three different selected agricultural wastes: kola nut pod raw and activated (KNPR and KNPA), bean husk raw and activated (BHR and BHA) and coconut husk raw and activated (CHR and CHA) were investigated, respectively. Influences of carbonization and acid activation on the activated carbon were investigated using SEM, FTIR, EDX, pHpzc and Boehm titration techniques, respectively. Carbonization was done at 350 °C for 2 h followed by activation with 0.3 M H3PO4 (ortho-phosphoric acid). Results obtained from SEM, FTIR, and EDX revealed that, carbonization followed by acid activation had a significant influence on morphology and elemental composition of the samples. SEM showed well-developed pores on the surface of the precursors after acid treatment, FTIR spectra revealed reduction, broadening, disappearance or appearance of new peaks after acid activation. EDX results showed highest percentage of carbon by atom respectively in the order BHA > KNPA > CHA respectively. The pHpzc was found to be 5.32, 4.57 and 3.69 for KNPA, BHA and CHA, respectively. Boehm titration result compliments that of pHpzc, indicating that the surfaces of the prepared adsorbents are predominantly acidic. This study promotes a sustainable innovative use of agro-wastes in the production of cheap and readily available activated carbons, thereby ensuring more affordable water and effluent treatment adsorbents.

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

NASA Astrophysics Data System (ADS)

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

2018-05-01

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

Noninvasive Spatially Offset and Transmission Raman Mapping of Breast Tissue: A Multimodal Approach Towards the In Vivo assessment of Tissue Pathology

DTIC Science & Technology

2013-04-01

liquid nitrogen cooled mercury cadmium telluride ( MCT ) detector and compare their performance to a commercial FT-IR imaging instrument. We examine the...telluride ( MCT ) detector (InfraRed Associates, Stuart, FL), and in a second widefield imaging configuration, we employed a cooled focal plane array (FPA...experiment, a cooled focal plane array (FPA) was substituted for the bolometer. (b) A cooled single-element MCT detector is utilized with an adjustable

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

PubMed

Hotzel, Konrad; Heinze, Thomas

2016-11-03

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

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

NASA Astrophysics Data System (ADS)

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

2015-11-01

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

Finite Element Analysis of a NASA National Transonic Facility Wind Tunnel Balance

NASA Technical Reports Server (NTRS)

Lindell, Michael C.

1996-01-01

This paper presents the results of finite element analyses and correlation studies performed on a NASA National Transonic Facility (NTF) Wind Tunnel balance. In the past NASA has relied primarily on classical hand analyses, coupled with relatively large safety factors, for predicting maximum stresses in wind tunnel balances. Now, with the significant advancements in computer technology and sophistication of general purpose analysis codes, it is more reasonable to pursue finite element analyses of these balances. The correlation studies of the present analyses show very good agreement between the analyses and data measured with strain gages and therefore the studies give higher confidence for using finite element analyses to analyze and optimize balance designs in the future.

Finite Element Analysis of a NASA National Transonic Facility Wide Tunnel Balance

NASA Technical Reports Server (NTRS)

Lindell, Michael C. (Editor)

1999-01-01

This paper presents the results of finite element analyses and correlation studies performed on a NASA National Transonic Facility (NTF) Wind Tunnel balance. In the past NASA has relied primarily on classical hand analyses, coupled with relatively large safety factors, for predicting maximum stresses in wind tunnel balances. Now, with the significant advancements in computer technology and sophistication of general purpose analysis codes, it is more reasonable to pursue finite element analyses of these balances. The correlation studies of the present analyses show very good agreement between the analyses and data measured with strain gages and therefore the studies give higher confidence for using finite element analyses to analyze and optimize balance designs in the future.

Synthesis of mesoporous silica-coated magnetic nanoparticles modified with 4-amino-3-hydrazino-5-mercapto-1,2,4-triazole and its application as Cu(II) adsorbent from aqueous samples

NASA Astrophysics Data System (ADS)

Wondracek, Marcos Henrique P.; Jorgetto, Alexandre Oliveira; Silva, Adrielli Cristina P.; Ivassechen, Janaíne do Rocio; Schneider, José Fabián; Saeki, Margarida Juri; Pedrosa, Valber Albuquerque; Yoshito, Walter Kenji; Colauto, Fabiano; Ortiz, Wilson A.; Castro, Gustavo Rocha

2016-03-01

This study presents an alternative, rapid, and environment-friendly synthesis procedure of a magnetic core-shell mesoporous SBA-15 silica composite, its functionalization with 4-amino-3-hydrazino-5-mercapto-1,2,4-triazole (Purpald), and its application in dispersive solid-phase microextraction (DSPME) for Cu(II) from water. The materials were characterized through magnetization measurements, scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HR-TEM), Fourier transform infrared (FTIR), nuclear magnetic resonance (NMR) of 29Si and 13C, elemental analysis, and surface area measurements. FTIR and NMR analyses indicated the presence of the ligand on the functionalized material and that it was coupled through a Csbnd S bond. TEM images clearly show that the magnetite core particles were effectively coated with a silica shell. The material presented a surface area of 287.99 m2 g-1 and an average pore diameter of approximately 15.1 nm. The material had its point of zero charge (PZC) determined (6.17) and its adsorption capacity was evaluated as a function of time, pH, and metal concentration. Dynamic adsorption equilibrium was reached in 120 min, and it had a good correlation with the pseudo-second-order kinetic model (r2 = 0.9997). The maximum experimental adsorption capacity (0.0786 mmol g-1) and the value calculated by the linearized Langmuir model (0.0799 mmol g-1) are very approximate, indicating the formation of a monolayer over the material. Furthermore, the material proved to be very stable, because their adsorption capacity remained greater than 95% even after 10 cycles of adsorption/desorption. A high enrichment factor of 98.1-fold was observed, indicating that this material is suitable for the preconcentration of trace Cu(II) ions before analysis through flame atomic absorption spectrometry (FAAS).

[Preparation of porous ceramics based on waste ceramics and its Ni2+ adsorption characteristics].

PubMed

Zhang, Yong-Li; Wang, Cheng-Zhi; Shi, Ce; Shang, Ling-Ling; Ma, Rui; Dong, Wan-Li

2013-07-01

The preparation conditions of porous ceramics were determined by SEM, XRD and FT-IR characterizations as well as the nickel removal ability of porous ceramics to be: the mass fraction w of sesbania powder doped was 4%, and the calcination temperature was 800 degrees C. SEM and pore structure characterization illustrated that calcination caused changes in the structure and morphology of waste ceramics. With the increase of calcination temperature, the specific surface area and pore volume decreased, while the aperture increased. EDS analyses showed that the main elements of both the original waste porcelain powder and the porous ceramics were Si, Al and O. The SEM, XRD and FT-IR characterization of porous ceramics illustrated that the structure of porous ceramics was stable before and after adsorption. The series of experiments of Ni2+ adsorption using these porous ceramics showed that when the dosage of porous ceramics was 10 g x L(-1), the adsorption time was 60 min, the pH value was 6.32, and the concentration of nickel-containing wastewater was below 100 mg x L(-1), the Ni2+ removal of wastewater reached 89.7%. Besides, the porous ceramics showed higher removal efficiency on nickel in the wastewater. The Ni(2+)-containing wastewater was processed by the porous ceramics prepared, and the adsorption dynamics and adsorption isotherms of Ni2+ in wastewater by porous ceramics were investigated. The research results showed that the Ni2+ adsorption process of porous ceramics was in accordance with the quasi second-order kinetic model (R2 = 0.999 9), with Q(e) of 9.09 mg x g(-1). The adsorption process can be described by the Freundlich equation and Langmuir equation, and when the temperature increased from 20 degrees C to 40 degrees C, the maximum adsorption capacity Q(m) increased from 14.49 mg x g(-1) to 15.38 mg x g(-1).

Water in the Lithospheric Mantle Beneath a Phanerozoic Continental Belt: FTIR Analyses of Alligator Lake Xenoliths (Yukon, Canada)

NASA Technical Reports Server (NTRS)

Gelber, McKensie; Peslier, Ann H.; Brandon, Alan D.

2015-01-01

Water in the mantle influences melting, metasomatism, viscosity and electrical conductivity. The Alligator Lake mantle xenolith suite is one of three bimodal peridotite suites from the northern Canadian Cordillera brought to the surface by alkali basalts, i.e., it consists of chemically distinct lherzolites and harzburgites. The lherzolites have equilibration temperatures about 50 C lower than the harzburgites and are thought to represent the fertile upper mantle of the region. The harzburgites might have come from slightly deeper in the mantle and/or be the result of a melting event above an asthenospheric upwelling detected as a seismic anomaly at 400-500 km depth. Major and trace element data are best interpreted as the lherzolite mantle having simultaneously experienced 20-25% partial melting and a metasomatic event to create the harzburgites. Well-characterized xenoliths are being analyzed for water by FTIR. Harzburgites contain 29-52 ppm H2O in orthopyroxene (opx) and (is) approximately140 ppm H2O in clinopyroxene (cpx). The lherzolites have H2O contents of 27-150 ppm in opx and 46-361 ppm in cpx. Despite correlating with enrichments in LREE, the water contents of the harzburgite pyroxenes are low relative to those of typical peridotite xenoliths, suggesting that the metasomatic agents were water-poor, contrarily to what has been suggested before. The water content of cpx is about double that of opx indicating equilibrium. Olivine water contents are low ((is) less than 5 ppm H2O) and out of equilibrium with those of opx and cpx, which may be due to H loss during xenolith ascent. This is consistent with olivines containing more water in their cores than their rims. Olivines exclusively exhibit water bands in the 3400-3000 cm-1 range, which may be indicative of a reduced environment.

Molecular signatures of fossil leaves provide unexpected new evidence for extinct plant relationships.

PubMed

Vajda, Vivi; Pucetaite, Milda; McLoughlin, Stephen; Engdahl, Anders; Heimdal, Jimmy; Uvdal, Per

2017-08-01

Gene sequences form the primary basis for understanding the relationships among extant plant groups, but genetic data are unavailable from fossils to evaluate the affinities of extinct taxa. Here we show that geothermally resistant fossil cuticles of seed-bearing plants, analysed with Fourier transform infrared (FTIR) spectroscopy and hierarchical cluster analysis (HCA), retain biomolecular suites that consistently distinguish major taxa even after experiencing different diagenetic histories. Our results reveal that similarities between the cuticular biochemical signatures of major plant groups (extant and fossil) are mostly consistent with recent phylogenetic hypotheses based on molecular and morphological data. Our novel chemotaxonomic data also support the hypothesis that the extinct Nilssoniales and Bennettitales are closely allied, but only distantly related to Cycadales. The chemical signature of the cuticle of Czekanowskia (Leptostrobales) is strongly similar to that of Ginkgo leaves and supports a close evolutionary relationship between these groups. Finally, our results also reveal that the extinct putative araucariacean, Allocladus, when analysed through HCA, is grouped closer to Ginkgoales than to conifers. Thus, in the absence of modern relatives yielding molecular information, FTIR spectroscopy provides valuable proxy biochemical data complementing morphological characters to distinguish fossil taxa and to help elucidate extinct plant relationships.

Encapsulation of CO2 into amorphous alpha-cyclodextrin powder at different moisture contents - Part 2: Characterization of complexed powders and determination of crystalline structure.

PubMed

Ho, Thao M; Howes, Tony; Jack, Kevin S; Bhandari, Bhesh R

2016-09-01

This study aims to characterize CO2-α-cyclodextrin (α-CD) inclusion complexes produced from amorphous α-CD powder at moisture contents (MC) close to or higher than the critical level of crystallization (e.g. 13, 15 and 17% MC on wet basis, w.b.) at 0.4 and 1.6MPa pressure for 72h. The results of (13)C NMR, SEM, DSC and X-ray analyses showed that these MC levels were high enough to induce crystallization of CO2-α-CD complexed powders during encapsulation, by which amount of CO2 encapsulated by amorphous α-CD powder was significantly increased. The formation of inclusion complexes were well confirmed by results of FTIR and (13)C NMR analyses through an appearance of a peak associated with CO2 on the FTIR (2334cm(-1)) and NMR (125.3ppm) spectra. Determination of crystal packing patterns of CO2-α-CD complexed powders showed that during crystallization, α-CD molecules were arranged in cage-type structure in which CO2 molecules were entrapped in isolated cavities. Copyright © 2016 Elsevier Ltd. All rights reserved.

Solubility and dissolution performances of spray-dried solid dispersion of Efavirenz in Soluplus.

PubMed

Lavra, Zênia Maria Maciel; Pereira de Santana, Davi; Ré, Maria Inês

2017-01-01

Efavirenz (EFV), a first-line anti-HIV drug largely used as part of antiretroviral therapies, is practically insoluble in water and belongs to BCS class II (low solubility/high permeability). The aim of this study was to improve the solubility and dissolution performances of EFV by formulating an amorphous solid dispersion of the drug in polyvinyl caprolactam-polyvinyl acetate-polyethylene glycol graft copolymer (Soluplus ® ) using spray-drying technique. To this purpose, spray-dried dispersions of EFV in Soluplus ® at different mass ratios (1:1.25, 1:7, 1:10) were prepared and characterized using particle size measurements, SEM, XRD, DSC, FTIR and Raman microscopy mapping. Solubility and dissolution were determined in different media. Stability was studied at accelerated conditions (40 °C/75% RH) and ambient conditions for 12 months. DSC and XRD analyses confirmed the EFV amorphous state. FTIR spectroscopy analyses revealed possible drug-polymer molecular interaction. Solubility and dissolution rate of EFV was enhanced remarkably in the developed spray-dried solid dispersions, as a function of the polymer concentration. Spray-drying was concluded to be a proper technique to formulate a physically stable dispersion of amorphous EFV in Soluplus ® , when protected from moisture.

Green thermal-assisted synthesis and characterization of novel cellulose-Mg(OH)2 nanocomposite in PEG/NaOH solvent.

PubMed

Ponomarev, Nikolai; Repo, Eveliina; Srivastava, Varsha; Sillanpää, Mika

2017-11-15

Synthesis of nanocomposites was performed using microcrystalline cellulose (MCC), MgCl 2 in PEG/NaOH solvent by a thermal-assisted method at different temperatures by varying time and the amount of MCC. Results of XRD, FTIR, and EDS mapping showed that the materials consisted of only cellulose (CL) and magnesium hydroxide (MH). According to FTIR and XRD, it was found that crystallinity of MH in cellulose nanocomposites is increased with temperature and heating time and decreased with increasing of cellulose amount. The PEG/NaOH solvent has a significant effect on cellulose and Mg(OH) 2 morphology. BET and BJH results demonstrated the effects of temperature and cellulose amount on the pore size corresponding to mesoporous materials. TG and DTG analyses showed the increased thermal stability of cellulose nanocomposites with increasing temperature. TEM and SEM analyses showed an even distribution of MH nanostructures with various morphology in the cellulose matrix. The cellulose presented as the polymer matrix in the nanocomposites. It was supposed the possible interaction between cellulose and Mg(OH) 2 . The novel synthesis method used in this study is feasible, cost-efficient and environmentally friendly. Copyright © 2017 Elsevier Ltd. All rights reserved.

Synthesis, spectroscopic characterization, biological screenings, DNA binding study and POM analyses of transition metal carboxylates.

PubMed

Uddin, Noor; Sirajuddin, Muhammad; Uddin, Nizam; Tariq, Muhammad; Ullah, Hameed; Ali, Saqib; Tirmizi, Syed Ahmed; Khan, Abdur Rehman

2015-04-05

This article contains the synthesis of a novel carboxylic acid derivative, its transition metal complexes and evaluation of biological applications. Six carboxylate complexes of transition metals, Zn(II) and Hg(II), have been successfully synthesized and characterized by FT-IR and NMR (1H, 13C). The ligand, HL, (4-[(2,6-Diethylphenyl)amino]-4-oxobutanoic acid) was also characterized by single crystal X-ray analysis. The complexation occurs via oxygen atoms of the carboxylate moiety. FT-IR date show the bidentate nature of the carboxylate moiety of the ligand as the Δν value in all complexes is less than that of the free ligand. The ligand and its complexes were screened for antifungal and antileishmanial activities. The results showed that the ligand and its complexes are active with few exceptions. UV-visible spectroscopy and viscometry results reveal that the ligand and its complexes interact with the DNA via intercalative mode of interaction. A new and efficient strategy to identify the pharmacophores and anti-pharmacophores sites in carboxylate derivatives for the antibacterial/antifungal activity using Petra, Osiris and Molinspiration (POM) analyses was also carried out. Copyright © 2014 Elsevier B.V. All rights reserved.

Synthesis, spectroscopic characterization, biological screenings, DNA binding study and POM analyses of transition metal carboxylates

NASA Astrophysics Data System (ADS)

Uddin, Noor; Sirajuddin, Muhammad; Uddin, Nizam; Tariq, Muhammad; Ullah, Hameed; Ali, Saqib; Tirmizi, Syed Ahmed; Khan, Abdur Rehman

2015-04-01

This article contains the synthesis of a novel carboxylic acid derivative, its transition metal complexes and evaluation of biological applications. Six carboxylate complexes of transition metals, Zn(II) and Hg(II), have been successfully synthesized and characterized by FT-IR and NMR (1H, 13C). The ligand, HL, (4-[(2,6-Diethylphenyl)amino]-4-oxobutanoic acid) was also characterized by single crystal X-ray analysis. The complexation occurs via oxygen atoms of the carboxylate moiety. FT-IR date show the bidentate nature of the carboxylate moiety of the ligand as the Δν value in all complexes is less than that of the free ligand. The ligand and its complexes were screened for antifungal and antileishmanial activities. The results showed that the ligand and its complexes are active with few exceptions. UV-visible spectroscopy and viscometry results reveal that the ligand and its complexes interact with the DNA via intercalative mode of interaction. A new and efficient strategy to identify the pharmacophores and anti-pharmacophores sites in carboxylate derivatives for the antibacterial/antifungal activity using Petra, Osiris and Molinspiration (POM) analyses was also carried out.

Biogeochemical Typing of Paddy Field by a Data-Driven Approach Revealing Sub-Systems within a Complex Environment - A Pipeline to Filtrate, Organize and Frame Massive Dataset from Multi-Omics Analyses

PubMed Central

Ogawa, Diogo M. O.; Moriya, Shigeharu; Tsuboi, Yuuri; Date, Yasuhiro; Prieto-da-Silva, Álvaro R. B.; Rádis-Baptista, Gandhi; Yamane, Tetsuo; Kikuchi, Jun

2014-01-01

We propose the technique of biogeochemical typing (BGC typing) as a novel methodology to set forth the sub-systems of organismal communities associated to the correlated chemical profiles working within a larger complex environment. Given the intricate characteristic of both organismal and chemical consortia inherent to the nature, many environmental studies employ the holistic approach of multi-omics analyses undermining as much information as possible. Due to the massive amount of data produced applying multi-omics analyses, the results are hard to visualize and to process. The BGC typing analysis is a pipeline built using integrative statistical analysis that can treat such huge datasets filtering, organizing and framing the information based on the strength of the various mutual trends of the organismal and chemical fluctuations occurring simultaneously in the environment. To test our technique of BGC typing, we choose a rich environment abounding in chemical nutrients and organismal diversity: the surficial freshwater from Japanese paddy fields and surrounding waters. To identify the community consortia profile we employed metagenomics as high throughput sequencing (HTS) for the fragments amplified from Archaea rRNA, universal 16S rRNA and 18S rRNA; to assess the elemental content we employed ionomics by inductively coupled plasma optical emission spectroscopy (ICP-OES); and for the organic chemical profile, metabolomics employing both Fourier transformed infrared (FT-IR) spectroscopy and proton nuclear magnetic resonance (1H-NMR) all these analyses comprised our multi-omics dataset. The similar trends between the community consortia against the chemical profiles were connected through correlation. The result was then filtered, organized and framed according to correlation strengths and peculiarities. The output gave us four BGC types displaying uniqueness in community and chemical distribution, diversity and richness. We conclude therefore that the BGC typing is a successful technique for elucidating the sub-systems of organismal communities with associated chemical profiles in complex ecosystems. PMID:25330259

Biogeochemical typing of paddy field by a data-driven approach revealing sub-systems within a complex environment--a pipeline to filtrate, organize and frame massive dataset from multi-omics analyses.

PubMed

Ogawa, Diogo M O; Moriya, Shigeharu; Tsuboi, Yuuri; Date, Yasuhiro; Prieto-da-Silva, Álvaro R B; Rádis-Baptista, Gandhi; Yamane, Tetsuo; Kikuchi, Jun

2014-01-01

We propose the technique of biogeochemical typing (BGC typing) as a novel methodology to set forth the sub-systems of organismal communities associated to the correlated chemical profiles working within a larger complex environment. Given the intricate characteristic of both organismal and chemical consortia inherent to the nature, many environmental studies employ the holistic approach of multi-omics analyses undermining as much information as possible. Due to the massive amount of data produced applying multi-omics analyses, the results are hard to visualize and to process. The BGC typing analysis is a pipeline built using integrative statistical analysis that can treat such huge datasets filtering, organizing and framing the information based on the strength of the various mutual trends of the organismal and chemical fluctuations occurring simultaneously in the environment. To test our technique of BGC typing, we choose a rich environment abounding in chemical nutrients and organismal diversity: the surficial freshwater from Japanese paddy fields and surrounding waters. To identify the community consortia profile we employed metagenomics as high throughput sequencing (HTS) for the fragments amplified from Archaea rRNA, universal 16S rRNA and 18S rRNA; to assess the elemental content we employed ionomics by inductively coupled plasma optical emission spectroscopy (ICP-OES); and for the organic chemical profile, metabolomics employing both Fourier transformed infrared (FT-IR) spectroscopy and proton nuclear magnetic resonance (1H-NMR) all these analyses comprised our multi-omics dataset. The similar trends between the community consortia against the chemical profiles were connected through correlation. The result was then filtered, organized and framed according to correlation strengths and peculiarities. The output gave us four BGC types displaying uniqueness in community and chemical distribution, diversity and richness. We conclude therefore that the BGC typing is a successful technique for elucidating the sub-systems of organismal communities with associated chemical profiles in complex ecosystems.

A little adjustment of synthetic strategy led to a new highly repeated heteropolyblue: Structure, characterizations and photocatalytic properties

NASA Astrophysics Data System (ADS)

Chen, Wu-Hua; Zhang, Zhu-Sen; Zhao, Jin-Hua; Qiu, Ze-Hai; Yuan, Qiu-Lan; Huang, Tian-Fu; Lin, Xue-Yu; Hu, Zhi-Biao

2017-06-01

Hydrothermal synthesis is known as the most efficient method to prepare novel structural polyoxometalate (POM)-based materials, but controlled synthesis of a structure-directing POM is always challenging task. The experimental repeatability is usually one of the key topics. To explore a reliable hydrothermal synthesis approach for new POMs will be a meaningful work. Our previous work, which we have hydrothermally synthesized the first Cr-complexes-capped Keggin-type POM, [Hdma]3[H2phen]{[Cr(phen)]2[MoV8MoVI4O36(PO4)]}·nH2O (n ≈ 2) (Chen et al., polyhedron, 2015, 85, 117), afford us some commendable synthetic experiences, arouse us some introspections as well for its tricky preparation conditions and low experimental repeatability. Based on the aforementioned work, a new high-repetition-rate and more steady heteropolyblue, [H3O]0.5(Hdma)2.5(dma)0.25{[Cr(phen)]2[MoV6MoVI6O8(PO4)]}·2H2O (1) (dma = dimethylamine (C2H7N), phen = 1,10-phenanthroline (C12H8N2)), has been successfully obtained by virtue of reasonably adjusting synthetic strategy. The adjustment of synthetic strategy includes controlling ratio of reactants and aging time, reasonably using redoxes and stepwise self-assembly plans. Compound 1 is the second POM with Keggin-type polyanion capped by Cr-complexes. Experiments demonstrate that compound 1 has good catalytic activity in the both degradation reactions of rhodamine B (RHB) and methyl orange (MO) under ultraviolet (UV)-light and oxidant H2O2 conditions. Detailed structural characterizations include single-crystal X-ray diffraction (XRD) analyses, energy-dispersive X-ray spectrometry (EDS) analyses, elemental analyses, cerate oxidimetry, powder XRD, fourier transform infrared (FT-IR) spectroscopy, ultraviolet-visible-near-infrared (UV-Vis-NIR) solid diffuse reflection spectrum and X-ray photoelectron spectroscopy (XPS) analyses. The electrochemical property (cyclic voltammetry (CV)) of compound 1 has also been studied.

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

Stoichiometric determination of moisture in edible oils by Mid-FTIR spectroscopy.

PubMed

van de Voort, F R; Tavassoli-Kafrani, M H; Curtis, J M

2016-04-28

A simple and accurate method for the determination of moisture in edible oils by differential FTIR spectroscopy has been devised based on the stoichiometric reaction of the moisture in oil with toluenesulfonyl isocyanate (TSI) to produce CO2. Calibration standards were devised by gravimetrically spiking dry dioxane with water, followed by the addition of neat TSI and examination of the differential spectra relative to the dry dioxane. In the method, CO2 peak area changes are measured at 2335 cm(-1) and were shown to be related to the amount of moisture added, with any CO2 inherent to residual moisture in the dry dioxane subtracted ratioed out. CO2 volatility issues were determined to be minimal, with the overall SD of dioxane calibrations being ∼18 ppm over a range of 0-1000 ppm. Gravimetrically blended dry and water-saturated oils analysed in a similar manner produced linear CO2 responses with SD's of <15 ppm on average. One set of dry-wet blends was analysed in duplicate by FTIR and by two independent laboratories using coulometric Karl Fischer (KF) procedures. All 3 methods produced highly linear moisture relationships with SD's of 7, 16 and 28 ppm, respectively over a range of 200-1500 ppm. Although the absolute moisture values obtained by each method did not exactly coincide, each tracked the expected moisture changes proportionately. The FTIRTSI-H2O method provides a simple and accurate instrumental means of determining moisture in oils rivaling the accuracy and specificity of standard KF procedures and has the potential to be automated. It could also be applied to other hydrophobic matrices and possibly evolve into a more generalized method, if combined with polar aprotic solvent extraction. Copyright © 2016 Elsevier B.V. All rights reserved.

Influence of hyperbaric oxygen on biomechanics and structural bone matrix in type 1 diabetes mellitus rats.

PubMed

Limirio, Pedro Henrique Justino Oliveira; da Rocha Junior, Huberth Alexandre; Morais, Richarlisson Borges de; Hiraki, Karen Renata Nakamura; Balbi, Ana Paula Coelho; Soares, Priscilla Barbosa Ferreira; Dechichi, Paula

2018-01-01

The aim of this study was to evaluate the biomechanics and structural bone matrix in diabetic rats subjected to hyperbaric oxygen therapy (HBO). Twenty-four male rats were divided into the following groups: Control; Control + HBO; Diabetic, and Diabetic + HBO. Diabetes was induced with streptozotocin (STZ) in the diabetic Groups. After 30 days, HBO was performed every 48h in HBO groups and all animals were euthanized 60 days after diabetic induction. The femur was submitted to a biomechanical (maximum strength, energy-to-failure and stiffness) and Attenuated Total Reflectance Fourier transform infrared (ATR-FTIR) analyses (crosslink ratio, crystallinity index, matrix-to-mineral ratio: Amide I + II/Hydroxyapatite (M:MI) and Amide III + Collagen/HA (M:MIII)). In biomechanical analysis, diabetic animals showed lower values of maximum strength, energy and stiffness than non-diabetic animals. However, structural strength and stiffness were increased in groups with HBO compared with non-HBO. ATR-FTIR analysis showed decreased collagen maturity in the ratio of crosslink peaks in diabetic compared with the other groups. The bone from the diabetic groups showed decreased crystallinity compared with non-diabetic groups. M:MI showed no statistical difference between groups. However, M:MIII showed an increased matrix mineral ratio in diabetic+HBO and control+HBO compared with control and diabetic groups. Correlations between mechanical and ATR-FTIR analyses showed significant positive correlation between collagen maturity and stiffness. Diabetes decreased collagen maturation and the mineral deposition process, thus reducing biomechanical properties. Moreover, the study showed that HBO improved crosslink maturation and increased maximum strength and stiffness in the femur of T1DM animals.

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.

75 FR 70623 - Airworthiness Directives; DORNIER LUFTFAHRT GmbH Models Dornier 228-100, Dornier 228-101, Dornier...

Federal Register 2010, 2011, 2012, 2013, 2014

2010-11-18

... measurements as well as finite element modelling and fatigue analyses to better understand the stress... include strain measurements as well as finite element modeling and fatigue analyses to better understand... finite element modelling and fatigue analyses to better understand the stress distribution onto the frame...

Smoke and mirrors: Ultra-rapid-scan FT-IR spectrometry

NASA Astrophysics Data System (ADS)

Manning, C. J.

1998-06-01

Fourier transform-infrared spectrometers have dominated the marketplace and the experimental literature of vibrational spectroscopy for almost three decades. These versatile instruments have been applied to a wide variety of measurements in both industrial and research settings. There has been, however, an ongoing need for enhanced time resolution. Limitations of time resolution in FT-IR measurements arise from the modulation frequencies intrinsic to the spectral multiplexing. Events which are slower than the minimum scan time, about 40 milliseconds at 4-cm-1 resolution, can be readily monitored with conventional instrumentation. For shorter transients, various step-scan, stroboscopic and asynchronous methods have been demonstrated to provide excellent time resolution, down to nanoseconds, but these approaches are limited to events which can be repeated many times with minimal variations. Some of these methods are also susceptible to low-frequency noise sources. The intrinsic scan time of conventional FT-IR spectrometers is limited by the force that can be applied to the moving mirror. In commercial systems the moving mirror is invariably driven by a voice coil linear motor. The maximum force that can be exerted by the voice coil is sharply limited to a few Newtons. It is desirable to decrease the scan time by a large factor, but the required force scales as the square of the scan rate, while the voltage applied to the coil must scale as the cube of the rate. A more suitable approach to very-rapid-scan FT-IR spectrometry may be the use of rotating optical components which do not have to turn around at the end of travel. There is, however, an apparent symmetry mismatch between rotating elements and the nominally planar wavefronts in a Michelson interferometer. In spite of the mismatch, numerous interferometer designs based on rotating elements have been proposed and demonstrated. Some of these designs are suitable for operation with scan times from tens of milliseconds to milliseconds, and perhaps faster, at 4-cm-1 resolution. A novel interferometer design utilizing a single-sided precessing disk mirror allows a complete interferogram to be measured in 1 millisecond or less. A prototype instrument of this design has been constructed and tested. One application reported here is the measurement of a transient combustion event. While combustion reactions can be conveniently repeated under some circumstances, such as with gas-phase reactants, the shot-to-shot variation is unacceptably large for step-scan measurements. Preliminary data, illustrating operation and performance of the system, are presented. It is thought that the high modulation frequencies have resulted in superior rejection of multiplicative noise.

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

NASA Astrophysics Data System (ADS)

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

2015-10-01

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

Quantitative Effects of P Elements on Hybrid Dysgenesis in Drosophila Melanogaster

PubMed Central

Rasmusson, K. E.; Simmons, M. J.; Raymond, J. D.; McLarnon, C. F.

1990-01-01

Genetic analyses involving chromosomes from seven inbred lines derived from a single M' strain were used to study the quantitative relationships between the incidence and severity of P-M hybrid dysgenesis and the number of genomic P elements. In four separate analyses, the mutability of sn(w), a P element-insertion mutation of the X-linked singed locus, was found to be inversely related to the number of autosomal P elements. Since sn(w) mutability is caused by the action of the P transposase, this finding supports the hypothesis that genomic P elements titrate the transposase present within a cell. Other analyses demonstrated that autosomal transmission ratios were distorted by P element action. In these analyses, the amount of distortion against an autosome increased more or less linearly with the number of P elements carried by the autosome. Additional analyses showed that the magnitude of this distortion was reduced when a second P element-containing autosome was present in the genome. This reduction could adequately be explained by transposase titration; there was no evidence that it was due to repressor molecules binding to P elements and inhibiting their movement. The influence of genomic P elements on the incidence of gonadal dysgenesis was also investigated. Although no simple relationship between the number of P elements and the incidence of the trait could be discerned, it was clear that even a small number of elements could increase the incidence markedly. The failure to find a quantitative relationship between P element number and the incidence of gonadal dysgenesis probably reflects the complex etiology of this trait. PMID:2155853

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

Akagi, Sheryl; Burling, Ian R.; Mendoza, Albert

We report trace-gas emission factors from three pine-understory prescribed fires in South Carolina, U.S. measured during the fall of 2011. The fires were an attempt to simulate high-intensity burns and the fuels included mature pine stands not frequently subjected to prescribed fire that were lit following a sustained period of drought. In this work we focus on the emission factor measurements made using a fixed open-path gas analyzer Fourier transform infrared (FTIR) system. We compare these emission factors with those measured using a roving, point sampling, land-based FTIR and an airborne FTIR that were deployed on the same fires. Wemore » also compare to emission factors measured by a similar open-path FTIR system deployed on savanna fires in Africa. The data suggest that the method in which the smoke is sampled can strongly influence the relative abundance of the emissions that are observed. The airborne FTIR probed the bulk of the emissions, which were lofted in the convection column and the downwind chemistry while the roving ground-based point sampling FTIR measured the contribution of individual residual smoldering combustion fuel elements scattered throughout the burn site. The open-path FTIR provided a fixed path-integrated sample of emissions produced directly upwind mixed with emissions that were redirected by wind gusts, or right after ignition and before the adjacent plume achieved significant vertical development. It typically probed two distinct combustion regimes, “flaming-like” (immediately after adjacent ignition) and “smoldering-like”, denoted “early” and “late”, respectively. The calculated emission factors from open-path measurements were closer to the airborne than to the point measurements, but this could vary depending on the calculation method or from fire to fire given the changing MCE and dynamics over the duration of a typical burn. The emission factors for species whose emissions are not highly fuel dependent (e.g. CH4 and CH3OH) from all three systems can be plotted versus modified combustion efficiency and fit to a single consistent trend suggesting that differences between the systems for these species may be mainly due to the unique mix of flaming and smoldering that each system sampled. For other more fuel dependent species, the different fuels sampled also likely contributed to platform differences in emission factors. The path-integrated sample of the ground-level smoke layer adjacent to the fire provided by the open-path measurements is important for estimating fire-line exposure to smoke for wildland fire personnel. We provide a table of estimated fire-line exposures for numerous known air toxics based on synthesizing results from several studies. Our data suggest that peak exposures are more likely to challenge permissible exposure limits for wildland fire personnel than shift-average exposures.« less

Coordinated in Situ Analyses of Organic Nanoglobules in the Sutter's Mill Meteorite

NASA Technical Reports Server (NTRS)

Nakamura-Messenger, K.; Messenger, S.; Keller, L. P.; Clemett, S. J.; Nguyen, A. N.; Gibson, E. K.

2013-01-01

The Sutter's Mill meteorite is a newly fallen carbonaceous chondrite that was collected and curated quickly after its fall. Preliminary petrographic and isotopic investigations suggest affinities to the CM2 carbonaceous chondrites. The primitive nature of this meteorite and its rapid recovery provide an opportunity to investigate primordial solar system organic matter in a unique new sample. Here we report in-situ analyses of organic nanoglobules in the Sutter's Mill meteorite using UV fluorescence imaging, Fourier-transform infrared spectroscopy (FTIR), scanning transmission electron microscopy (STEM), NanoSIMS, and ultrafast two-step laser mass spectrometry (ultra-L2MS).

A computer graphics program for general finite element analyses

NASA Technical Reports Server (NTRS)

Thornton, E. A.; Sawyer, L. M.

1978-01-01

Documentation for a computer graphics program for displays from general finite element analyses is presented. A general description of display options and detailed user instructions are given. Several plots made in structural, thermal and fluid finite element analyses are included to illustrate program options. Sample data files are given to illustrate use of the program.

Element variations in rhyolitic magma resulting from gas transport

NASA Astrophysics Data System (ADS)

Berlo, K.; Tuffen, H.; Smith, V. C.; Castro, J. M.; Pyle, D. M.; Mather, T. A.; Geraki, K.

2013-11-01

Tuffisite veins are glass-filled fractures formed when magma fragments during degassing within the conduit. These veins form transient channels through which exsolved gases can escape from magma. The purpose of this study is to determine the extent to which chemical heterogeneity within the melt results from gas transport, and assess how this can be used to study magma degassing. Two tuffisite veins from contrasting rhyolitic eruptions at Torfajökull (Iceland) and Chaitén (Chile) were studied in detail. The tuffisite vein from Torfajökull is from a shallow dissected conduit (∼70 ka) that fed a degassed lava flow, while the sample from Chaitén was a bomb ejected during the waning phases of Plinian activity in May 2008. The results of detailed in situ chemical analyses (synchrotron XRF, FTIR, LA-ICP-MS) show that in both veins larger vesiculated fragments are enriched in volatile elements (Torfajökull: H, Li, Cl; Chaitén: Li, Cl, Cu, Zn, As, Sn, Sb) compared to the host, while the surrounding smaller particles are depleted in the Torfajökull vein (Li, Cl, Zn, Br, Rb, Pb), but enriched in the Chaitén vein (K, Cu, Zn, As, Mo, Sb, Pb). The lifespans of both veins and the fluxes of gas and particles through them can be estimated using diffusion profiles and enrichment factors. The Torfajökull vein had a longer lifespan (∼a day) and low particle velocities (∼cm/s), while the Chaitén vein was shorter lived (<1 h) with a high gas velocity (∼m/s). These differences are consistent with the contrasting eruption mechanisms (effusive vs. explosive). The amount of magma that degassed through the Chaitén vein is more than ten times the volume of the vein itself, requiring the vein to tap into pre-exsolved gas pockets. This study highlights that tuffisite veins are highly efficient gas pathways and thereby impart chemical diversity in volatile elements on the melt.

[The analyses and identification of Flos rhododendri mollis and Flos chrysanthemi indici via infrared spectroscopy].

PubMed

Jin, Zhe-Xiong; Wang, Yue; Zhou, Qun; Chen, Jian-Bo; Ma, Fang; Sun, Su-Qin

2014-09-01

In this study, major chemical components of Flos rhododendri mollis and Flos chrysanthemi indici were characterized using Fourier transform infrared spectroscopy (FTIR). For Flos rhododendri mollis, the bands at 1,648 and 1,543 cm(-1) were attributed to amide I and amide II , respectively, indicating that it contained proteins probably resulting in immunization. In case of Flos chrysanthemi indici, stretching vibration of C==O function group was responsible for the bands at 1,734 and 1,515 cm(-1), as a result of essential oils, lipids, etc. Since FTIR spectra of Flos rhododendri mollis and Flos chrysanthemi indici are almost identical and it is difficult to discriminate them, two-step identification was investigated via secondary derivative of the FTIR spectra. The bands at 1,656 and 1,515 cm(-1) corresponds to flavonoides in Flos rhododendri mollis and Flos chrysanthemi indici. In the secondary derivative of the FTIR spectrum of Flos chrysanthemi indici, characteristic bands of inulin were present at 1,163, 1,077, 1,026, 986 and 869 cm(-1), and therefore Flos chrysanthemi indici contained inulin as well. Tri-step identification was carried out for Flos rhododendri mollis and Flos chrysanthemi indici by means of comparing their 2D-IR correlation spectra in different wave number range. In the characteristic range of flavonoides (1,700-1,400 cm(-1)), Flos rhododendri mollis exhibited 3 obvious autopeaks, while 10 autopeaks were visualized in the 2D-IR correlation spectrum of Flos chrysanthemi indici Moreover, in the characteristic range of glucoside (1,250-900 cm(-1)), 10 and 9 autopeaks were present in the 2D-IR correlation spectra of Flos rhododendri mollis and Flos chrysanthemi indici, respectively. Therefore, the tri-step identification of FTIR is a time-saving; accurate, cost-saving and convenient method to effectively distinguish traditional Chinese medicines.

[Study on the fine structure of K-feldspar of Qichun granite].

PubMed

Du, Deng-Wen; Hong, Han-Lie; Fan, Kan; Wang, Chao-Wen; Yin, Ke

2013-03-01

Fine structure of K-feldspar from the Qichun granite was investigated using X-ray diffraction (XRD), Fourier infrared absorption spectroscopy (FTIR), and inductively coupled plasma mass spectrometry methods to understand the evolution of the granitic magmatism and its correlation to molybdenite mineralization. The XRD results showed that K-feldspar of the potassic alteration veins has higher ordering index and triclinicity and is namely microcline with triclinic symmetry. K-feldspar of the early cretaceous granite has relatively lower ordering index and has widening [131] peak and is locally triclinic ordering. K-feldspar of the late cretaceous granite has lowest ordering index and sharp [131] peak and is honiogeneously monoclinic. The FTIR results showed that the IR spectra of the Qichun K-feldspar are similar to that of orthoclase reported by Farmer (1974). The 640 cm-1 absorption band increases while the 540 cm-' absorption band decreases with increase in K-feldspar ordering index, also, the 1,010 cm-1 absorption band separates into 1,010 and 1,046 cm-1 absorption bands, with a change in the band shape from widening to sharp outline. The ICP-MS results suggested that K-feldspar of the early cretaceous granite has relatively higher metal elements and rare earth elements, and the granite exhibits better mineralization background, K-feldspar of the potassic alteration veins has markedly lower Sr and Ba, indicating that the alteration fluid originated from the granitic magmatism, and hence, potassic alteration is a good indicator for molybdenite exploration.

Competitive sorption of carbonate and arsenic to hematite: combined ATR-FTIR and batch experiments.

PubMed

Brechbühl, Yves; Christl, Iso; Elzinga, Evert J; Kretzschmar, Ruben

2012-07-01

The competitive sorption of carbonate and arsenic to hematite was investigated in closed-system batch experiments. The experimental conditions covered a pH range of 3-7, arsenate concentrations of 3-300 μM, and arsenite concentrations of 3-200 μM. Dissolved carbonate concentrations were varied by fixing the CO(2) partial pressure at 0.39 (atmospheric), 10, or 100 hPa. Sorption data were modeled with a one-site three plane model considering carbonate and arsenate surface complexes derived from ATR-FTIR spectroscopy analyses. Macroscopic sorption data revealed that in the pH range 3-7, carbonate was a weak competitor for both arsenite and arsenate. The competitive effect of carbonate increased with increasing CO(2) partial pressure and decreasing arsenic concentrations. For arsenate, sorption was reduced by carbonate only at slightly acidic to neutral pH values, whereas arsenite sorption was decreased across the entire pH range. ATR-FTIR spectra indicated the predominant formation of bidentate binuclear inner-sphere surface complexes for both sorbed arsenate and sorbed carbonate. Surface complexation modeling based on the dominant arsenate and carbonate surface complexes indicated by ATR-FTIR and assuming inner-sphere complexation of arsenite successfully described the macroscopic sorption data. Our results imply that in natural arsenic-contaminated systems where iron oxide minerals are important sorbents, dissolved carbonate may increase aqueous arsenite concentrations, but will affect dissolved arsenate concentrations only at neutral to alkaline pH and at very high CO(2) partial pressures. Copyright © 2012 Elsevier Inc. All rights reserved.

FTIR Analyses of Hypervelocity Impact Deposits: DebriSat Tests

DTIC Science & Technology

2015-03-27

Aerospace Concept Design Center advised on selection of materials for various subsystems. • Test chamber lined with “soft catch” foam panels to trap...C-0001 Authorized by: Space Systems Group Distribution Statement A: Approved for public release; distribution unlimited Report...Pre Preshot target was a multi-shock shield supplied by NASA designed to catch the projectile. It consisted of seven bumper panels consisting of

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

Azmi, M. A.; Ismail, N. A. A.; Rizamarhaiza, M.

Rice husk was thermally decomposed to yield powder composed of silica (SiO{sub 2}). Temperatures of 700°C and 1000°C were chosen as the decomposition temperatures. X-Ray Diffraction (XRD), X-Ray Florescence (XRF), Fourier Transform Infrared (FTIR), and Field Emission Scanning Electron Microscope (FESEM) analyses were conducted on a synthetic silica powder (SS-SiO{sub 2}) and the rice husk ash as for the comparative characterisation study. XRD analyses clearly indicated that the decomposed rice husk yielded silica of different nature which are Crystalline Rice Husk Silica (C-RHSiO{sub 2}) and Amorphous Rice Husk Silica (A-RHSiO{sub 2}). Moreover, it was found that SS-SiO{sub 2} was ofmore » Quartz phase, C-RHSiO{sub 2} was of Trydimite and Cristobalite. Through XRF detection, the highest SiO{sub 2} purity was detected in SS-SiO{sub 2} followed by C-RHSiO{sub 2} and A-RHSiO{sub 2} with purity percentages of 99.60%, 82.30% and 86.30% respectively. FTIR results clearly indicated silica (SiO{sub 2}) bonding 1056, 1064, 1047, 777, 790 and 798 cm{sup −1}) increased as the crystallinity silica increased. The Cristobalite phase was detected in C-RH SiO{sub 2} at the wavelength of 620 cm{sup −1}. Morphological features as observed by FESEM analyses confirmed that, SS-SiO{sub 2} and C-RH SiO{sub 2} showed prominent coarse granular morphology.« less

Controllable Synthesis of Lindqvist Alkoxopolyoxovanadate Clusters as Heterogeneous Catalysts for Sulfoxidation of Sulfides.

PubMed

Li, Ji-Kun; Dong, Jing; Wei, Chuan-Ping; Yang, Song; Chi, Ying-Nan; Xu, Yan-Qing; Hu, Chang-Wen

2017-05-15

Six alkoxohexavanadate-based Cu- or Co-POVs [Cu(dpa)(acac)(H 2 O)] 2 [V 6 O 13 (OMe) 6 ] (1), [Cu(phen)(acac)(MeOH)] 2 [V 6 O 13 (OMe) 6 ] (2), [Co(dpa)(acac) 2 ] 2 [V 6 O 13 (OMe) 6 ]·2MeOH (3), [Co(phen)(acac) 2 ] 2 [V 6 O 13 (OMe) 6 ] (4), [Cu(dpa)(acac)] 2 [V IV 2 V V 4 O 12 (OMe) 7 ] (5), and [Cu(dpa)(acac)(MeOH)] 2 [V IV 2 V V 4 O 11 (OMe) 8 ] (6) (POV = polyoxovanadate; dpa = 2,2'-dipyridine amine; phen = 1,10-phenanthroline; acac = acetylacetone anion) have been synthesized by controlling the reaction conditions and characterized by single-crystal X-ray diffraction and powder X-ray diffraction analyses, FT-IR spectroscopy, element analyses, and X-ray photoelectron spectroscopy. In compounds 1-4 and 6, Cu or Co complexes and alkoxohexavanadate anions are assembled through electrostatic interactions. Differently, in compound 5, seven-methoxo-substituted Lindqvist-type [V 6 O 12 (OMe) 7 ] 2- are bridged to Cu complex via terminal O atoms by coordination bonds. All compounds 1-6 exhibit excellent heterogeneous catalytic performance in oxidative desulfurization and CEES ((2-chloroethyl) ethyl sulfide, a sulfur mustard simulant) abatement with H 2 O 2 as oxidant. Among them, the catalytic activity of 6 [conv. of DBT (dibenzothiophene) up to 100% in 6 h; conv. of CEES reached 100% and selectivity of CEESO ((2-chloroethyl) ethyl sulfoxide) up to 85% after 4 h] outperforms others and can be reused without losing its activity.

D/H and Water Concentrations of Submarine MORB Glass Around the World: Analytical Aspects, Standardization, and (re)defining Mantle D/H Ranges

NASA Astrophysics Data System (ADS)

Bindeman, I. N.; Dixon, J. E.; Langmuir, C. H.; Palandri, J. L.

2015-12-01

The advent and calibration of the Thermal Combustion Element Analyzer (TCEA) continuous flow system coupled with the large-radius mass spectrometer MAT253 permits precise (±0.02 wt.% H2O, ±1-3‰ D/H) measurements in 1-10 mg of volcanic glass (0.1 wt.% H2O requires ~10 mg glass), which permits the targeting of small amounts of the freshest concentrate. This is a >100 factor reduction in sample size over conventional methods, four times over more common Delta series instruments. We investigated in triplicate 115 samples of submarine MORB glasses ranging from water-poor (0.1-0.2wt%) to water-rich (1.2-1.5wt%). These samples were previously investigated for major and trace elements, radiogenic isotopes; a large subset of these samples coming from the FAZAR expedition were studied previously by FTIR for water concentration. We also ran samples previously studied by the conventional off-line technique: MORB glass including those from the Easter Platform and the Alvin 526-1 standard (0.2wt% H2O). We observe excellent 1:1 correspondence (1.02x+0.02, R2=0.94) of wt% water by FTIR and TCEA suggesting complete extraction of water and no dependence on water concentration. We measure 51‰ total range in D/H that correlates with all other chemical and isotopic indicators of mantle enrichment, with the heaviest values occurring in the most enriched samples. When used uncorrected values of H2 gas run against H2 gas of known composition, this range agrees nicely with previous D/H range for MORB (-30 to -90‰), measured for samples run conventionally. Uncorrected analyses of Alvin glass 526-1 gives -66‰. When run against SMOW, SLAP and -41‰ water sealed in silver cups, the range is shifted by -15‰; when standardization is done by with three commonly used mica standards as is done most commonly in different labs, the range is shifted downward by -30-32‰. There are no isotopic offsets related to total water or D/H range requiring different slope or non-linear correction. The NBS30 mica standard has been recently shown to be heavier and more heterogeneous than previously thought, and older conventional methods that relied on Pt reduction unreliable. Based on these new TCEA results, the D/H values of MORB and mantle samples may need to be revised to lighter values by 15‰.

A comparison between different finite elements for elastic and aero-elastic analyses.

PubMed

Mahran, Mohamed; ELsabbagh, Adel; Negm, Hani

2017-11-01

In the present paper, a comparison between five different shell finite elements, including the Linear Triangular Element, Linear Quadrilateral Element, Linear Quadrilateral Element based on deformation modes, 8-node Quadrilateral Element, and 9-Node Quadrilateral Element was presented. The shape functions and the element equations related to each element were presented through a detailed mathematical formulation. Additionally, the Jacobian matrix for the second order derivatives was simplified and used to derive each element's strain-displacement matrix in bending. The elements were compared using carefully selected elastic and aero-elastic bench mark problems, regarding the number of elements needed to reach convergence, the resulting accuracy, and the needed computation time. The best suitable element for elastic free vibration analysis was found to be the Linear Quadrilateral Element with deformation-based shape functions, whereas the most suitable element for stress analysis was the 8-Node Quadrilateral Element, and the most suitable element for aero-elastic analysis was the 9-Node Quadrilateral Element. Although the linear triangular element was the last choice for modal and stress analyses, it establishes more accurate results in aero-elastic analyses, however, with much longer computation time. Additionally, the nine-node quadrilateral element was found to be the best choice for laminated composite plates analysis.

In-vitro bioactivity of zirconia doped borosilicate glasses

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

Samudrala, Rajkumar; Azeem, P. Abdul, E-mail: rk.satyaswaroop@gmail.com, E-mail: drazeem2002@yahoo.com

2015-06-24

Glass composition 31B{sub 2}O{sub 3}-20SiO{sub 2}-24.5Na{sub 2}O-(24.5-x) CaO-xZrO{sub 2} x=1,2,3,4,5 were prepared by melt-quenching Technique. The formation of hydroxyapatite layer on the surface of glasses after immersion in simulated body fluid (SBF) was explored through XRD, Fourier transform infrared (FTIR) and Scanning electron microscopy (SEM-EDX) analyses. In this report, we observed that hydroxyapatite formation for 5days of immersion time. Also observed that with increasing the immersion time up to 15days, higher amount of hydroxyapatite layer formation on the surface of glasses. The varying composition of zirconia in glass samples influences shown by XRD, FTIR studies. The present results indicate that,more » in-vitro bioactivity of glasses decreased with increasing zirconia incorporation.« less

Development of transition metal dichalcogenide based quantum dots for light emitting diodes

NASA Astrophysics Data System (ADS)

Seth, Subhashree; Sharma, S. K.

2018-05-01

Photoluminescent quantum dots (QDs) were synthesized by facile colloidal chemical route. Its properties were characterized and analysed by utilizing Fluorescence, FTIR and UV-Vis spectrophotometers. The resultant MoS2 QD exhibits fluorescence at 470 nm for excitation wavelength 400 nm. The as prepared sample exhibits excitation dependent emission due to polydispersion of MoS2 in the dispersive medium which is the characteristics of colloidal synthesis. It is also observed that resultant MoS2 QDs show size tunable emission in the visible region. The FTIR spectrum confirms the attachment of oleic acid on the surface of MoS2. Absorption spectrum shows a band at 346 nm and a shoulder band at 400 nm. The band gap of quantum dots was obtained as 3.5 eV. CIE diagram indicates the shifting of colour coordinates towards green region with increasing excitation wavelength.

High resolution FTIR spectrum of the ν 6 band of deuterated formic acid (DCOOH)

NASA Astrophysics Data System (ADS)

Goh, K. L.; Ong, P. P.; Tan, T. L.; Teo, H. H.

1999-07-01

The high resolution FTIR spectrum of the ν 6 band of DCOOH has been measured with a resolution of 0.004 cm -1 in the spectral range of 920-1020 cm -1. The ν 6 band was found to be perturbed by the neighbouring ν 8 band situated at about 100 cm -1 lower. Using a Watson's A-reduced Hamiltonian in the Ir representation, and with the inclusion of a-, and b-Coriolis coupling constants, a simultaneous fit of ν 6 and ν 8 was performed, fitting a total of 1656 infrared transitions of ν 6 with an rms uncertainty of 0.00038 cm -1. A set of accurate rovibrational constants for ν 6 were obtained. The ν 6 band was analysed to be primarily A-typed with a band centre at 970.88931±0.00003 cm -1.

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.

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

Batista, Adriana S.M.; Gual, Maritza R.; Faria, Luiz O.

Poly(vinylidene fluoride) homopolymers [PVDF] homopolymers were irradiated with gamma doses ranging from 0.5 to 2.75 MGy. Differential scanning calorimetry (DSC) and FTIR spectrometry were used in order to study the effects of gamma radiation in the amorphous and crystalline polymer structures. The FTIR data revealed absorption bands at 1730 and 1853 cm{sup -1} which were attributed to the stretch of C=O bonds, at 1715 and 1754 cm{sup -1} which were attributed to the C=C stretching and at 3518, 3585 and 3673 cm{sup -1} which were associated with NH stretch of NH{sub 2} and OH. The melting latent heat (LM) measuredmore » by DSC was used to construct an unambiguous relationship with the delivered dose. Regression analyses revealed that the best mathematical function that fits the experimental calibration curve is a 4-degree polynomial function, with an adjusted Rsquare of 0.99817. (authors)« less

Application of vibrational spectroscopy, thermal analyses and X-ray diffraction in the rapid evaluation of the stability in solid-state of ranitidine, famotidine and cimetidine.

PubMed

Jamrógiewicz, Marzena; Ciesielski, Aleksander

2015-03-25

This paper reports the study on applicability of Fourier transform infrared (FTIR), near-infrared (NIR) and Raman spectroscopy, differential scanning calorimetry (DSC) and X-ray diffraction (XRD) for the estimation of the chemical stability and photostability of histamine H2-receptor antagonist substances. Ranitidine hydrochloride (RAN), famotidine (FAM) and cimetidine (CIM) were tested and differences in sensitivity were measured via soft independence modeling of class analogies (Simca) model. The low values of variations for FAM and CIM and high variations obtained for RAN using FTIR and NIR techniques indicated that these methods were suitable and applicable to classify the degradation of RAN. Examined methods are recommendable in the first technological stage of drug production, and the preclinical and clinical development of pharmaceuticals or their quality control. Copyright © 2015 Elsevier B.V. All rights reserved.

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

Applications of mid-infrared spectroscopy in the clinical laboratory setting.

PubMed

De Bruyne, Sander; Speeckaert, Marijn M; Delanghe, Joris R

2018-01-01

Fourier transform mid-infrared (MIR-FTIR) spectroscopy is a nondestructive, label-free, highly sensitive and specific technique that provides complete information on the chemical composition of biological samples. The technique both can offer fundamental structural information and serve as a quantitative analysis tool. Therefore, it has many potential applications in different fields of clinical laboratory science. Although considerable technological progress has been made to promote biomedical applications of this powerful analytical technique, most clinical laboratory analyses are based on spectroscopic measurements in the visible or ultraviolet (UV) spectrum and the potential role of FTIR spectroscopy still remains unexplored. In this review, we present some general principles of FTIR spectroscopy as a useful method to study molecules in specimens by MIR radiation together with a short overview of methods to interpret spectral data. We aim at illustrating the wide range of potential applications of the proposed technique in the clinical laboratory setting with a focus on its advantages and limitations and discussing the future directions. The reviewed applications of MIR spectroscopy include (1) quantification of clinical parameters in body fluids, (2) diagnosis and monitoring of cancer and other diseases by analysis of body fluids, cells, and tissues, (3) classification of clinically relevant microorganisms, and (4) analysis of kidney stones, nails, and faecal fat.

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

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

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

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

2016-05-06

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

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

PubMed

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

2013-01-01

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

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

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

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

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

NASA Astrophysics Data System (ADS)

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

2017-11-01

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

Combined SIMS, NanoSIMS, FTIR, and SEM Studies of OH in Nominally Anhydrous Minerals (NAMs)

NASA Astrophysics Data System (ADS)

Mosenfelder, J. L.; Le Voyer, M.; Rossman, G. R.; Guan, Y.; Bell, D. R.; Asimow, P. D.; Eiler, J.

2010-12-01

The accurate analysis of trace concentrations of hydrogen in NAMs is a long-standing problem, with wide-ranging implications in geology and planetology. SIMS and FTIR are two powerful and complementary analytical tools capable of measuring concentrations down to levels of less than 1 ppm H2O. Both methods, however, are subject to matrix effects and rely on other techniques such as manometry or nuclear reaction analysis (NRA) for quantitative calibration. We compared FTIR and SIMS data for a wide variety of NAMs: olivine, orthopyroxene, clinopyroxene, pyrope and grossular garnet, rutile, zircon, kyanite, andalusite, and sillimanite. Some samples were also characterized using high-resolution FE-SEM to assess the potential contribution of submicrocopic inclusions to the analyses. For SIMS, we use high mass resolution (≥5000 MRP) to measure 16O1H, using 30Si and/or 18O as reference isotopes. We use both primary standards, measured independently using manometry or NRA (e.g., [1]), and secondary standards, measured using polarized FTIR referenced back to calibrations developed on primary standards. Our major focus was on on olivine, for which we collected repeated calibration data with both SIMS and NanoSIMS, bracketing measurements of H diffusion profiles in both natural and experimentally annealed crystals at levels of 5-100 ppm H2O. With both instruments we establish low blanks (≤5 ppm) and high precision (typically less than 5% 2-σ errors in 16O1H/30Si), critical requirements for the low concentration levels being measured. Assessment of over 300 analyses on 11 olivines allows us to evaluate the suitability of different standards, several of which are in use in other laboratories [2,3,4]. Seven olivines, with 0-125 ppm H2O, give highly reproducible results and allow us to establish well-constrained calibration slopes with high correlation coefficients (r2 = 0.98-99), in contrast to previous studies [2,3,4]. However, four kimberlitic megacrysts with 140-243 ppm H2O show 16O1H/30Si ratios that vary by up to a factor of 2 even in sequential analyses (cf. [3,4]). A potential cause of these discrepancies is the presence of sub-micron scale pores (as small as 100 nm), which we have documented by SEM. These pores probably contain liquid H2O and/or condensed hydrous phase precipitates. Although the ionization potential of fluids under high-vacuum conditions is an under-studied problem, these sub-micron features may contribute to the measured 16O1H, resulting in analyses with erratic depth profiles and corresponding high uncertainties (up to 15% 2-σ). However, if we omit analyses with such high uncertainties, the data for all olivines fit well together. Our results imply that the Bell et al. IR calibration [1] can be applied accurately to all olivines with IR bands from ~3400-3650 cm-1, without the need for band-specific IR absorption coefficients (cf. [3]). A five-fold total variation was observed among the calibration line slopes for the different minerals analyzed, confirming the need for mineral-specific calibrations. [1]Bell et al. (2003), JGR, 108 [2] Tenner et al. (2009), Chem. Geol., 262, 42-56 [3] Kovács, I. et al. (2010), Am. Min., 95, 292-299 [4] O'Leary et al. (2010), EPSL

Synthesis, crystal structure and bioactivity of manganese complexes with asymmetric chiral Schiff base

NASA Astrophysics Data System (ADS)

Zhang, Enfeng; Wei, Yi; Huang, Fuping; Yu, Qing; Bian, Hedong; Liang, Hong; Lei, Fuhou

2018-03-01

A couple of chiral unsymmtrical Schiff base ligands, (1R,2R) (-)chxn (salH) (naftalH) and (1S,2S) (-)chxn (salH) (naftalH) had been synthesized by the condensation of salicylaldehyde and 2-hydroxy-1-naphthaldehyde with two isomers of (1R,2R)-trans-1,2-cyclohexanediamin and (1S,2S)-trans-1,2-cyclohexanediamin, respectively. At the same time, two manganese complexes have been synthesized and fully characterized by FT-IR spectrum, elemental analyses, single crystal X-ray diffraction. The interaction of the two Mn (III) complexes with bovine serum albumin (BSA) was investigated by spectroscopic techniques. The result reveals that the complexes can strongly quench the intrinsic fluorescence of BSA through a static quenching mechanism. The binding constant and binding mode has been determined. The secondary structure and the amino acid residues microenvironment of BSA change in the presence of these complexes. SOD-like activity and ABTS free radical scavenging ability were also studied. The antioxidant capacity of the compounds showed that the complexes and their corresponding BSA adducts showed some SOD activity. The results of ABTS free radical scavenging showed that the activity of the BSA adduct was more obvious than that of the complex.

Assessment of the unidentified organic matter fraction in fogwater using fluorescence spectroscopy

NASA Astrophysics Data System (ADS)

Valsaraj, K.; Birdwell, J.

2010-07-01

Dissolved organic matter (DOM) in fogwaters from southeastern Louisiana and central-eastern China has been characterized using excitation-emission matrix (EEM) fluorescence spectroscopy. The results demonstrate that fluorescence spectroscopy can be used to obtain a qualitative assessment of the large fraction of fogwater organic carbon (~40 - 80% by weight) that cannot be identified in terms of specific chemical compounds. The method has the principle advantage that it can be applied at natural abundance concentrations, thus eliminating the need for large sample volumes required to isolate DOM for characterization by other spectroscopic (NMR, FTIR) and chemical (elemental) analyses. It was anticipated that the fogwater organic matter fluorescence spectra would resemble those of surface and rain waters, containing peaks indicative of both humic substances and fluorescent amino acids. Humic- and protein-like fluorophores were observed in the fogwater spectra and fluorescence-derived indices had values comparable to other natural waters. Biological character (intensity of tyrosine and tryptophan peaks) was found to increase with organic carbon concentration. Fogwater organic matter appears to contain a mixture of terrestrially- and microbially-derived material. The fluorescence results show that most of the unidentified fogwater organic carbon can be represented by humic-like and biologically-derived substances similar to those present in other aquatic systems.

Low-Temperature Heat Capacities and Standard Molar Enthalpy of Formation of Potassium Benzoate C7H5O2K(s)

NASA Astrophysics Data System (ADS)

Yang, Wei-Wei; di, You-Ying; Yin, Zhen-Fen; Kong, Yu-Xia; Tan, Zhi-Cheng

2009-04-01

Potassium benzoate C7H5O2K (CAS Registry No. 582-25-2) was synthesized by the method of liquid phase reaction. Chemical and elemental analyses, FTIR, and X-ray powder diffraction (XRD) techniques were applied to characterize the composition and structure of the compound. Low-temperature heat capacities of the compound were measured by a precision automated adiabatic calorimeter over the temperature range from 78 K to 398 K. A polynomial equation of the heat capacities as a function of temperature was fitted by the least-squares method. Smoothed heat capacities and thermodynamic functions of the compound were calculated based on the fitted polynomial. In accordance with Hess’s law, a reasonable thermochemical cycle was designed, and 100 mL of 1 mol · dm-3 NaOH solution was chosen as the calorimetric solvent. The standard molar enthalpies of dissolution for the reactants and products of the supposed reaction in the selected solvent were measured by an isoperibol solution-reaction calorimeter. Finally, the standard molar enthalpy of formation of the title compound C7H5O2K (s) was derived to be -(610.94 ± 0.77) kJ · mol-1.

Fabrication of 3D lawn-shaped N-doped porous carbon matrix/polyaniline nanocomposite as the electrode material for supercapacitors

NASA Astrophysics Data System (ADS)

Zhang, Xiuling; Ma, Li; Gan, Mengyu; Fu, Gang; Jin, Meng; Lei, Yao; Yang, Peishu; Yan, Maofa

2017-02-01

A facile approach to acquire electrode materials with prominent electrochemical property is pivotal to the progress of supercapacitors. 3D nitrogen-doped porous carbon matrix (PCM), with high specific surface area (SSA) up to 2720 m2 g-1, was obtained from the carbonization and activation of the nitrogen-enriched composite precursor (graphene/polyaniline). Then 3D lawn-shaped PCM/PANI composite was obtained by the simple in-situ polymerization. The morphology and structure of these resulting composites were characterized by combining SEM and TEM measurements, Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD) spectroscopy analyses and Raman spectroscope. The element content of all samples was evaluated using CHN analysis. The results of electrochemical testing indicated that the PCM/PANI composite displays a higher capacitance value of 527 F g-1 at 1 A g-1 compared to 338 F g-1 for pure PANI, and exhibits appreciable rate capability with a retention of 76% at 20 A g-1 as well as fine long-term cycling performance (with 88% retention of specific capacitance after 1000 cycles at 10 A g-1). Simultaneously, the excellent capacitance performance coupled with the facile synthesis of PCM/PANI indicates it is a promising electrode material for supercapacitors.

Novel aminohydrazide cross-linked chitosan filled with multi-walled carbon nanotubes as antimicrobial agents.

PubMed

Mohamed, Nadia A; Abd El-Ghany, Nahed A

2018-04-21

Four chemically modified chitosan derivatives 1-4 were designed and synthesized via a series of four reactions; first by reaction with benzaldehyde to protect its amino groups (Derivative 1), second by reaction with epichlorohydrine (Derivative 2), third by reaction with aminobenzhydrazide (Derivative 3), and forth by removing of benzaldehyde to restore the free amino groups on the chitosan (Derivative 4). Two multi-walled carbon nanotube (MWCNT) biocomposites based on Derivative 4 were also prepared. The structure of the prepared derivatives and MWCNT composites was elucidated using elemental analyses, FTIR, XRD, SEM and TEM. The modified chitosan derivatives and MWCNT composites showed better antimicrobial activities than that of chitosan against Enterococcus faecalis, Staphylococcus epidermidis, Escherichia coli, Aspergillus niger, Cryptococcus neoformans and Candida tropicalis as judged by their higher inhibition zone diameters using the agar well diffusion technique. These derivatives and MWCNT composites are more potent against Gram-positive bacteria than against Gram-negative bacteria. The MWCNT composites displayed comparable or even better antimicrobial activities than the reference bactericides or fungicides. Thus, structural modification of chitosan through combination with functionalized moieties and MWCNTs in one system was taken as a way to achieve promising templates for antimicrobial agents and to be appropriate candidates for medical applications. Copyright © 2018 Elsevier B.V. All rights reserved.

Preparation, characterisation and study of in vitro biologically active azamacrocyclic Cu(II) dicarboxylate complexes

NASA Astrophysics Data System (ADS)

Antonijević-Nikolić, Mirjana; Antić-Stanković, Jelena; Tanasković, Sladjana B.; Korabik, Maria J.; Gojgić-Cvijović, Gordana; Vučković, Gordana

2013-12-01

New cationic Cu(II) complexes with N, N‧, N″, N″‧-tetrakis(2-pyridylmethyl)-1,4,8,11-tetraazacyclotetradecane (tpmc) and aliphatic dicarboxylic acids: pentanedioic (glutaric acid = glutH2), hexanedioic acid (adipic acid = adipH2) and decanedioic acid (sebacic acid = sebH2) of general formula [Cu4(L)(tpmc)2](ClO4)6·xH2O, L = glut, x = 2; L = adip, x = 7; L = seb, x = 6 were isolated. Their composition and charges are proposed based on elemental analyses and molar conductivity measurements. By the comparison of their UV-Vis, reflectance, FTIR and EPR spectral data, CV and SQUID magnetic measurements, with those for the complex with butanedioic acid (succinic acid = succH2) of known molecular structure and analysis of LC/MS spectra, geometry with two [Cu2tpmc]4+ units bridged by dicarboxylate dianion engaging all oxygens is proposed. Within units, Cu(II) ions are also bridged with N portion of cyclam ring. All four complexes were screened to in vitro antimicrobial and cytotoxic activity along with free primary and secondary ligands, Cu(II) salt and solvent controls. Detected antibacterial and cytotoxic activity for the complexes was enhanced in most cases than the corresponding controls.

Molecular structure and spectral properties of ethyl 3-quinolinecarboxylate (E3Q) and [Ag(E3Q)2(TCA)] complex (TCA = Trichloroacetate)

NASA Astrophysics Data System (ADS)

Soliman, Saied M.; Kassem, Taher S.; Badr, Ahmed M. A.; Abou Youssef, Morsy A.; Assem, Rania

2014-09-01

A new [Ag(E3Q)2(TCA)] complex; (E3Q = Ethyl 3-quinolinecarboxylate and TCA = Trichloroacetate) has been synthesized and characterized using elemental analysis, FTIR, NMR and mass spectroscopy. The molecular geometry and spectroscopic properties of the complex as well as the free ligand have been calculated using the hybrid B3LYP method. The calculations predicted a distorted tetrahedral arrangement around Ag(I) ion. The vibrational spectra of the studied compounds have been assigned using potential energy distribution (PED). TD-DFT method was used to predict the electronic absorption spectra. The most intense absorption band showed a bathochromic shift and lowering of intensity in case of the complex (233.7 nm, f = 0.5604) compared to E3Q (λmax = 228.0 nm, f = 0.9072). The calculated 1H NMR chemical shifts using GIAO method showed good correlations with the experimental data. The computed dipole moment, polarizability and HOMO-LUMO energy gap were used to predict the nonlinear optical (NLO) properties. It is found that Ag(I) enhances the NLO activity. The natural bond orbital (NBO) analyses were used to elucidate the intramolecular charge transfer interactions causing stabilization for the investigated systems.

Synthesis, characterization, spectrophotometric, structural and antimicrobial studies of the newly charge transfer complex of p-phenylenediamine with π acceptor picric acid.

PubMed

Khan, Ishaat M; Ahmad, Afaq; Oves, M

2010-12-01

Charge transfer complex (CTC) of donor, p-phenylenediamine (PPD) and acceptor, 2,4,6-trinitrophenol (picric acid) has been studied in methanol at room temperature. The CT complex was synthesized and characterized by elemental analysis, FTIR spectra, 1H NMR spectroscopy and electronic absorption spectra which indicate the CT interaction associated with proton migration from the acceptor to the donor followed by hydrogen bonding via N+-H⋯O-. The thermal stability of CT complex was studied using TGA and DTA analyses techniques. The CT complex was screened for its antifungal activity against Aspergillus niger (Laboratory isolate), Candida albicans (IQA-109) and Penicillium sp. (Laboratory isolate) and antibacterial activity against two Gram-positive bacteria Staphylococcus aureus (MSSA 22) and Bacillus subtilis (ATCC 6051) and two Gram-negative bacteria Escherichia coli (K 12) and Pseudomonas aeruginosa (MTCC 2488). It gives good antimicrobial activity. The stoichiometry of the CT complex was found to be 1:1. The physical parameters of CT complex were evaluated by the Benesi-Hildebrand equation. On the basis of the studies, the structure of CT complex is [(PPDH)+(PA)-], and a general mechanism for its formation is proposed. Copyright © 2010 Elsevier B.V. All rights reserved.

Molecular and Immunological Characterization of Ragweed (Ambrosia artemisiifolia L.) Pollen after Exposure of the Plants to Elevated Ozone over a Whole Growing Season

PubMed Central

Kanter, Ulrike; Heller, Werner; Durner, Jörg; Winkler, J. Barbro; Engel, Marion; Behrendt, Heidrun; Holzinger, Andreas; Braun, Paula; Hauser, Michael; Ferreira, Fatima; Mayer, Klaus; Pfeifer, Matthias; Ernst, Dieter

2013-01-01

Climate change and air pollution, including ozone is known to affect plants and might also influence the ragweed pollen, known to carry strong allergens. We compared the transcriptome of ragweed pollen produced under ambient and elevated ozone by 454-sequencing. An enzyme-linked immunosorbent assay (ELISA) was carried out for the major ragweed allergen Amb a 1. Pollen surface was examined by scanning electron microscopy and attenuated total reflectance–Fourier transform infrared spectroscopy (ATR-FTIR), and phenolics were analysed by high-performance liquid chromatography. Elevated ozone had no influence on the pollen size, shape, surface structure or amount of phenolics. ATR-FTIR indicated increased pectin-like material in the exine. Transcriptomic analyses showed changes in expressed-sequence tags (ESTs), including allergens. However, ELISA indicated no significantly increased amounts of Amb a 1 under elevated ozone concentrations. The data highlight a direct influence of ozone on the exine components and transcript level of allergens. As the total protein amount of Amb a 1 was not altered, a direct correlation to an increased risk to human health could not be derived. Additional, the 454-sequencing contributes to the identification of stress-related transcripts in mature pollen that could be grouped into distinct gene ontology terms. PMID:23637846

Processing and optical characterization of lead calcium titanate borosilicate glass doped with germanium

NASA Astrophysics Data System (ADS)

Gautam, C. R.; Das, Sangeeta; Gautam, S. S.; Madheshiya, Abhishek; Singh, Anod Kumar

2018-04-01

In this study, various compositions of lead calcium titanate borosilicate glass doped with a fixed amount of germanium were synthesized using the rapid melt quench technique. The amorphous nature of the synthesized glass was confirmed by X-ray diffraction and scanning electron microscopy analyses. The structural and optical properties were deduced using Raman, Fourier transform infrared (FTIR), and ultraviolet-visible (UV-Vis) spectroscopy. FTIR spectroscopy confirmed the presence of borate groups in triangular and tetrahedral coordination. Infrared and Raman analyses detected the vibrational bonds of Gesbnd Osbnd Ge, Bsbnd Osbnd Ge, Sisbnd Osbnd Ge, Sisbnd Osbnd Si, and Pbsbnd Osbnd Ge. The energy band gaps were evaluated for the prepared glass samples based on Tauc plots of the UV-Vis spectra. The calculated values of the optical band gap decreased from 2.91 to 2.85 eV as the PbO content increased from x = 0.0 to x = 0.7. Furthermore, the Urbach energy was studied based on the UV-Vis results to confirm the disordered structure of the glass. The calculated densities of the glass samples (1.5835 g/cm3 to 3.9184 g/cm3) increased as the concentration of PbO increased, whereas they decreased with the molar volume.

Enzymatic Purification of Microplastics in Environmental Samples.

PubMed

Löder, Martin G J; Imhof, Hannes K; Ladehoff, Maike; Löschel, Lena A; Lorenz, Claudia; Mintenig, Svenja; Piehl, Sarah; Primpke, Sebastian; Schrank, Isabella; Laforsch, Christian; Gerdts, Gunnar

2017-12-19

Micro-Fourier transform infrared (micro-FTIR) spectroscopy and Raman spectroscopy enable the reliable identification and quantification of microplastics (MPs) in the lower micron range. Since concentrations of MPs in the environment are usually low, the large sample volumes required for these techniques lead to an excess of coenriched organic or inorganic materials. While inorganic materials can be separated from MPs using density separation, the organic fraction impedes the ability to conduct reliable analyses. Hence, the purification of MPs from organic materials is crucial prior to conducting an identification via spectroscopic techniques. Strong acidic or alkaline treatments bear the danger of degrading sensitive synthetic polymers. We suggest an alternative method, which uses a series of technical grade enzymes for purifying MPs in environmental samples. A basic enzymatic purification protocol (BEPP) proved to be efficient while reducing 98.3 ± 0.1% of the sample matrix in surface water samples. After showing a high recovery rate (84.5 ± 3.3%), the BEPP was successfully applied to environmental samples from the North Sea where numbers of MPs range from 0.05 to 4.42 items m -3 . Experiences with different environmental sample matrices were considered in an improved and universally applicable version of the BEPP, which is suitable for focal plane array detector (FPA)-based micro-FTIR analyses of water, wastewater, sediment, biota, and food samples.

Air-water ‘tornado’-type microwave plasmas applied for sugarcane biomass treatment

NASA Astrophysics Data System (ADS)

Bundaleska, N.; Tatarova, E.; Dias, F. M.; Lino da Silva, M.; Ferreira, C. M.; Amorim, J.

2014-02-01

The production of cellulosic ethanol from sugarcane biomass is an attractive alternative to the use of fossil fuels. Pretreatment is needed to separate the cellulosic material, which is packed with hemicellulose and lignin in cell wall of sugarcane biomass. A microwave ‘tornado’-type air-water plasma source operating at 2.45 GHz and atmospheric pressure has been applied for this purpose. Samples of dry and wet biomass (˜2 g) have been exposed to the late afterglow plasma stream. The experiments demonstrate that the air-water highly reactive plasma environment provides a number of long-lived active species able to destroy the cellulosic wrapping. Scanning electron microscopy has been applied to analyse the morphological changes occurring due to plasma treatment. The effluent gas streams have been analysed by Fourier-transform infrared spectroscopy (FT-IR). Optical emission spectroscopy and FT-IR have been applied to determine the gas temperature in the discharge and late afterglow plasma zones, respectively. The optimal range of the operational parameters is discussed along with the main active species involved in the treatment process. Synergistic effects can result from the action of singlet O2(a 1Δg) oxygen, NO2, nitrous acid HNO2 and OH hydroxyl radical.

Rapid, accurate, and comparative differentiation of clinically and industrially relevant microorganisms via multiple vibrational spectroscopic fingerprinting.

PubMed

Muhamadali, Howbeer; Subaihi, Abdu; Mohammadtaheri, Mahsa; Xu, Yun; Ellis, David I; Ramanathan, Rajesh; Bansal, Vipul; Goodacre, Royston

2016-08-15

Despite the fact that various microorganisms (e.g., bacteria, fungi, viruses, etc.) have been linked with infectious diseases, their crucial role towards sustaining life on Earth is undeniable. The huge biodiversity, combined with the wide range of biochemical capabilities of these organisms, have always been the driving force behind their large number of current, and, as of yet, undiscovered future applications. The presence of such diversity could be said to expedite the need for the development of rapid, accurate and sensitive techniques which allow for the detection, differentiation, identification and classification of such organisms. In this study, we employed Fourier transform infrared (FT-IR), Raman, and surface enhanced Raman scattering (SERS) spectroscopies, as molecular whole-organism fingerprinting techniques, combined with multivariate statistical analysis approaches for the classification of a range of industrial, environmental or clinically relevant bacteria (P. aeruginosa, P. putida, E. coli, E. faecium, S. lividans, B. subtilis, B. cereus) and yeast (S. cerevisiae). Principal components-discriminant function analysis (PC-DFA) scores plots of the spectral data collected from all three techniques allowed for the clear differentiation of all the samples down to sub-species level. The partial least squares-discriminant analysis (PLS-DA) models generated using the SERS spectral data displayed lower accuracy (74.9%) when compared to those obtained from conventional Raman (97.8%) and FT-IR (96.2%) analyses. In addition, whilst background fluorescence was detected in Raman spectra for S. cerevisiae, this fluorescence was quenched when applying SERS to the same species, and conversely SERS appeared to introduce strong fluorescence when analysing P. putida. It is also worth noting that FT-IR analysis provided spectral data of high quality and reproducibility for the whole sample set, suggesting its applicability to a wider range of samples, and perhaps the most suitable for the analysis of mixed cultures in future studies. Furthermore, our results suggest that while each of these spectroscopic approaches may favour different organisms (sample types), when combined, they would provide complementary and more in-depth knowledge (structural and/or metabolic state) of biological systems. To the best of our knowledge, this is the first time that such a comparative and combined spectroscopic study (using FT-IR, Raman and SERS) has been carried out on microbial samples.

Life assessment of structural components using inelastic finite element analyses

NASA Technical Reports Server (NTRS)

Arya, Vinod K.; Halford, Gary R.

1993-01-01

The need for enhanced and improved performance of structural components subject to severe cyclic thermal/mechanical loadings, such as in the aerospace industry, requires development of appropriate solution technologies involving time-dependent inelastic analyses. Such analyses are mandatory to predict local stress-strain response and to assess more accurately the cyclic life time of structural components. The NASA-Lewis Research Center is cognizant of this need. As a result of concerted efforts at Lewis during the last few years, several such finite element solution technologies (in conjunction with the finite element program MARC) were developed and successfully applied to numerous uniaxial and multiaxial problems. These solution technologies, although developed for use with MARC program, are general in nature and can easily be extended for adaptation with other finite element programs such as ABAQUS, ANSYS, etc. The description and results obtained from two such inelastic finite element solution technologies are presented. The first employs a classical (non-unified) creep-plasticity model. An application of this technology is presented for a hypersonic inlet cowl-lip problem. The second of these technologies uses a unified creep-plasticity model put forth by Freed. The structural component for which this finite element solution technology is illustrated, is a cylindrical rocket engine thrust chamber. The advantages of employing a viscoplastic model for nonlinear time-dependent structural analyses are demonstrated. The life analyses for cowl-lip and cylindrical thrust chambers are presented. These analyses are conducted by using the stress-strain response of these components obtained from the corresponding finite element analyses.

Reporting of meta-analyses of randomized controlled trials with a focus on drug safety: an empirical assessment.

PubMed

Hammad, Tarek A; Neyarapally, George A; Pinheiro, Simone P; Iyasu, Solomon; Rochester, George; Dal Pan, Gerald

2013-01-01

Due to the sparse nature of serious drug-related adverse events (AEs), meta-analyses combining data from several randomized controlled trials (RCTs) to evaluate drug safety issues are increasingly being conducted and published, influencing clinical and regulatory decision making. Evaluation of meta-analyses involves the assessment of both the individual constituent trials and the approaches used to combine them. The Preferred Reporting Items for Systematic Reviews and Meta-Analyses (PRISMA) reporting framework is designed to enhance the reporting of systematic reviews and meta-analyses. However, PRISMA may not cover all critical elements useful in the evaluation of meta-analyses with a focus on drug safety particularly in the regulatory-public health setting. This work was conducted to (1) evaluate the adherence of a sample of published drug safety-focused meta-analyses to the PRISMA reporting framework, (2) identify gaps in this framework based on key aspects pertinent to drug safety, and (3) stimulate the development and validation of a more comprehensive reporting tool that incorporates elements unique to drug safety evaluation. We selected a sample of meta-analyses of RCTs based on review of abstracts from high-impact journals as well as top medical specialty journals between 2009 and 2011. We developed a preliminary reporting framework based on PRISMA with specific additional reporting elements critical for the evaluation of drug safety meta-analyses of RCTs. The reporting of pertinent elements in each meta-analysis was reviewed independently by two authors; discrepancies in the independent evaluations were resolved through discussions between the two authors. A total of 27 meta-analyses, 12 from highest impact journals, 13 from specialty medical journals, and 2 from Cochrane reviews, were identified and evaluated. The great majority (>85%) of PRISMA elements were addressed in more than half of the meta-analyses reviewed. However, the majority of meta-analyses (>60%) did not address most (>80%) of the additional reporting elements critical for the evaluation of drug safety. Some of these elements were not addressed in any of the reviewed meta-analyses. This review included a sample of meta-analyses, with a focus on drug safety, recently published in high-impact journals; therefore, we may have underestimated the extent of the reporting problem across all meta-analyses of drug safety. Furthermore, temporal trends in reporting could not be evaluated in this review because of the short time interval selected. While the majority of PRISMA elements were addressed by most studies reviewed, the majority of studies did not address most of the additional safety-related elements. These findings highlight the need for the development and validation of a drug safety reporting framework and the importance of the current initiative by the Council for International Organizations of Medical Sciences (CIOMS) to create a guidance document for drug safety information synthesis/meta-analysis, which may improve reporting, conduct, and evaluation of meta-analyses of drug safety and inform clinical and regulatory decision making.

An integrated micro-volume fiber-optic sensor for oxygen determination in exhaled breath based on iridium(III) complexes immobilized in fluorinated xerogels.

PubMed

Xiong, Yan; Ye, Zhongbin; Xu, Jing; Zhu, Yuanqiang; Chen, Chen; Guan, Yafeng

2013-03-21

A novel integrated fiber-optic sensor with micro detection volume is developed and evaluated for O(2) determination on a breath-by-breath basis in human health monitoring applications. The sensing element was fabricated by dip-coating an uncladded optical fiber with [Ir(piq)(2)(acac)]-doped hybrid fluorinated ORMOSIL (organically modified silicate) film, which was prepared from 3,3,3-trifluoropropyltrimethoxysilane (TFP-TriMOS) and n-propyltrimethoxysilane (n-propyl-TriMOS). The sensor was then constructed by inserting the prepared optical fiber into a transparent capillary. A microchannel formed between the optical fiber and the capillary inner wall acted as a flow cell for the sample flowing through. The evanescent wave (EW) field produced on the fiber core surface can excite the O(2)-sensitive fluorophores of [Ir(piq)(2)(acac)] to produce emission fluorescence. O(2) can be sensed by its quenching effect on the emission fluorescence intensity. Spectroscopic properties have been characterized by FTIR and fluorescence measurements. Stern-Volmer and Demas models were both employed to analyse the sensor sensitivity, which is 13.0 with the LOD = 0.009% (3σ) and the response time is about 1 s. By integrating the sensing and detection elements on the optical fiber, the novel configuration showed advantages of easy fabrication and low cost. Parameters of sensitivity, response time, repeatability, humidity effect and temperature effect were discussed in detail. The proposed sensor showed potential for practical in-breath O(2) analysis application due to its advantages of easy fabrication, low cost, fast response, excellent hydrophobicity, negligible temperature interference and suitable sensitivity.

Low temperature and UV curable sol-gel coatings for long lasting optical fiber biosensors

NASA Astrophysics Data System (ADS)

Otaduy, D.; Villar, A.; Gomez-Herrero, E.; Goitandia, A. M.; Gorritxategi, E.; Quintana, I.

2010-04-01

The use of optical fibers as sensing element is increasing in clinical, pharmaceutical and industrial applications. Excellent light delivery, long interaction length, low cost and ability not only to excite the target molecules but also to capture the emitted light from the targets are the hallmarks of optical fiber as biosensors. In biosensors based on fiber optics the interaction with the analyte can occur within an element of the optical fiber. One of the techniques for this kind of biosensors is to remove the fiber optic cladding and substitute it for biological coatings that will interact with the parameter to sensorize. The deposition of these layers can be made by sol-gel technology. The sol-gel technology is being increasingly used mainly due to the high versatility to tailor their optical features. Incorporation of suitable chemical and biochemical sensing agents have allowed determining pH, gases, and biochemical species, among others. Nonetheless, the relatively high processing temperatures and short lifetime values mean severe drawbacks for a successful exploitation of sol-gel based coated optical fibres. With regard to the latter, herein we present the design, preparation and characterization of novel sol-gel coated optical fibres. Low temperature and UV curable coating formulations were optimized to achieve a good adhesion and optical performance. The UV photopolymerizable formulation was comprised by glycidoxypropyltrimethoxysilane (GLYMO), Tetraethylorthosilicate (TEOS) and an initiator. While the thermoset coating was prepared by using 3-aminopropyltrimethoxysilane, GLYMO, and TEOS as main reagents. Both curable sol-gel coated fibres were analysed by FTIR, SEM and optical characterization. Furthermore, in the present work a new technique for silica cladding removal has been developed by ultra-short pulses laser processing, getting good dimensional accuracy and surface integrity.

Study of optical properties of BaMn1-xCrxO3 (x=0.0, 0.1, 0.2, 0.3, 0.4, 0.5) manganites using microwave synthesis method

NASA Astrophysics Data System (ADS)

Rani, Reena; Yadav, Kamlesh

2015-08-01

Barium manganite (BaMnO3), a perovskite based material, has been studied extensively. BaMnO3 properties can be changed by doping different elements at manganese (Mn) lattice site. We have prepared BaMnO3 and BaMn1-xCrxO3 (x=0.1, 0.2, 0.3, 0.4, 0.5) by Microwave Synthesizer. Data obtained from Fourier Transform Infrared Spectroscopy (FTIR) that the band gap of pure BaMnO3 is less as compare to the Cr doped BaMnO3. It is also clear from the FTIR that the band gap decreased with increasing the concentration of chromium. Broaden peak at 3201 cm-1 correspond to the stretching vibration of hydroxyl group (OH or H2O). The peaks appear on 724, 863 and 974 cm-1 is corresponding to the stretching vibration of metal oxide (M-O) bonds in the BaMnO3. BaMnO3 have applications in memory storage devices.

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

PubMed Central

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

2013-01-01

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

Comparison of aldehyde emissions simulation with FTIR measurements in the exhaust of a spark ignition engine fueled by ethanol

NASA Astrophysics Data System (ADS)

Zarante, Paola Helena Barros; Sodré, José Ricardo

2018-07-01

This work presents a numerical simulation model for aldehyde formation and exhaust emissions from ethanol-fueled spark ignition engines. The aldehyde simulation model was developed using FORTRAN software, with the input data obtained from the dedicated engine cycle simulation software AVL BOOST. The model calculates formaldehyde and acetaldehyde concentrations from post-flame partial oxidation of methane, ethane and unburned ethanol. The calculated values were compared with experimental data obtained from a mid-size sedan powered by a 1.4-l spark ignition engine, tested on a chassis dynamometer. Exhaust aldehyde concentrations were determined using a Fourier Transform Infrared (FTIR) Spectroscopy analyzer. In general, the results demonstrate that the concentrations of aldehydes and the source elements increased with engine speed and exhaust gas temperature. The measured acetaldehyde concentrations showed values from 3 to 6 times higher than formaldehyde in the range studied. The model could predict reasonably well the qualitative experimental trends, with the quantitative results showing a maximum discrepancy of 39% for acetaldehyde concentration and 21 ppm for exhaust formaldehyde.

Comparison of aldehyde emissions simulation with FTIR measurements in the exhaust of a spark ignition engine fueled by ethanol

NASA Astrophysics Data System (ADS)

Zarante, Paola Helena Barros; Sodré, José Ricardo

2018-02-01

This work presents a numerical simulation model for aldehyde formation and exhaust emissions from ethanol-fueled spark ignition engines. The aldehyde simulation model was developed using FORTRAN software, with the input data obtained from the dedicated engine cycle simulation software AVL BOOST. The model calculates formaldehyde and acetaldehyde concentrations from post-flame partial oxidation of methane, ethane and unburned ethanol. The calculated values were compared with experimental data obtained from a mid-size sedan powered by a 1.4-l spark ignition engine, tested on a chassis dynamometer. Exhaust aldehyde concentrations were determined using a Fourier Transform Infrared (FTIR) Spectroscopy analyzer. In general, the results demonstrate that the concentrations of aldehydes and the source elements increased with engine speed and exhaust gas temperature. The measured acetaldehyde concentrations showed values from 3 to 6 times higher than formaldehyde in the range studied. The model could predict reasonably well the qualitative experimental trends, with the quantitative results showing a maximum discrepancy of 39% for acetaldehyde concentration and 21 ppm for exhaust formaldehyde.

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

PubMed

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

2015-12-05

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

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

NASA Astrophysics Data System (ADS)

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

2018-03-01

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

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

PubMed

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

2016-01-01

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

Impact of gamma radiation on the eruption rate of rat incisors

NASA Astrophysics Data System (ADS)

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

2015-09-01

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

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

PubMed

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

2017-09-12

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

Molecular layer deposition of alucone films using trimethylaluminum and hydroquinone

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

Choudhury, Devika; Sarkar, Shaibal K., E-mail: shaibal.sarkar@iitb.ac.in; Mahuli, Neha

2015-01-01

A hybrid organic–inorganic polymer film grown by molecular layer deposition (MLD) is demonstrated here. Sequential exposures of trimethylaluminum [Al(CH{sub 3}){sub 3}] and hydroquinone [C{sub 6}H{sub 4}(OH){sub 2}] are used to deposit the polymeric films, which is a representative of a class of aluminum oxide polymers known as “alucones.” In-situ quartz crystal microbalance (QCM) studies are employed to determine the growth characteristics. An average growth rate of 4.1 Å per cycle at 150 °C is obtained by QCM and subsequently verified with x-ray reflectivity measurements. Surface chemistry during each MLD-half cycle is studied in depth by in-situ Fourier transform infrared (FTIR) vibrationmore » spectroscopy. Self limiting nature of the reaction is confirmed from both QCM and FTIR measurements. The conformal nature of the deposit, typical for atomic layer deposition and MLD, is verified with transmission electron microscopy imaging. Secondary ion mass spectroscopy measurements confirm the uniform elemental distribution along the depth of the films.« less

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

NASA Astrophysics Data System (ADS)

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

2012-06-01

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

Effect of Sn on the oxide subscale structure formed on a 3% Si steel

NASA Astrophysics Data System (ADS)

Cesar, Maria das G. M. M.; Silveira, Carolina C.; Paolinelli, Sebastião C.; Cicale, Stefano

2018-04-01

Addition of tin in 3% Si steel is a method to improve magnetic properties since tin in steel is known as an element that segregates at grain boundaries, inhibits grain growth and has a dragging effect on grain boundary movement. However, tin is generally known as an element that has a harmful effect on surface coating properties. The oxide subscale formed on the decarburization annealing of a 3% Si steel containing tin was investigated by SEM, EDS, GDS and FTIR. The forsterite film was evaluated by SEM, EDS and GDS. The higher tin content decreased thickness, oxygen and fayalite/silica ratio in the subscale and resulted into a discontinuous forsterite film with poor oxidation resistance. After secondary coating the samples presented a reddish color due to the formation of iron oxide and poor dielectric property.

Boundary element analyses for sound transmission loss of panels.

PubMed

Zhou, Ran; Crocker, Malcolm J

2010-02-01

The sound transmission characteristics of an aluminum panel and two composite sandwich panels were investigated by using two boundary element analyses. The effect of air loading on the structural behavior of the panels is included in one boundary element analysis, by using a light-fluid approximation for the eigenmode series to evaluate the structural response. In the other boundary element analysis, the air loading is treated as an added mass. The effect of the modal energy loss factor on the sound transmission loss of the panels was investigated. Both boundary element analyses were used to study the sound transmission loss of symmetric sandwich panels excited by a random incidence acoustic field. A classical wave impedance analysis was also used to make sound transmission loss predictions for the two foam-filled honeycomb sandwich panels. Comparisons between predictions of sound transmission loss for the two foam-filled honeycomb sandwich panels excited by a random incidence acoustic field obtained from the wave impedance analysis, the two boundary element analyses, and experimental measurements are presented.

Mode of action studies on the formation of enamel minerals from a novel toothpaste containing calcium silicate and sodium phosphate salts.

PubMed

Sun, Yuekui; Li, Xiaoke; Deng, Yan; Sun, Jianing N; Tao, DanYing; Chen, Hui; Hu, Qinghong; Liu, Renjiang; Liu, Weining; Feng, Xiping; Wang, Jinfang; Carvell, Mel; Joiner, Andrew

2014-06-01

To investigate in vitro and in situ the deposition and formation of hydroxyapatite (HAP) on enamel surfaces following brushing with a novel toothpaste containing calcium silicate (CaSi), sodium phosphate salts and fluoride. Polished enamel blocks were brushed in vitro with a slurry of the CaSi toothpaste. After one brush and four weeks simulated brushing the enamel surfaces were analysed. In an in situ protocol, enamel blocks were attached to first or second molar teeth of healthy subjects, exposed to 4 weeks twice per day brushing with the CaSi toothpaste and then analysed. The surface deposits were analysed using scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), transmission electron microscopy (TEM) and selected area electron diffraction (SAED). In addition, the CaSi toothpaste was slurried in simulated oral fluid (SOF) over a 3 hour period and the solids were isolated and analysed by Fourier transform infrared spectroscopy (FTIR). The FTIR study demonstrated that calcium phosphate phases had formed and these became increasingly crystalline over 3 hours. CaSi was deposited onto enamel surfaces following one brushing with the toothpaste in vitro.The deposited particles showed evidence of HAP crystalline phases associated with the CaSi. Following 4 weeks brushing in vitro, the deposition increased and analyses showed that the deposited material was HAP. These results were confirmed by the in situ study. Calcium silicate can be deposited onto enamel surfaces from a novel toothpaste formulation where it can form the enamel mineral HAP. A novel toothpaste formulation containing CaSi can form HAP on enamel surfaces. The potential of this technology is for a novel approach to the repair of demineralised enamel and the protection of enamel during acid exposure. © 2014 Elsevier Ltd. All rights reserved.

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.

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.

A simple, sensitive and non-destructive technique for characterizing bovine dental enamel erosion: attenuated total reflection Fourier transform infrared spectroscopy

PubMed Central

Kim, In-Hye; Son, Jun Sik; Min, Bong Ki; Kim, Young Kyoung; Kim, Kyo-Han; Kwon, Tae-Yub

2016-01-01

Although many techniques are available to assess enamel erosion in vitro, a simple, non-destructive method with sufficient sensitivity for quantifying dental erosion is required. This study characterized the bovine dental enamel erosion induced by various acidic beverages in vitro using attenuated total reflection Fourier transform infrared (ATR-FTIR) spectroscopy. Deionized water (control) and 10 acidic beverages were selected to study erosion, and the pH and neutralizable acidity were measured. Bovine anterior teeth (110) were polished with up to 1 200-grit silicon carbide paper to produce flat enamel surfaces, which were then immersed in 20 mL of the beverages for 30 min at 37 °C. The degree of erosion was evaluated using ATR-FTIR spectroscopy and Vickers' microhardness measurements. The spectra obtained were interpreted in two ways that focused on the ν1, ν3 phosphate contour: the ratio of the height amplitude of ν3 PO4 to that of ν1 PO4 (Method 1) and the shift of the ν3 PO4 peak to a higher wavenumber (Method 2). The percentage changes in microhardness after the erosion treatments were primarily affected by the pH of the immersion media. Regression analyses revealed highly significant correlations between the surface hardness change and the degree of erosion, as detected by ATR-FTIR spectroscopy (P<0.001). Method 1 was the most sensitive to these changes, followed by surface hardness change measurements and Method 2. This study suggests that ATR-FTIR spectroscopy is potentially advantageous over the microhardness test as a simple, non-destructive, sensitive technique for the quantification of enamel erosion. PMID:27025266

A simple, sensitive and non-destructive technique for characterizing bovine dental enamel erosion: attenuated total reflection Fourier transform infrared spectroscopy.

PubMed

Kim, In-Hye; Son, Jun Sik; Min, Bong Ki; Kim, Young Kyoung; Kim, Kyo-Han; Kwon, Tae-Yub

2016-03-30

Although many techniques are available to assess enamel erosion in vitro, a simple, non-destructive method with sufficient sensitivity for quantifying dental erosion is required. This study characterized the bovine dental enamel erosion induced by various acidic beverages in vitro using attenuated total reflection Fourier transform infrared (ATR-FTIR) spectroscopy. Deionized water (control) and 10 acidic beverages were selected to study erosion, and the pH and neutralizable acidity were measured. Bovine anterior teeth (110) were polished with up to 1 200-grit silicon carbide paper to produce flat enamel surfaces, which were then immersed in 20 mL of the beverages for 30 min at 37 °C. The degree of erosion was evaluated using ATR-FTIR spectroscopy and Vickers' microhardness measurements. The spectra obtained were interpreted in two ways that focused on the ν1, ν3 phosphate contour: the ratio of the height amplitude of ν3 PO4 to that of ν1 PO4 (Method 1) and the shift of the ν3 PO4 peak to a higher wavenumber (Method 2). The percentage changes in microhardness after the erosion treatments were primarily affected by the pH of the immersion media. Regression analyses revealed highly significant correlations between the surface hardness change and the degree of erosion, as detected by ATR-FTIR spectroscopy (P<0.001). Method 1 was the most sensitive to these changes, followed by surface hardness change measurements and Method 2. This study suggests that ATR-FTIR spectroscopy is potentially advantageous over the microhardness test as a simple, non-destructive, sensitive technique for the quantification of enamel erosion.

Quantification of polyhydroxyalkanoates in mixed and pure cultures biomass by Fourier transform infrared spectroscopy: comparison of different approaches.

PubMed

Isak, I; Patel, M; Riddell, M; West, M; Bowers, T; Wijeyekoon, S; Lloyd, J

2016-08-01

Fourier transform infrared (FTIR) spectroscopy was used in this study for the rapid quantification of polyhydroxyalkanoates (PHA) in mixed and pure culture bacterial biomass. Three different statistical analysis methods (regression, partial least squares (PLS) and nonlinear) were applied to the FTIR data and the results were plotted against the PHA values measured with the reference gas chromatography technique. All methods predicted PHA content in mixed culture biomass with comparable efficiency, indicated by similar residuals values. The PHA in these cultures ranged from low to medium concentration (0-44 wt% of dried biomass content). However, for the analysis of the combined mixed and pure culture biomass with PHA concentration ranging from low to high (0-93% of dried biomass content), the PLS method was most efficient. This paper reports, for the first time, the use of a single calibration model constructed with a combination of mixed and pure cultures covering a wide PHA range, for predicting PHA content in biomass. Currently no one universal method exists for processing FTIR data for polyhydroxyalkanoates (PHA) quantification. This study compares three different methods of analysing FTIR data for quantification of PHAs in biomass. A new data-processing approach was proposed and the results were compared against existing literature methods. Most publications report PHA quantification of medium range in pure culture. However, in our study we encompassed both mixed and pure culture biomass containing a broader range of PHA in the calibration curve. The resulting prediction model is useful for rapid quantification of a wider range of PHA content in biomass. © 2016 The Society for Applied Microbiology.

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

PubMed

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

2013-07-01

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

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

PubMed

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

2016-04-01

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

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

NASA Astrophysics Data System (ADS)

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

2010-01-01

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

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

NASA Astrophysics Data System (ADS)

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

2018-07-01

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

Preparation of polyaniline/PbS core-shell nano/microcomposite and its application for photocatalytic H2 electrogeneration from H2O.

PubMed

Rabia, Mohamed; Mohamed, H S H; Shaban, Mohamed; Taha, S

2018-01-18

Lead sulfide (PbS) and polyaniline (PANI) nano/microparticles were prepared. Then, PANI/PbS core-shell nano/microcomposites (I, II, and III) were prepared by oxidative polymerization of different aniline concentrations (0.01, 0.03, and 0.05 M), respectively, in the presence of 0.05 M PbS. FT-IR, XRD, SEM, HR-TEM, and UV-Vis analyses were carried out to characterize the samples. From the FT-IR data, there are redshifts in PbS and PANI nano/microparticles bands in comparison with PANI/PbS nano/microcomposites. The average crystallite sizes of PANI/PbS core-shell nano/microcomposites (I, II, and III) from XRD analyses were 46.5, 55, and 42.16 nm, respectively. From the optical analyses, nano/microcomposite (II) has the optimum optical properties with two band gaps values of 1.41 and 2.79 eV. Then, the nano/microcomposite (II) membrane electrode supported on ITO glass was prepared and applied on the photoelectrochemical (PEC) H 2 generation from H 2 O. The characteristics current-voltage and current-time behaviors were measured at different wavelengths from 390 to 636 nm. Also, the incident photon-to-current conversion efficiency (IPCE) under monochromatic illumination condition was calculated. The optimum values for IPCE were 36.5 and 35.2% at 390 and 405 nm, respectively. Finally, a simple mechanism for PEC H 2 generation from H 2 O using the nano/microcomposite (II) membrane electrode was mentioned.

Deciphering the groove binding modes of tau-fluvalinate and flumethrin with calf thymus DNA

NASA Astrophysics Data System (ADS)

Tao, Mo; Zhang, Guowen; Pan, Junhui; Xiong, Chunhong

2016-02-01

Tau-fluvalinate (TFL) and flumethrin (FL), widely used in agriculture and a class of synthetic pyrethroid pesticides with a similar structure, may cause a potential security risk. Herein, the modes of binding in vitro of TFL and FL with calf thymus DNA (ctDNA) were characterized by fluorescence, UV-vis absorption, circular dichroism (CD) and Fourier transform infrared (FT-IR) spectroscopy with the aid of viscosity measurements, melting analyses and molecular docking studies. The fluorescence titration indicated that both TFL and FL bound to ctDNA forming complexes through hydrogen bonding and van der Waals forces. The binding constants of TFL and FL with ctDNA were in the range of 104 L mol- 1, and FL exhibited a higher binding propensity than TFL. The iodide quenching effect, single/double-stranded DNA effects, and ctDNA melting and viscosity measurements demonstrated that the binding of both TFL and FL to ctDNA was groove mode. The FT-IR analyses suggested the A-T region of the minor groove of ctDNA as the preferential binding for TFL and FL, which was confirmed by the displacement assays with Hoechst 33258 probe, and the molecular docking visualized the specific binding. The changes in CD spectra indicated that both FL and TFL induced the perturbation on the base stacking and helicity of B-DNA, but the disturbance caused by FL was more obvious. Gel electrophoresis analyses indicated that both TFL and FL did not cause significant DNA cleavage. This study provides novel insights into the binding properties of TFL/FL with ctDNA and its toxic mechanisms.

Trace-element analyses of core samples from the 1967-1988 drillings of Kilauea Iki lava lake, Hawaii

USGS Publications Warehouse

Helz, Rosalind Tuthill

2012-01-01

This report presents previously unpublished analyses of trace elements in drill core samples from Kilauea Iki lava lake and from the 1959 eruption that fed the lava lake. The two types of data presented were obtained by instrumental neutron-activation analysis (INAA) and energy-dispersive X-ray fluorescence analysis (EDXRF). The analyses were performed in U.S. Geological Survey (USGS) laboratories from 1989 to 1994. This report contains 93 INAA analyses on 84 samples and 68 EDXRF analyses on 68 samples. The purpose of the study was to document trace-element variation during chemical differentiation, especially during the closed-system differentiation of Kilauea Iki lava lake.

Study on molecular structure, spectroscopic properties (FTIR and UV-Vis), NBO, QTAIM, HOMO-LUMO energies and docking studies of 5-fluorouracil, a substance used to treat cancer

NASA Astrophysics Data System (ADS)

Almeida, Michell O.; Barros, Daiane A. S.; Araujo, Sheila C.; Faria, Sergio H. D. M.; Maltarollo, Vinicius G.; Honorio, Kathia M.

2017-09-01

Cancer cells can expand to other parts of body through blood system and nodes from a mechanism known as metastasis. Due to the large annual growth of cancer cases, various biological targets have been studied and related to this disorder. A very interesting target related to cancer is human epidermal growth factor receptor 2 (HER2). In this study, we analyzed the main intermolecular interactions between a drug used in the cancer treatment (5-fluorouracil) and HER2. Molecular modeling methods were also employed to assess the molecular structure, spectroscopic properties (FTIR and UV-Vis), NBO, QTAIM and HOMO-LUMO energies of 5-FU. From the docking simulations it was possible to analyze the interactions that occur between some residues in the binding site of HER2 and 5-FU. To validate the choice of basis set that was used in the NBO and QTAIM analyses, theoretical calculations were performed to obtain FT-IR and UV/Vis spectra, and the theoretical results are consistent with the experimental data, showing that the basis set chosen is suitable. For the maximum λ from the theoretical calculation (254.89 nm) of UV/Vis, the electronic transition from HOMO to LUMO occurs at 4.89 eV. From NBO analyses, we observed interactions between Asp863 and 5-FU, i.e. the orbitals with high transfer of electrons are LP O15 (donor NBO) and BD* (π) N1-H10 (acceptor NBO), being that the value of this interaction is 7.72 kcal/mol. Results from QTAIM indicate one main intermolecular H bond, which is necessary to stabilize the complex formed between the ligands and the biological target. Therefore, this study allowed a careful evaluation on the main structural, spectroscopic and electronic properties involved in the interaction between 5-FU and HER2, an important biological complex related to the cancer treatment.

Deposition Uniformity of Coal Dust on Filters and Its Effect on the Accuracy of FTIR Analyses for Silica.

PubMed

Miller, Arthur L; Drake, Pamela L; Murphy, Nathaniel C; Cauda, Emanuele G; LeBouf, Ryan F; Markevicius, Gediminas

Miners are exposed to silica-bearing dust which can lead to silicosis, a potentially fatal lung disease. Currently, airborne silica is measured by collecting filter samples and sending them to a laboratory for analysis. Since this may take weeks, a field method is needed to inform decisions aimed at reducing exposures. This study investigates a field-portable Fourier transform infrared (FTIR) method for end-of-shift (EOS) measurement of silica on filter samples. Since the method entails localized analyses, spatial uniformity of dust deposition can affect accuracy and repeatability. The study, therefore, assesses the influence of radial deposition uniformity on the accuracy of the method. Using laboratory-generated Minusil and coal dusts and three different types of sampling systems, multiple sets of filter samples were prepared. All samples were collected in pairs to create parallel sets for training and validation. Silica was measured by FTIR at nine locations across the face of each filter and the data analyzed using a multiple regression analysis technique that compared various models for predicting silica mass on the filters using different numbers of "analysis shots." It was shown that deposition uniformity is independent of particle type (kaolin vs. silica), which suggests the role of aerodynamic separation is negligible. Results also reflected the correlation between the location and number of shots versus the predictive accuracy of the models. The coefficient of variation (CV) for the models when predicting mass of validation samples was 4%-51% depending on the number of points analyzed and the type of sampler used, which affected the uniformity of radial deposition on the filters. It was shown that using a single shot at the center of the filter yielded predictivity adequate for a field method, (93% return, CV approximately 15%) for samples collected with 3-piece cassettes.

New metal-organic complexes based on bis(tetrazole) ligands: Synthesis, structures and properties

NASA Astrophysics Data System (ADS)

Du, Ceng-Ceng; Fan, Jian-Zhong; Wang, Xin-Fang; Zhou, Sheng-Bin; Wang, Duo-Zhi

2017-04-01

In this paper, a series of new complexes, [Zn2(HL1)2(H2O)4]·H2O (1), [Co2(HL1)2]·TEA (2), [Co3(HL1)2(H2L1)2(H2O)4]n (3), [Cu(HL1)(H2O)2]n (4), {[Cu5(HL2)2(OH)4(ClO4)2]·4H2O}n (5) and [Cu2(L3)]n (6) were successfully prepared by utilizing three bis(tetrazole) ligands [bis-(1H-tetrazol-5-ylmethyl)-amine (H3L1), bis-(1H-tetrazol-5-ylethyl)-amine (H3L2) and 1,5-bis(5-tetrazolo)-3-thiapentane (H2L3)], all of which have been characterized by elemental analyses, FT-IR spectroscopy, powder X-ray diffraction (PXRD), thermogravimetric analyses as well as single-crystal X-ray diffraction analyses showing different dimensionalities (0D, 1D and 3D). Complexes 1 and 2 are 0D structures, 1 shows a dinuclear structure, 2 displays two crystallographically different mononuclear structures, 1 and 2 are further assembled to form 3D supramolecular framework and 2D supramolecular network by hydrogen-bonding interactions, respectively. Complexes 3, 4 and 5 are 1D structures, 3 features a mononuclear unit and a 1D chain, which are arranged into 3D supramolecular architecture by hydrogen-bonding interactions, 4 presents a zigzag chain, 5 shows an infinite chain structure constructed from pentanuclear Cu(II) subunits and ClO4- anions. Complex 6 exhibits a 3D coordination framework based on cyclic [Cu4(L3)2] dimmer subunits as nodes possessing an 8-connected network topology with the point symbol {424·64}. Further, semiconductor behaviors, the solid-state luminescent properties of the complexes 1-3 and 6 were measured and studied seriously at room temperature.

Three reversible polymorphic copper(I) complexes triggered by ligand conformation: insights into polymorphic crystal habit and luminescent properties.

PubMed

Chai, Wenxiang; Hong, Mingwei; Song, Li; Jia, Guohua; Shi, Hongsheng; Guo, Jiayu; Shu, Kangying; Guo, Bing; Zhang, Yicheng; You, Wenwu; Chen, Xueyuan

2015-05-04

Three luminescent polymorphs based on a new copper(I) complex Cu(2-QBO)(PPh3)PF6 (1, PPh3 = triphenylphosphine, 2-QBO = 2-(2'-quinolyl)benzoxazole) have been synthesized and characterized by FT-IR, UV-vis, elemental analyses, and single-crystal X-ray diffraction analyses. Each polymorph can reversibly convert from one to another through appropriate procedures. Interestingly, such interconversion can be distinguished by their intrinsic crystal morphologies and colors (namely α, dark yellow plate, β, orange block, γ, light yellow needle) as well as photoluminescent (PL) properties. X-ray crystal structure analyses of these three polymorphs show three different supramolecular structures from 1D to 3D, which are expected to be responsible for the formation of three different crystal morphologies such as needle, plate, and block. Combination of the experimental data with DFT calculations on these three polymorphs reveals that the polymorphic interconversion is triggered by the conformation isomerization of the 2-QBO ligand and can be successfully controlled by the polarity of the process solvents (affecting the molecular dipole moment) and thermodynamics (affecting the molecular total energy). It is also found that the different crystal colors of polymorphs and their PL properties are derived from different θ values (dihedral angle between benzoxazolyl and quinolyl group of the 2-QBO ligand) and P-Cu-P angles based on TD-DFT calculations. Moreover, an interesting phase interconversion between γ and β has also been found under different temperature, and this result is consistent with the DFT calculations in which the total energy of β is larger than that of γ. This polymorphism provides a good model to study the relationship between the structure and the physical properties in luminescent copper(I) complexes as well as some profound insights into their PL properties.

Identifying fire plumes in the Arctic with tropospheric FTIR measurements and transport models

NASA Astrophysics Data System (ADS)

Viatte, C.; Strong, K.; Hannigan, J.; Nussbaumer, E.; Emmons, L.; Conway, S.; Paton-Walsh, C.; Hartley, J.; Benmergui, J.; Lin, J.

2014-10-01

We investigate Arctic tropospheric composition using ground-based Fourier Transform Infrared (FTIR) solar absorption spectra, recorded at the Polar Environment Atmospheric Research Laboratory (PEARL, Eureka, Nunavut, Canada, 80°5' N, 86°42' W) and at Thule (Greenland, 76°53' N, -68°74' W) from 2008 to 2012. The target species: carbon monoxide (CO), hydrogen cyanide (HCN), ethane (C2H6), acetylene (C2H2), formic acid (HCOOH), and formaldehyde (H2CO) are emitted by biomass burning and can be transported from mid-latitudes to the Arctic. By detecting simultaneous enhancements of three biomass burning tracers (HCN, CO, and C2H6), ten and eight fire events are identified at Eureka and Thule, respectively, within the five-year FTIR timeseries. Analyses of Hybrid Single Particle Lagrangian Integrated Trajectory Model (HYSPLIT) back-trajectories coupled with Moderate Resolution Imaging Spectroradiometer (MODIS) fire hot spot data, Stochastic Time-Inverted Lagrangian Transport model (STILT) footprints, and Ozone Monitoring Instrument (OMI) UV aerosol index maps are used to attribute burning source regions and travel time durations of the plumes. By taking into account the effect of aging of the smoke plumes, measured FTIR enhancement ratios were corrected to obtain emission ratios and equivalent emission factors. The means of emission factors for extratropical forest estimated with the two FTIR datasets are 0.39 ± 0.15 g kg-1 for HCN, 1.23 ± 0.49 g kg-1 for C2H6, 0.34 ± 0.16 g kg-1 for C2H2, 2.13 ± 0.92 g kg-1 for HCOOH, and 3.14 ± 1.28 g kg-1 for CH3OH. To improve our knowledge concerning the dynamical and chemical processes associated with Arctic pollution from fires, the two sets of FTIR measurements were compared to the Model for Ozone and Related chemical Tracers, version 4 (MOZART-4). Seasonal cycles and day-to-day variabilities were compared to assess the ability of the model to reproduce emissions from fires and their transport. Good agreement in winter confirms that transport is well implemented in the model. For C2H6, however, the lower wintertime concentration estimated by the model as compared to the FTIR observations highlight an underestimation of its emission. Results show that modelled and measured total columns are correlated (linear correlation coefficient r > 0.6 for all gases except for H2CO at Eureka and HCOOH at Thule), but suggest a~general underestimation of the concentrations in the model for all seven tropospheric species in the high Arctic.

Identifying fire plumes in the Arctic with tropospheric FTIR measurements and transport models

NASA Astrophysics Data System (ADS)

Viatte, C.; Strong, K.; Hannigan, J.; Nussbaumer, E.; Emmons, L. K.; Conway, S.; Paton-Walsh, C.; Hartley, J.; Benmergui, J.; Lin, J.

2015-03-01

We investigate Arctic tropospheric composition using ground-based Fourier transform infrared (FTIR) solar absorption spectra, recorded at the Polar Environment Atmospheric Research Laboratory (PEARL, Eureka, Nunavut, Canada, 80°05' N, 86°42' W) and at Thule (Greenland, 76°53' N, -68°74' W) from 2008 to 2012. The target species, carbon monoxide (CO), hydrogen cyanide (HCN), ethane (C2H6), acetylene (C2H2), formic acid (HCOOH), and formaldehyde (H2CO) are emitted by biomass burning and can be transported from mid-latitudes to the Arctic. By detecting simultaneous enhancements of three biomass burning tracers (HCN, CO, and C2H6), ten and eight fire events are identified at Eureka and Thule, respectively, within the 5-year FTIR time series. Analyses of Hybrid Single Particle Lagrangian Integrated Trajectory (HYSPLIT) model back-trajectories coupled with Moderate Resolution Imaging Spectroradiometer (MODIS) fire hotspot data, Stochastic Time-Inverted Lagrangian Transport (STILT) model footprints, and Ozone Monitoring Instrument (OMI) UV aerosol index maps, are used to attribute burning source regions and travel time durations of the plumes. By taking into account the effect of aging of the smoke plumes, measured FTIR enhancement ratios were corrected to obtain emission ratios and equivalent emission factors. The means of emission factors for extratropical forest estimated with the two FTIR data sets are 0.40 ± 0.21 g kg-1 for HCN, 1.24 ± 0.71 g kg-1 for C2H6, 0.34 ± 0.21 g kg-1 for C2H2, and 2.92 ± 1.30 g kg-1 for HCOOH. The emission factor for CH3OH estimated at Eureka is 3.44 ± 1.68 g kg-1. To improve our knowledge concerning the dynamical and chemical processes associated with Arctic pollution from fires, the two sets of FTIR measurements were compared to the Model for OZone And Related chemical Tracers, version 4 (MOZART-4). Seasonal cycles and day-to-day variabilities were compared to assess the ability of the model to reproduce emissions from fires and their transport. Good agreement in winter confirms that transport is well implemented in the model. For C2H6, however, the lower wintertime concentration estimated by the model as compared to the FTIR observations highlights an underestimation of its emission. Results show that modeled and measured total columns are correlated (linear correlation coefficient r > 0.6 for all gases except for H2CO at Eureka and HCOOH at Thule), but suggest a general underestimation of the concentrations in the model for all seven tropospheric species in the high Arctic.

Cellular injury evidenced by impedance technology and infrared microspectroscopy

NASA Astrophysics Data System (ADS)

le Roux, K.; Prinsloo, L. C.; Meyer, D.

2015-03-01

Fourier Transform Infrared (FTIR) spectroscopy is finding increasing biological application, for example in the analysis of diseased tissues and cells, cell cycle studies and investigating the mechanisms of action of anticancer drugs. Cancer treatment studies routinely define the types of cell-drug responses as either total cell destruction by the drug (all cells die), moderate damage (cell deterioration where some cells survive) or reversible cell cycle arrest (cytostasis). In this study the loss of viability and related chemical stress experienced by cells treated with the medicinal plant, Plectranthus ciliatus, was investigated using real time cell electronic sensing (RT-CES) technology and FTIR microspectroscopy. The use of plants as medicines is well established and ethnobotany has proven that crude extracts can serve as treatments against various ailments. The aim of this study was to determine whether FTIR microspectroscopy would successfully distinguish between different types of cellular injury induced by a potentially anticancerous plant extract. Cervical adenocarcinoma (HeLa) cells were treated with a crude extract of Pciliatus and cells monitored using RT-CES to characterize the type of cellular responses induced. Cell populations were then investigated using FTIR microspectroscopy and statistically analysed using One-way Analysis of Variance (ANOVA) and Principal Component Analysis (PCA). The plant extract and a cancer drug control (actinomycin D) induced concentration dependent cellular responses ranging from nontoxic, cytostatic or cytotoxic. Thirteen spectral peaks (915 cm-1, 933 cm-1, 989 cm-1, 1192 cm-1, 1369 cm-1, 1437 cm-1, 1450 cm-1, 1546 cm-1, 1634 cm-1, 1679 cm-1 1772 cm-1, 2874 cm-1 and 2962 cm-1) associated with cytotoxicity were significantly (p value < 0.05, one way ANOVA, Tukey test, Bonferroni) altered, while two of the bands were also indicative of early stress related responses. In PCA, poor separation between nontoxic and cytostatic responses was evident while clear separation was linked to cytotoxicity. RT-CES detected morphological changes as indicators of cell injury and could distinguish between viable, cytostatic and cytotoxic responses. FTIR microspectroscopy confirmed that cytostatic cells were viable and could still recover while also describing early cellular stress related responses on a molecular level.

FTIR microspectroscopy and SIMS study of water-poor cordierite from El Hoyazo, Spain: Application to mineral and melt devolatilization

NASA Astrophysics Data System (ADS)

Della Ventura, Giancarlo; Bellatreccia, Fabio; Cesare, Bernardo; Harley, Simon; Piccinini, Massimo

2009-12-01

This paper reports the microchemical and microspectroscopic FTIR study of cordierite from a partially melted graphite-bearing granulitic enclave within the dacitic lava dome of El Hoyazo (SE Spain). Optically transparent single-crystals, hand picked from the rock, were oriented using X-ray diffraction and studied by Fourier-transform infrared (FTIR). Single-crystal FTIR spectroscopy shows that the examined cordierite is CO 2-rich and almost H 2O-free. Two weak and sharp peaks are observed at 3708 and 3595 cm - 1 , respectively, which are strongly polarised for E // a. These peaks are assigned to combination modes of CO 2. Very weak bands due to H 2O molecules oriented with the H…H vector // c (type I water) are occasionally observed in certain zones of the grains, associated with absorptions due to hydrated inclusions of alteration products. The very intense bands observed in the 2600-2000 cm - 1 region are assigned to CO 2 molecules oriented // a; the spectra also show the presence of 13C and 18O, and weak amounts of CO in the sample. Microspectrometric mapping shows that the distribution of C is relatively homogeneous, whereas that of H 2O is complicated by a very broad absorption extending from 3700 to 3100 cm - 1 . High-resolution FTIR imaging, done using a focal-plane array of detectors, shows that this broad absorption is associated with microfractures. SIMS analyses give an average concentration of H 2O = 0.033 ± 0.007 wt.% and CO 2 = 0.21 ± 0.07 wt.%. On the basis of these data, molar absorption coefficients can be calibrated for CO 2: ɛiCO2 (integrated) = 11,000 ± 4000 l/(mol cm - 2 ) and ɛlCO2 (linear) = 800 ± 250 l/(mol cm - 1 ). Due to the extremely low amount of H 2O and its inhomogeneous distribution, calibration of absorption ɛH2O coefficients is unreliable. The very low H 2O contents in the El Hoyazo cordierite indicate continued mineral-melt volatile exchange during decompression from ˜ 5 kbar to significantly shallower levels.

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.

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.

Electrical properties of samarium cobaltite nanoparticles synthesized using Sol–Gel autocombustion route

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

Sathyamoorthy, B.; Md Gazzali, P.M.; Murugesan, C.

2014-05-01

Highlights: • The structural evolution and its electrical properties of samarium cobaltite nanograins are discussed. • Optimization of SmCoO{sub 3} nanograins is achieved by post sintering as-prepared gel at 800 °C. • The impedance spectra indicate the semiconducting behavior SmCoO{sub 3} nanograins. - Abstract: Nanograins of SmCoO{sub 3} are prepared by citric acid assisted Sol–Gel autocombustion route. The characterizations of crystal structure, surface morphology and electrical properties of SmCoO{sub 3} powder are done using XRD, HRSEM, FTIR and BDS. The structural evolution of SmCoO{sub 3} upon increasing the annealing temperature is followed using XRD and FTIR analyses. The powder samplemore » contains polycrystalline grains with average size equal to 35 nm and orthorhombic perovskite structure with Pbnm space group. The vibrational bands observed in FTIR spectrum at 545 cm{sup −1} and 439 cm{sup −1} correspond to Co-O stretching modes in cobaltite system. HRSEM images of the sample show the formation of hexagonal shaped grains of samarium cobaltite. The AC electrical conductivity of 4.914 × 10{sup −5} S cm{sup −1} at 295 K is measured for SmCoO{sub 3} nanoparticles. The impedance spectra bring out the semiconducting behavior of the material.« less

A Sensitive Method for Examining Whole Cell Biochemical Composition in Single Cells of Filamentous Fungi using Synchrotron FTIR Spectromicroscopy

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

Konstantin,J.; Gough, K.; Julian, R.

2008-01-01

Cell function is related to cell composition. The asexual state of filamentous fungi (molds and mildews) has two main life cycle stages: vegetative hyphae for substrate colonization and nutrient acquisition, and asexual spores for survival and dispersal. Hyphal composition changes over a few tens of microns during growth and maturation; spores are different from hyphae. Most biochemical analyses are restricted to studying a few components at high spatial resolution (e.g. histochemistry) or many compounds at low spatial resolution (e.g. GC-MS). Synchrotron FTIR spectromicroscopy can be used to study fungal cell biology by fingerprinting varieties of carbohydrates, proteins, and lipids atmore » about 6 microm spatial resolution. FTIR can distinguish fungal species and changes during hyphal growth, and reveals that even fungi grown under optimal vs mildly stressed conditions exhibit dramatic biochemical changes without obvious morphological effects. Here we compare hypha and spore composition of two fungi, Neurospora and Rhizopus. There are clear biochemical changes when Neurospora hyphae commit to spore development, during spore maturation and following germination, many of which are consistent with results from molecular genetics, but have not been shown before at high spatial resolution. Rhizopus spores develop within a fluid-containing sporangium that becomes dry at maturity. Rhizopus spores had similar protein content and significantly more carbohydrate than the sporangial fluid, both of which are novel findings.« less

Diagnosis of ovarian tumour tissues by SR-FTIR spectroscopy: A pilot study.

PubMed

Grzelak, M M; Wróbel, P M; Lankosz, M; Stęgowski, Z; Chmura, Ł; Adamek, D; Hesse, B; Castillo-Michel, H

2018-05-21

Ovarian cancer is the seventh most common cancer among women across the world with very high mortality rates. Histology is considered the gold standard for tumour diagnosis. FTIR spectroscopy is relies on registering biochemical differences in the samples analysed, including biological specimens. Therefore, the Synchrotron radiation based-Fourier transform infrared spectroscopy (SR-FTIR) was used for the preliminary investigation of the molecular composition of the human, non-fixed ovarian neoplastic tissues with different type of biological potential. The study that was carried out on thin tissue sections, placed on barium fluoride infrared windows, was focused on investigating spatial distribution of the biochemical markers in various ovarian tumours. Since the structural constituents of tissues accumulate different molecules which may correspond to the specific type of ovarian tumours, the main goal of this study was to check if the mean intensities of the spectral lines of some bio-molecules can be treated as ovarian cancer bio-indicators. Moreover, an attempt to identify and understand the underlying biochemical changes associated with the disease was carried out. The major spectral differences in the frequency and intensities were identified as bonds of lipids, protein massif and nucleic acids. The results obtained suggest that Fourier transform infrared spectroscopy can be used as a supporting tool in the analysis of neoplastic ovarian tissue. Copyright © 2018 Elsevier B.V. All rights reserved.

A Fourier-Transform Infrared Study of Biochar Aging in Soils

PubMed Central

Singh, B.; Fang, Y.; Johnston, C.T.

2018-01-01

We used diffuse reflectance Fourier-transform infrared (DR-FTIR) spectroscopy, X-ray diffraction (XRD), and chemical and isotopic analyses to characterize the light fraction of four contrasting soils (control and biocharamended soils) to determine changes in biochar properties after aging. Two Eucalyptus saligna Sm. wood biochars, produced at 450°C (B450) and 550°C (B550), were incubated separately in each of the four soils for up to 12 mo at 20, 40, and 60°C. Total C and isotopic (δ13C) methods were used to quantify the amounts of biochar C and native C mineralized during incubation. The DR-FTIR spectra of the light fraction showed distinct absorption bands representing native soil organic C, biochar C, and mineral constituents present in the soils; the mineral bands were consistent with XRD data of the clay fraction of the four soils. Analysis of the DR-FTIR spectra in the ν(C–H) bands showed that the ratio of the aromatic ν(C–H) bands systematically increased relative to the aliphatic ν(C–H) bands with increasing mineralization of biochar C in the B550 amended soils, and this relationship was unique for each soil type. In contrast, this relationship was not observed for the B450 amended soils that contained a relatively smaller proportion of aromatic C. PMID:29657354

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

PubMed

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

2018-02-01

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

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

PubMed Central

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

2013-01-01

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

Synthesis and characterization of bis-thiourea having amino acid derivatives

NASA Astrophysics Data System (ADS)

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

2016-11-01

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

Synthesis of Novel Compounds as New Potent Tyrosinase Inhibitors

PubMed Central

Hamidian, Hooshang

2013-01-01

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

Utilization of struvite recovered from high-strength ammonium-containing simulated wastewater as slow-release fertilizer and fire-retardant barrier.

PubMed

Yetilmezsoy, Kaan; Kocak, Emel; Akbin, Havva Melda; Özçimen, Didem

2018-06-28

Sustainable uses of the struvite (magnesium ammonium phosphate hexahydrate, MgNH 4 PO 4 ·6H 2 O, MAP) recovered from the synthetic wastewater, as a high-quality slow-release fertilizer for the growth of nine medicinal plants and a fire-retardant barrier on the flammability of cotton fabric and wooden plate, were explored in this study. The previous experimental results demonstrated that under the optimal conditions, about 98.7% of [Formula: see text] (initial [Formula: see text] = 1000 mg/L) could be effectively and successfully recovered from simulated wastewater in the form of MAP precipitate. Rates of increase in total fresh weights, total dry weights, and fresh heights of plants grown in soil fertilized with the struvite were determined as 67%, 52%, and 12% for valerian; 121%, 75%, and 18% for cucumber; 421%, 260%, and 47% for dill; 314%, 318%, and 27% for coriander; 432%, 566%, and 30% for tomato; 285%, 683%, and 26% for parsley; 200%, 225%, and 9% for basil; 857%, 656%, and 92% for rocket; and 146%, 115%, and 28% for cress, respectively, compared to the control pots. The microstructure, elemental composition, surface area, thermal behaviour, and functional groups of the grown crystals were characterized using SEM, EDS, BET, TGA-DTG-DSC, and FTIR analyses, respectively. Flammability tests and thermal analyses concluded that the dried and crumbled/implanted form of struvite used as a fire-retardant barrier demonstrated a remarkable flame-resistant behaviour for both cotton fabric and wooden plate. Findings of this experimental study clearly corroborated the versatility of struvite as non-polluting and environmentally friendly clean product for the sustainable usage in different fields.

Spectroscopic study of the reaction mechanism of buspirone interaction with iodine and tetracyanoethylene reagents and its applications.

PubMed

Zayed, M A; El-Habeeb, Abeer A

2009-06-01

The reactions between the drug buspirone (busp) in its base form and iodine amphoteric reagent (n-donor and/or sigma-acceptor) and with tetracyanoethylene as a pi-acceptor reagent (TCNE) have been studied spectrophotometrically at different reactant concentrations, time intervals, temperatures, and with different solvents and wavelengths, with the aim of selecting the conditions that give the most suitable molar extinction coefficients. This study aims chiefly to throw light on the nature of these reactions and to select the most proper conditions for spectrophotometric application of these reagents to determine this biologically active drug used in treating different diseases. The reaction mechanism involves the formation of busp-I(2) outer and inner sphere complexes. The separated busp-I(2) solid product obtained was investigated using elemental analyses, FT-IR, thermal analyses (TA) and electron ionization mass spectrometry (EI-MS) and was found to be biologically active. The reaction mechanism of busp-TCNE involves the formation of a charge transfer (CT) complex. The analytical parameters of the proposed spectrophotometric procedures were calculated. These procedures were applied in the analysis of busp in its formulations as a drug used to treat psychiatric illnesses. The values of the Sandell sensitivity, standard deviation (SD), relative standard deviation (RSD) and recovery percentage show the high sensitivity of these procedures. This study also presents a promising new busp-I(2) drug derivative that can be used more efficiently for the same purposes as its parent. It gives a clear idea about the possible metabolites and metabolic pathways of busp and its derivative that may occur in vivo. Copyright 2009 John Wiley & Sons, Ltd.

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

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

Ran, Xing-Rui; Wang, Ning; Xie, Wei-Ping

2015-05-15

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, ([Ln{sup III}Ag{sup I}(na)(ina)(ox)]·2(H{sub 2}O)){sub 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. - Graphical abstract: Series of three-dimensional (3D)more » 4d–4f Ln(III)–Ag(I) porous coordination polymers (PCPs) with interesting chain-layer construction which are featured by tetranuclear Ln{sub 2}Ag{sub 2} and ‘non-linear’ N–Ag–N linkages. - Highlights: • Complexes 1–8 are first built by three kinds of organic ligands based on nicotinic acid and isonicotinic acid. • PCPs 1–8 are featured by tetranuclear Ln{sub 2}Ag{sub 2} and ‘non-linear’ N–Ag–N linkages. • The total solvent-accessible volume of PCP 2 comprises 11.6% of the crystal volume after dislodging the free water molecules. • Complexes 2 and 4 exhibit characteristic lanthanide-centered luminescence, while compounds 3 and 5 show antiferromagnetic behaviors.« less

Quantification of octacalcium phosphate, authigenic apatite and detrital apatite in coastal sediments using differential dissolution and standard addition

NASA Astrophysics Data System (ADS)

Oxmann, J. F.; Schwendenmann, L.

2014-06-01

Knowledge of calcium phosphate (Ca-P) solubility is crucial for understanding temporal and spatial variations of phosphorus (P) concentrations in water bodies and sedimentary reservoirs. In situ relationships between liquid- and solid-phase levels cannot be fully explained by dissolved analytes alone and need to be verified by determining particular sediment P species. Lack of quantification methods for these species limits the knowledge of the P cycle. To address this issue, we (i) optimized a specifically developed conversion-extraction (CONVEX) method for P species quantification using standard additions, and (ii) simultaneously determined solubilities of Ca-P standards by measuring their pH-dependent contents in the sediment matrix. Ca-P minerals including various carbonate fluorapatite (CFAP) specimens from different localities, fluorapatite (FAP), fish bone apatite, synthetic hydroxylapatite (HAP) and octacalcium phosphate (OCP) were characterized by XRD, Raman, FTIR and elemental analysis. Sediment samples were incubated with and without these reference minerals and then sequentially extracted to quantify Ca-P species by their differential dissolution at pH values between 3 and 8. The quantification of solid-phase phosphates at varying pH revealed solubilities in the following order: OCP > HAP > CFAP (4.5% CO3) > CFAP (3.4% CO3) > CFAP (2.2% CO3) > FAP. Thus, CFAP was less soluble in sediment than HAP, and CFAP solubility increased with carbonate content. Unspiked sediment analyses together with standard addition analyses indicated consistent differential dissolution of natural sediment species vs. added reference species and therefore verified the applicability of the CONVEX method in separately determining the most prevalent Ca-P minerals. We found surprisingly high OCP contents in the coastal sediments analyzed, which supports the hypothesis of apatite formation by an OCP precursor mechanism.

Quantification of octacalcium phosphate, authigenic apatite and detrital apatite in coastal sediments using differential dissolution and standard addition

NASA Astrophysics Data System (ADS)

Oxmann, J. F.; Schwendenmann, L.

2014-01-01

Knowledge of calcium phosphate (Ca-P) solubility is crucial for understanding temporal and spatial variations of phosphorus (P) concentrations in water bodies and sedimentary reservoirs. In-situ relationships between liquid and solid-phase levels cannot be fully explained by dissolved analytes alone and need to be verified by determination of particular sediment P species. Lack of quantification methods for these species limits the knowledge of the P cycle. To address this issue, we (i) optimized a specifically developed conversion-extraction (CONVEX) method for P species quantification using standard additions; and (ii) simultaneously determined solubilities of Ca-P standards by measuring their pH-dependent contents in the sediment matrix. Ca-P minerals including various carbonate fluorapatite (CFAP) specimens from different localities, fluorapatite (FAP), fish bone apatite, synthetic hydroxylapatite (HAP) and octacalcium phosphate (OCP) were characterized by XRD, Raman, FTIR and elemental analysis. Sediment samples were incubated with and without these reference minerals and then sequentially extracted to quantify Ca-P species by their differential dissolution at pH values between 3 and 8. The quantification of solid-phase phosphates at varying pH revealed solubilities in the following order: OCP > HAP > CFAP (4.5% CO3) > CFAP (3.4% CO3) > CFAP (2.2% CO3) > FAP. Thus, CFAP was less soluble in sediment than HAP, and CFAP solubility increased with carbonate content. Unspiked sediment analyses together with standard addition analyses indicated consistent differential dissolution of natural sediment species vs. added reference species and therefore verified the applicability of the CONVEX method in separately determining the most prevalent Ca-P minerals. We found surprisingly high OCP contents in the analyzed coastal sediments which supports the hypothesis of apatite formation by an OCP precursor.

Physicochemical properties and combustion behavior of duckweed during wet torrefaction.

PubMed

Zhang, Shuping; Chen, Tao; Li, Wan; Dong, Qing; Xiong, Yuanquan

2016-10-01

Wet torrefaction of duckweed was carried out in the temperature range of 130-250°C to evaluate the effects on physicochemical properties and combustion behavior. The physicochemical properties of duckweed samples were investigated by ultimate analysis, proximate analysis, FTIR, XRD and SEM techniques. It was found that wet torrefaction improved the fuel characteristics of duckweed samples resulting from the increase in fixed carbon content, HHVs and the decrease in nitrogen and sulfur content and atomic ratios of O/C and H/C. It can be seen from the results of FTIR, XRD and SEM analyses that the dehydration, decarboxylation, solid-solid conversion, and condensation polymerization reactions were underwent during wet torrefaction. In addition, the results of thermogravimetric analysis (TGA) in air indicated that wet torrefaction resulted in significant changes on combustion behavior and combustion kinetics parameters. Duckweed samples after wet torrefaction behaved more char-like and gave better combustion characteristics than raw sample. Copyright © 2016 Elsevier Ltd. All rights reserved.

Synthesis and Characterization of Chitosan-p-t-Butylcalix[4]arene acid

NASA Astrophysics Data System (ADS)

Handayani, D. S.; Frimadasi, W.; Kusumaningsih, T.; Pranoto

2018-03-01

The synthesis of chitosan-p-t-butylcalix[4]arene acid was done with DIC (N, N’-diisopropylcarbodiimide) as the coupling agent. The structural analysis of the chitosan-p-t-butylcalix[4]arene acid was conducted by spectrophotometer Fourier Transform Infra Red (FTIR) and X-Ray Diffraction (XRD). Meanwhile, the surface area was investigated by Surface Area Analysis, the Scanning Electrone Microscope (SEM) analysed the surface morphology, and also the melting point temperature was determined. FTIR analysis on Chitosan-p-t-butylcalix[4]arene provides an overlapped absorption of -OH and -NH groups at 3438.26 cm-1. Meanwhile, a C = C aromatic bond present at 1480.43 cm-1. XRD analysis shows some broaden peaks due to the amorphous phase of the prepared material. The prepared material is a brownish yellow solid, odorless and porous. The melting point, surface area, and the average pore radius are above 300 °C, 9.42 m2 / g, and 52.5938 Å, respectively.

Adsorption of Pb(II) ions onto biomass from Trifolium resupinatum: equilibrium and kinetic studies

NASA Astrophysics Data System (ADS)

Athar, Makshoof; Farooq, Umar; Aslam, Muhammad; Salman, M.

2013-09-01

The present study provides information about the binding of Pb(II) ions on an eco-friendly and easily available biodegradable biomass Trifolium resupinatum. The powdered biomass was characterized by FTIR, potentiometric titration and surface area analyses. The FTIR spectrum showed the presence of hydroxyl, carbonyl and amino functional groups and Pb(II) ions bound with the oxygen- and nitrogen-containing sites (hydroxyl and amino groups). The acidic groups were also confirmed by titrations. Effects of various environmental parameters (time, pH and concentration) have been studied. The biosorption process achieved equilibrium in a very short period of time (25 min). Non-linear approach for Langmuir and Freundlich models was used to study equilibrium process and root mean-square error was used as an indicator to decide the fitness of the mathematical model. The biosorption process was found to follow pseudo-second-order kinetics and was very fast. Thus, the biomass can be cost-effectively used for the binding of Pb(II) ions from aqueous solutions.

Preparation of graphene oxide as biomaterials for drug adsorption

NASA Astrophysics Data System (ADS)

Usca, G. Tubón; Gómez, C. Vacacela; Fiallos, D. Coello; Tavolaro, P.; Martino, G.; Caputi, L. S.; Tavolaro, A.

2015-02-01

Doxorubicin hydrochloride (DOX), is a class I anthracycline antibiotic (FDA approved in the 1970s) widely used as an effective chemotherapeutic drug for the treatment of many human neoplasms. Like most anticancer drugs, DOX can provoke severe toxicity to the body when it is administered at high doses systemically. Here we report the results of an investigation of drug adsorption on graphene oxide (GO) materials prepared by the Improved Hummer's method. High-purity GO has been prepared, characterized by XPS, UV-vis, FTIR-ATR, FESEM, UV- vis analyses, Zero Point Charge determinations and applied in the immobilization of doxorubicin, via simple noncovalent method. The adsorption percentage of the drug at pH 7 on GO was observed to be higher (equal to 90 %) than that obtained at acidic pH 3 (equal to 85%). Experimental result of adsorption of DOX on GO, obtained by FTIR-ATR spectroscopy analysis indicate that the inorganic material and the drug form and adduct by π-π stacking interactions.

Catalase-like activity studies of the manganese(II) adsorbed zeolites

NASA Astrophysics Data System (ADS)

ćiçek, Ekrem; Dede, Bülent

2013-12-01

Preparation of manganese(II) adsorbed on zeolite 3A, 4A, 5A. AW-300, ammonium Y zeolite, organophilic, molecular sieve and catalase-like enzyme activity of manganese(II) adsorbed zeolites are reported herein. Firstly zeolites are activated at 873 K for two hours before contact manganese(II) ions. In order to observe amount of adsorption, filtration process applied for the solution. The pure zeolites and manganese(II) adsorbed zeolites were analysed by FT-IR. As a result according to the FT-IR spectra, the incorporation of manganese(II) cation into the zeolite structure causes changes in the spectra. These changes are expected particularly in the pseudolattice bands connected with the presence of alumino and silicooxygen tetrahedral rings in the zeolite structure. Furthermore, the catalytic activities of the Mn(II) adsorbed zeolites for the disproportionation of hydrogen peroxide were investigated in the presence of imidazole. The Mn(II) adsorbed zeolites display efficiency in the disproportion reactions of hydrogen peroxide, producing water and dioxygen in catalase-like activity.

Analysis of 19th century ceramic fragments excavated from Pirenópolis (Goiás, Brazil) using FT-IR, Raman, XRF and SEM

NASA Astrophysics Data System (ADS)

Freitas, Renato P.; Coelho, Filipe A.; Felix, Valter S.; Pereira, Marcelo O.; de Souza, Marcos André Torres; Anjos, Marcelino J.

2018-03-01

This study used Raman, FT-IR and XRF spectroscopy and SEM to analyze ceramic fragments dating from the 19th century, excavated from an old farm in the municipality of Pirenópolis, Goiás, Brazil. The results show that the samples were produced in an open oven at a firing temperature below 500 °C, using raw materials including kaolinite, hematite, magnetite, quartz, microcline, albite, anhydrite, calcite, illite, orthoclase and MnO2. Although the analyses showed similarities in the manufacturing process and the presence of many minerals was common in all samples, multivariate statistical methods (PCA) allowed a more detailed assessment of similarities and differences in the mineral composition of the samples. The results of the PCA showed that the samples excavated in one of the slave quarters (senzalas) group with those excavated at the farmhouse, where the landowner lived, which indicates a paternalistic attitude towards captives, including the sharing of ceramic materials of everyday use.

Poly(allyl methacrylate) functionalized hydroxyapatite nanocrystals via the combination of surface-initiated RAFT polymerization and thiol-ene protocol: a potential anticancer drug nanocarrier.

PubMed

Bach, Long Giang; Islam, Md Rafiqul; Vo, Thanh-Sang; Kim, Se-Kwon; Lim, Kwon Taek

2013-03-15

Hydroxyapatite nanocrystals (HAP NCs) were encapsulated by poly(allyl methacrylate) (PolyAMA) employing controlled surface-initiated reversible addition-fragmentation chain transfer (SI-RAFT) polymerization of allyl methacrylate to afford HAP-PolyAMA nanohybrids. The subsequent thiol-ene coupling of nanohybrids with 2-mercaptosuccinic acid resulted HAP-Poly(AMA-COOH) possessing multicarboxyl group. The formation of the nanohybrids was confirmed by FT-IR and EDS analyses. The TGA and FE-SEM investigation were further suggested the grafting of PolyAMA onto HAP NCs. The utility of the HAP-PolyAMA nanohybrid as drug carrier was also explored. The pendant carboxyl groups on the external layers of nanohybrids were conjugated with anticancer drug cisplatin to afford HAP-Poly(AMA-COOH)/Pt complex. The formation of the complex was confirmed by FT-IR, XPS, and FE-SEM. In vitro evaluation of the synthesized complex as nanomedicine revealed its potential chemotherapeutic efficacy against cancer cell lines. Copyright © 2012 Elsevier Inc. All rights reserved.

Quantitative assessment of specific defects in roasted ground coffee via infrared-photoacoustic spectroscopy.

PubMed

Dias, Rafael Carlos Eloy; Valderrama, Patrícia; Março, Paulo Henrique; Dos Santos Scholz, Maria Brigida; Edelmann, Michael; Yeretzian, Chahan

2018-07-30

Chemical analyses and sensory evaluation are the most applied methods for quality control of roasted and ground coffee (RG). However, faster alternatives would be highly valuable. Here, we applied infrared-photoacoustic spectroscopy (FTIR-PAS) on RG powder. Mixtures of specific defective beans were blended with healthy (defect-free) Coffea arabica and Coffea canephora bases in specific ratios, forming different classes of blends. Principal Component Analysis allowed predicting the amount/fraction and nature of the defects in blends while partial Least Squares Discriminant Analysis revealed similarities between blends (=samples). A successful predictive model was obtained using six classes of blends. The model could classify 100% of the samples into four classes. The specificities were higher than 0.9. Application of FTIR-PAS on RG coffee to characterize and classify blends has shown to be an accurate, easy, quick and "green" alternative to current methods. Copyright © 2018 The Author(s). Published by Elsevier Ltd.. All rights reserved.

Synthesis, surface chemistry and pseudocapacitance mechanisms of VN nanocrystals derived by a simple two-step halide approach

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

Choi, Daiwon; Jampani, Prashanth H.; Jayakody, J. R. P.

Chloroamide precursors generated via a simple two-step ammonolysis reaction of transition metal chloride in the liquid phase at room temperature were heat treated in ammonia at moderate temperature to yield nano-sized VN crystallites. Grain growth inhibited by lowering the synthesis temperature (≈400°C) yielded agglomerated powders of spherical crystallites of cubic phase of VN with particle sizes as small as 6nm in diameter. X-ray diffraction, FTIR, mass spectroscopy (MS), and nuclear magnetic resonance (NMR) spectroscopy assessed the ammonolysis and nitridation reaction of the VCl 4-NH 3 system. X-ray Rietveld refinement, the BET technique and high-resolution transmission microscopy (HRTEM), energy dispersive x-raymore » (EDX) and thermogravimetric analysis (TGA) helped assess the crystallographic and microstructural nature of the VN nanocrystals. The surface chemistry and redox reaction leading to the gravimetric pseudo-capacitance value of (≈855 F/g) measured for the VN nanocrystals was determined and validated using FTIR, XPS and cyclic voltammetry analyses.« less

A green chemistry approach for the synthesis and characterization of bioactive gold nanoparticles using Azolla microphylla methanol extract

NASA Astrophysics Data System (ADS)

Kunjiappan, Selvaraj; Chowdhury, Ranjana; Bhattacharjee, Chiranjib

2014-06-01

This article reports the environmentally benign synthesis of gold nanoparticles (GNPs) using methanol extract of Azolla microphylla as the stabilizing and reducing agent. The GNPs were characterized by UV-vis spectrophotometry and FTIR, and the morphological characteristics were analyzed by XRD, FESEM-EDX and HRTEM. The GNPs could be formed in very short time, even in less than 30 min. The nanoparticles measured by UV-spectrophotometer demonstrated a peak at 540 nm corresponding to surface plasmon resonance spectra, and the peaks showed by FTIR suggested the presence of organic biomolecules on the surface of the GNPs. XRD results confirmed the crystalline nature of the GNPs, and FESEM-EDX and HRTEM analyses had been performed in the size ranges of 17-40 nm and 1.25-17.5 nm respectively. The synthesized GNPs showed excellent antioxidant activity. This study shows the feasibility of using plant sources for the biosynthesis of GNPs.

Eruption Depths, Magma Storage and Magma Degassing at Sumisu Caldera, Izu-Bonin Arc: Evidence from Glasses and Melt Inclusions

NASA Astrophysics Data System (ADS)

Johnson, E. R.

2015-12-01

Island arc volcanoes can become submarine during cataclysmal caldera collapse. The passage of a volcanic vent from atmospheric to under water environment involves complex modifications of the eruption style and subsequent transport of the pyroclasts. Here, we use FTIR measurements of the volatile contents of glass and melt inclusions in the juvenile pumice clasts in the Sumisu basin and its surroundings (Izu-Bonin arc) to investigate changes in eruption depths, magma storage and degassing over time. This study is based on legacy cores from ODP 126, where numerous unconsolidated (<65 ka), extremely thick (few m to >250 m), massive to normally graded pumice lapilli-tuffs were recovered over four cores (788C, 790A, 790B and 791A). Glass and clast geochemistry indicate the submarine Sumisu caldera as the source of several of these pumice lapilli-tuffs. Glass chips and melt inclusions from these samples were analyzed using FTIR for H2O and CO2 contents. Glass chips record variable H2O contents; most chips contain 0.6-1.6 wt% H2O, corresponding to eruption depths of 320-2100 mbsl. Variations in glass H2O and pressure estimates suggest that edifice collapse occurred prior-to or during eruption of the oldest of these samples, and that the edifice may have subsequently grown over time. Sanidine-hosted melt inclusions from two units record variably degassed but H2O-rich melts (1.1-5.6 wt% H2O). The lowest H2O contents overlap with glass chips, consistent with degassing and crystallization of melts until eruption, and the highest H2O contents suggest that large amounts of degassing accompanied likely explosive eruptions. Most inclusions, from both units, contain 2-4 wt% H2O, which further indicates that the magmas crystallized at pressures of ~50-100 MPa, or depths ~400-2800 m below the seafloor. Further glass and melt inclusion analyses, including major element compositions, will elucidate changes in magma storage, degassing and evolution over time.

Constitutive Analyses of Nontraditional Stabilization Additives

DTIC Science & Technology

2004-11-01

cm-I Figure 29. FTIRIATR spectrum of Ven-Set 950 soil stabilization agent Based on the information provided in the MSDS and the FTIR analysis above...emulsion. The MSDS states that it is composed of an acrylic polymer (52 percent) with zinc oxide (2 percent), activated carbon (8 to 9 percent), and...water. The polymer as yet is unidentified. However, it appears to be an acrylate/ methacrylate with some aromaticity (peak about 1,635 c-f’). The

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.

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.

STRUCTURAL ANALYSIS OF THE COMBUSTION SYNTHESIZED Y3+ DOPED CERIA (Ce0.9Y0.1O1.95)

NASA Astrophysics Data System (ADS)

Jeyanthi, C. Esther; Siddheswaran, R.; Kumar, Pushpendra; Mangalaraja, R. V.; Siva Shankar, V.; Rajarajan, K.

2013-07-01

Y3+ doped CeO2 nanopowders (Ce0.9Y0.1O1.95, abbreviated as YDC) were synthesized by citrate-nitrate-auto combustion process using cerium nitrate hexahydrate, yttrium nitrate hexahydrate and citric acid. The as-synthesized powders were calcined at 700°C and converted into dense bodies followed by sintering at 1200°C. The microstructure of the synthesized powders and sintered bodies were examined by scanning electron microscopy (SEM). The surface morphology of the nanoparticles and clusters were also analysed by transmission electron microscopy (TEM). The particles size of the YDC was found to be in the range from 10 to 30 nm, which is in good agreement with the crystallite size calculated from X-ray peak broadening method. Also, the X-ray diffraction confirmed that the Ce0.9Y0.1O1.95 crystallizes as the cubic fluorite structure of pure ceria. The optical absorption by functional molecules, impurities and oxygen vacancies were analysed by FTIR and Raman spectroscopic studies. From the FTIR spectrum, the absorption peak found at 530 cm-1 is attributed to the vibrations of metal-oxygen bonds. The characteristic Raman peak was found to be 468 cm-1, and the minute absorption of oxygen vacancies were observed in the region 500-640 cm-1.

Innovative non-thermal plasma disinfection process inside sealed bags: Assessment of bactericidal and sporicidal effectiveness in regard to current sterilization norms

PubMed Central

Charpentier, Emilie; Le-Bras, Florian; Maho, Thomas; Robert, Eric; Pouvesle, Jean-Michel; Polidor, Franck; Gangloff, Sophie C.; Boudifa, Mohamed

2017-01-01

In this work, we developed a device capable to generate a non-thermal plasma discharge inside a sealed bag. The aim of this study was to assess the effectiveness of the oxygen, nitrogen and argon plasma sterilization on Pseudomonas aeruginosa, Staphylococcus aureus and Bacillus subtilis spores according to the NF EN 556 Norm. Moreover the bag integrity which is a critical key to maintain the sterile state of items after the end of the process was verified by Fourier Transform Infrared (FTIR) and X-ray Photoelectron Spectrometry (XPS) analyses. After plasma treatments, the bacterial counting showed a 6 log reduction of P. aeruginosa and S. aureus in 45 min and 120 min respectively whatever the gas used and a 4 log reduction of B. subtilis spores in 120 min with only oxygen plasma. These results were confirmed by Scanning Electron Microscopy (SEM) observations showing altered bacteria or spores and numerous debris. Taking into account the studied microorganisms, the oxygen plasma treatment showed the highest efficiency. FTIR and XPS analyses showed that this treatment induced no significant modification of the bags. To conclude this non-thermal plasma sterilization technique could be an opportunity to sterilize heat and chemical-sensitive medical devices and to preserve their sterile state after the end of the process. PMID:28662202

Superelement Analysis of Tile-Reinforced Composite Armor

NASA Technical Reports Server (NTRS)

Davila, Carlos G.

1998-01-01

Super-elements can greatly improve the computational efficiency of analyses of tile-reinforced structures such as the hull of the Composite Armored Vehicle. By taking advantage of the periodicity in this type of construction, super-elements can be used to simplify the task of modeling, to virtually eliminate the time required to assemble the stiffness matrices, and to reduce significantly the analysis solution time. Furthermore, super-elements are fully transferable between analyses and analysts, so that they provide a consistent method to share information and reduce duplication. This paper describes a methodology that was developed to model and analyze large upper hull components of the Composite Armored Vehicle. The analyses are based on two types of superelement models. The first type is based on element-layering, which consists of modeling a laminate by using several layers of shell elements constrained together with compatibility equations. Element layering is used to ensure the proper transverse shear deformation in the laminate rubber layer. The second type of model uses three-dimensional elements. Since no graphical pre-processor currently supports super-elements, a special technique based on master-elements was developed. Master-elements are representations of super-elements that are used in conjunction with a custom translator to write the superelement connectivities as input decks for ABAQUS.

Extraction of information from major element chemical analyses of lunar basalts

NASA Technical Reports Server (NTRS)

Butler, J. C.

1985-01-01

Major element chemical analyses often form the framework within which similarities and differences of analyzed specimens are noted and used to propose or devise models. When percentages are formed the ratios of pairs of components are preserved whereas many familiar statistical and geometrical descriptors are likely to exhibit major changes. This ratio preserving aspect forms the basis for a proposed framework. An analysis of compositional variability within the data set of 42 major element analyses of lunar reference samples was selected to investigate this proposal.

Comparisons of Elemental Profiles of the Western Spruce Budworm Reared on Three host Foilages and Artificial Medium

Treesearch

John A. McLean; P. Laks; T.L. Shore

1983-01-01

Western spruce budworm were reared on three host foliages and artificial medium. Trace element analyses showed large differences in elemental concentrations between food sources and only minor differences between insect life stages. Discriminant analyses were carried out to test the distinctiveness of adult chemoprints from each rearing regime. Fe, Cu, and Zn were...

FTIR-ATR-based prediction and modelling of lignin and energy contents reveals independent intra-specific variation of these traits in bioenergy poplars

PubMed Central

2011-01-01

Background There is an increasing demand for renewable resources to replace fossil fuels. However, different applications such as the production of secondary biofuels or combustion for energy production require different wood properties. Therefore, high-throughput methods are needed for rapid screening of wood in large scale samples, e.g., to evaluate the outcome of tree breeding or genetic engineering. In this study, we investigated the intra-specific variability of lignin and energy contents in extractive-free wood of hybrid poplar progenies (Populus trichocarpa × deltoides) and tested if the range was sufficient for the development of quantitative prediction models based on Fourier transform infrared spectroscopy (FTIR). Since lignin is a major energy-bearing compound, we expected that the energy content of wood would be positively correlated with the lignin content. Results Lignin contents of extractive-free poplar wood samples determined by the acetyl bromide method ranged from 23.4% to 32.1%, and the calorific values measured with a combustion calorimeter varied from 17260 to 19767 J g-1. For the development of calibration models partial least square regression and cross validation was applied to correlate FTIR spectra determined with an attenuated total reflectance (ATR) unit to measured values of lignin or energy contents. The best models with high coefficients of determination (R2 (calibration) = 0.91 and 0.90; R2 (cross-validation) = 0.81 and 0.79) and low root mean square errors of cross validation (RMSECV = 0.77% and 62 J g-1) for lignin and energy determination, respectively, were obtained after data pre-processing and automatic wavenumber restriction. The calibration models were validated by analyses of independent sets of wood samples yielding R2 = 0.88 and 0.86 for lignin and energy contents, respectively. Conclusions These results show that FTIR-ATR spectroscopy is suitable as a high-throughput method for lignin and energy estimations in large data sets. Our study revealed that the intra-specific variations in lignin and energy contents were unrelated to each other and that the lignin content, therefore, was no predictor of the energy content. Employing principle component analyses we showed that factor loadings for the energy content were mainly associated with carbohydrate ring vibrations, whereas those for lignin were mainly related to aromatic compounds. Therefore, our analysis suggests that it may be possible to optimize the energy content of trees without concomitant increase in lignin. PMID:21477346

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

PubMed

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

2014-07-15

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

Characterization of Limestone as Raw Material to Hydrated Lime

NASA Astrophysics Data System (ADS)

Salem Hwidi, Rajeb; Nuraiti Tengku Izhar, Tengku; Saad, Farah Naemah Mohd

2018-03-01

In Malaysia, limestone is essentially important for the economic growth as raw materials in the industry sector. Nevertheless, a little attention was paid to the physical, chemical, mineralogical, and morphological properties of the limestone using X-ray fluorescence (X-RF), X-ray diffraction (X-RD), Fourier transform infrared spectroscopy (FTIR), and Scanning electron microscopy / energy dispersive x-ray spectroscopy (SEM-EDS) respectively. Raw materials (limestone rocks) were collected from Bukit Keteri area, Chuping, Kangar, Perlis, Malaysia. Lab crusher and lab sieved were utilized to prepare five different size of ground limestone at (75 µm, 150 µm, 225 µm, 300, and 425 µm) respectively. It is found that the main chemical composition of bulk limestone was Calcium oxide (CaO) at 97.58 wt.% and trace amount of MnO, Al2O3, and Fe2O3 at 0.02%, 0.35%, and 0.396% respectively. XRD diffractograms showed characteristic peaks of calcite and quartz. Furthermore, main FTIR absorption bands at 1,419, 874.08 and 712.20 cm-1 indicated the presence of calcite. The micrographs showed clearly the difference of samples particle size. Furthermore, EDS peaks of Ca, O, and C elements confirmed the presence of CaCO3 in the samples.

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

NASA Astrophysics Data System (ADS)

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

2018-01-01

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

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

NASA Astrophysics Data System (ADS)

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

2018-07-01

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

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

PubMed

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

2010-02-01

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

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

PubMed Central

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

2016-01-01

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

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.

Structural and electrical properties of CZTS thin films by electrodeposition

NASA Astrophysics Data System (ADS)

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

2018-06-01

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

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

NASA Astrophysics Data System (ADS)

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

2015-11-01

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

Thermal, dielectric studies on pure and amino acid ( L-glutamic acid, L-histidine, L-valine) doped KDP single crystals

NASA Astrophysics Data System (ADS)

Kumaresan, P.; Moorthy Babu, S.; Anbarasan, P. M.

2008-05-01

Amino acids ( L-glutamic acid, L-histidine, L-valine) doped potassium dihydrogen phospate crystals are grown by solution growth technique. Slow cooling as well as slow evaporation methods were employed to grow these crystals. The concentration of dopants in the mother solution was varied from 0.1 mol% to 10 mol%. The solubility data for all dopants concentration were determined. There is variation in pH value and hence, there is habit modification of the grown crystals were characterized with UV-VIS, FT-IR studies, SHG trace elements and dielectric studies reveal slight distortion of lattice parameter for the heavily doped KDP crystals. UV-Visible spectra confirm the improvement in the transparency of these crystals on doping metal ions. FT-IR spectra reveal strong absorption band between 1400 and 1600 cm -1 for metal ion doped crystals. TGA-DTA studies reveal good thermal stability. The dopants increase the hardness value of the material and it also depends on the concentration of the dopants. Amino acids doping improved the NLO properties. The detailed results on the spectral parameters, habit modifications and constant values will be presented.

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

DOE PAGES

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

2014-11-04

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

Assessment of the effects of air pollution on european monuments through a geochemical characterization of black crusts

NASA Astrophysics Data System (ADS)

Comite, Valeria; Barca, Donatella; Belfiore, Cristina Maria; Bonazza, Alessandra; La Russa, Mauro Francesco; Ruffolo, SIlvestro Antonio; Pezzino, Antonino; Sabbioni, Cristina

2014-05-01

This contribution focuses on spectrometric analyses carried out on black crust samples, collected from buildings and churches belonging to the European built Heritage, i.e., the Corner Palace in Venice (Italy), the Cathedral of St. Rombouts in Mechelen (Belgium), the Church of St. Eustache in Paris (France) and the Tower of London (United Kingdom). Such monuments, all built in carbonate stones, were selected for their historic and artistic relevance, as well as for their location in different urban environments. For an exhaustive account of the sampled black crusts, an approach integrating complementary techniques was used, including OM, SEM-EDS, FT-IR and LA-ICP-MS. The complete characterization of the damage layers provided information on their chemical composition, the state of conservation of the underlying substrates and the interactions between crusts and stones. In particular, the geochemical study in terms of trace elements revealed that all crusts are enriched in heavy metals (As, Cd, Co, Cr, Cu, Fe, Mn, Mo, Ni, Pb, Sb, Sn, Ti, V, and Zn) compared to substrates. The different concentrations of such elements in all analyzed crust samples can be ascribed to several factors, such as: height of sampling, morphology of the sampled surfaces (vertical or horizontal), exposure to atmospheric agents as well as to direct (road or boat traffic) or indirect (industries) sources of pollution, accumulation time of pollutants on the surface, wash out and particulate air pollution. Specifically, the crusts collected at lower heights (Corner Palace, Cathedral of St. Rombouts, Tower of London) resulted to be mainly influenced by mobile sources of pollution (vehicular or boat traffic), while samples taken at higher heights (Church of St. Eustache and Corner Palace) are generally mostly affected by stationary combustion sources. In some cases, the detailed analysis of multilayered crusts (Palazzo Corner) contributed to recognize the variation of combustion sources responsible for the deterioration of surfaces over time. In addition, the possibility of analyzing altered portions of the substrate (Tower of London) permitted to observe that some elements (Zn, Cu and Ni) show concentrations similar and, sometimes, higher than the overlying crusts. This result can be explained by the geochemical mobility of such elements (at specific environmental conditions), which accelerate the process of sulfating, rapidly promoting the formation of new layers of crust. In conclusion, the study of black crusts and altered substrates in terms of trace elements may provide information useful to understand the influence of the pollutants in the genesis of such degradation forms.

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

PubMed

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

2016-07-01

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

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

PubMed

Surati, Kiran R; Thaker, B T

2010-01-01

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

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

NASA Astrophysics Data System (ADS)

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

2018-05-01

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

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

PubMed Central

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

2016-01-01

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

Functional group and individual maceral chemistry of high volatile bituminous coals from southern Indiana: Controls on coking

USGS Publications Warehouse

Walker, R.; Mastalerz, Maria

2004-01-01

The individual maceral chemistries of two Pennsylvanian, high volatile bituminous coals, the Danville Coal Member (Dugger Formation, R o=0.55%) and the Lower Block Coal Member (Brazil Formation, R o=0.56%) of Indiana, were investigated using electron microprobe and Fourier Transform Infrared Spectrometry (FTIR) techniques, with the purpose of understanding differences in their coking behavior. Microprobe results reveal that carbon contents are highest in inertinite and sporinite, followed by desmocollinite and telocollinite. Oxygen and organic nitrogen are most abundant in telocollinite and desmocollinite; sporinite and inertinite contain lesser amounts of these two elements. Organic sulfur contents are highest in sporinite, lowest in inertinite, and intermediate in desmocollinite and telocollinite. Vitrinites within the Danville and Lower Block coals are very similar in elemental composition, while Lower Block inertinites and sporinites have higher carbon, lower oxygen, and sulfur contents which, when combined with the inertinite-and sporinite-rich composition of the Lower Block seam, strongly influences its whole coal chemistry. Fourier transform infrared spectrometry revealed greater aromatic hydrogen in the Lower Block coal, along with higher CH2/CH3 ratios, which suggest that liptinites contribute considerable amounts of long-chain, unbranched aliphatics to the overall kerogen composition of the Lower Block coal. Long-chain, unbranched aliphatics crack at higher temperatures, producing tar and oily byproducts during coking; these may help increase Lower Block plasticity. Electron microprobe and FTIR results indicate that individual maceral chemistries, combined with the maceral composition of the seam, are the primary control of better coking properties of the Lower Block coal. ?? 2003 Elsevier B.V. All rights reserved.

The Effect of Pressure and Temperature on Mid-Infrared Sensing of Dissolved Hydrocarbons in Water.

PubMed

Heath, Charles; Myers, Matthew; Pejcic, Bobby

2017-12-19

Attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectroscopy using a polymer coated internal reflection element/waveguide is an established sensor platform for the detection of a range of organic and hydrocarbon molecules dissolved in water. The polymer coating serves two purposes: to concentrate hydrocarbons from the aqueous phase and to exclude water along with other interfering molecules from the surface of the internal reflection element. Crucial to reliable quantification and analytical performance is the calibration of the ATR-FTIR sensor which is commonly performed in water under mild ambient conditions (i.e., 25 °C and 1 atm). However, there is a pressing need to monitor environmental and industrial processes/events that may occur at high pressures and temperatures where this calibration approach is unsuitable. Using a ruggedized optical fiber probe with a diamond-based ATR, we have conducted mid-infrared sensor experiments to understand the influence of high pressure (up to 207 bar) and temperature (up to 80 °C) on the detection of toluene and naphthalene dissolved in water. Using a poly(isobutylene) film, we have shown that the IR spectroscopic response is relatively unaffected by changes in pressure; however, a diminished response was observed with increasing temperature. We reveal that changes in the refractive index of the polymer film with temperature have only a minor effect on sensitivity. A more plausible explanation for the observed significant change in sensor response with temperature is that the partitioning process is exothermic and becomes less favorable with increasing temperature. This Article shows that the sensitivity is relatively invariant to pressure; however, the thermal variations are significant and need to be considered when quantifying the concentration of hydrocarbons in water.

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

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

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

2010-01-12

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

Field evaluation of Fourier transform infrared continuous emissions monitoring (FTIR CEM) systems

NASA Astrophysics Data System (ADS)

Dunder, Thomas A.; Geyer, Thomas J.; Kinner, Laura L.; Plummer, Grant M.

1995-02-01

Recent environmental regulations, including the Clean Air Act and the Enhanced Monitoring Regulations, may require continuous emissions monitoring (CEM) of hazardous air pollutants (HAPs). A promising technique for this application is Fourier transform infrared spectroscopy (FTIR). FTIR spectroscopy can, in principle, be used to monitor virtually any gas phase species. Two evaluations of FTIR CEM systems are discussed. The first study, performed in 1993 - 94, compared two FTIR CEM systems on a side-by-side basis in an extended field test at two coal-fired electric power plants. The FTIR CEM systems monitored the legally mandated criteria pollutants and diluents (CO, CO2, NO, NO2, and SO2) as well as H2O. In addition, one system monitored two HAPs (HCl and HF) and NH3. The FTIR CEM measurements were compared with those from the compliance CEM systems at the facilities. Several relative accuracy test audits were also performed to verify the FTIR CEM accuracy. The second evaluation was recently commenced on behalf of the Environmental Protection Agency. In this study, FTIR CEM systems are evaluated specifically for the monitoring of HAP species by conducting laboratory and field tests. The evaluation culminates in the development of proposed performance specifications and protocols for FTIR CEM systems.

Effect of catalyst calcination temperature in the visible light photocatalytic oxidation of gaseous formaldehyde by multi-element doped titanium dioxide.

PubMed

de Luna, Mark Daniel G; Laciste, Maricris T; Tolosa, Nolan C; Lu, Ming-Chun

2018-03-20

The present study investigates the influence of calcination temperature on the properties and photoactivity of multi-element doped TiO 2 . The photocatalysts were prepared by incorporating silver (Ag), fluorine (F), nitrogen (N), and tungsten (W) into the TiO 2 structure via the sol-gel method. Spectroscopic techniques were used to elucidate the correlation between the structural and optical properties of the doped photocatalyst and its photoactivity. XRD results showed that the mean crystallite size increased for undoped photocatalysts and decreased for the doped photocatalysts when calcination was done at higher temperatures. UV-Vis spectra showed that the absorption cut-off wavelength shifted towards the visible light region for the as-synthesized photocatalysts and band gap narrowing was attributed to multi-element doping and calcination. FTIR spectra results showed the shifting of OH-bending absorption bands towards increasing wave numbers. The activity of the photocatalysts was evaluated in terms of gaseous formaldehyde removal under visible light irradiation. The highest photocatalytic removal of gaseous formaldehyde was found at 88%. The study confirms the effectiveness of multi-element doped TiO 2 to remove gaseous formaldehyde in air by visible light photocatalysis and the results have a lot of potential to extend the application to other organic air contaminants.

Comparison of properties of new sources of partially purified inulin to those of commercially pure chicory inulin.

PubMed

Mudannayake, Deshani C; Wimalasiri, Kuruppu M S; Silva, Kahandage F S T; Ajlouni, Said

2015-05-01

Newly developed inulin powders were prepared from roots of Asparagus falcatus (AF) and Taraxacum javanicum (TJ) plants grown in Sri Lanka. Inulin content, analyzed by enzymatic spectrophotometric as well as high-performance liquid chromatographic methods, showed that AF and TJ inulin powders contain 65.5% and 45.4% (dry wt) inulin, respectively, compared with 72% dry wt in the commercially available chicory inulin. Treating the AF and TJ inulin powders using ion exchange techniques significantly (P < 0.05) reduced their contents of micro (Zn, Cu, Mn, Fe) and macro (Na, K, Ca, Mg) elements. Enzymatic hydrolysis of inulin into fructose and glucose by fructanase, and FT-IR analyses proved that the developed AF and TJ inulins have characteristic molecular composition similar to commercial inulin. TJ inulin contained significantly (P < 0.05) greater amounts of total phenolics (4.37 mg GAE/g), total flavonoids (2.79 mg QE/g), and antioxidant capacity (833.11 mM TE/g) than AF inulin, which contained 1.33 mg GAE/g of total phenolics, 0.43 mg QE/g of total flavonoids, and 406.26 mM TE/g antioxidant capacity. The current study suggests that the newly developed inulin from AF and TJ roots could be used as an alternative commercial source of inulin for the food industry. © 2015 Institute of Food Technologists®

Analysis of atmospheric paniculate matter; application of optical and selected geochemical techniques

USGS Publications Warehouse

Mastalerz, Maria; Glikson, M.; Simpson, R.W.

1999-01-01

An increase in participate matter in the atmosphere has been shown to be linked to increased mortality but this relationship is poorly understood. Light microscopy, electron microscopy, electron microprobe, and micro-FTIR techniques have been applied to study atmospheric particulates in Brisbane, Australia as a part of a study on asthma. The particulate matter samples were collected daily from April to August 1992, and the sampling covered the autumn period which is typically a time of high asthma incidence in Brisbane. Volumetrically, most atmospheric particulate matter is less than 2 ??m in size. The microscopic analysis reveals that this material is composed mainly of combusted and incompletely burned hydrocarbons from motor vehicle exhaust emissions, quiescent spores of Mucorales, soil bacteria, and inorganic matter in the form of quartz and other silicates. Elemental and functional group analyses confirm microscope identification, documenting carbon-rich, aromatic exhaust material, more aliphatic pollen and spore material and inorganic matter. Fungal spores dominate bioaerosol and are very abundant from the end of April through May to mid-June. The cytoplasmic content of pollens or fungal spores is commonly regarded as allergenic. Particulates from the exhaust emissions and crustal material in a sub-micrometer size range may act as carriers or dispersive mechanisms for cytoplasmic material from fungal spores and pollens, perhaps causing periods of the highest exhaust emission to be the most allergenic. ?? 1998 Elsevier Science B.V. All rights reserved.

Structural, photophysical, and theoretical studies of imidazole-based excited-state intramolecular proton transfer molecules

NASA Astrophysics Data System (ADS)

Somasundaram, Sivaraman; Kamaraj, Eswaran; Hwang, Su Jin; Park, Sanghyuk

2018-02-01

Imidazole-based excited state intramolecular proton transfer (ESIPT) blue fluorescent molecules, 2-(1-(4-chlorophenyl)-4,5-diphenyl-1H-imidazol-2-yl)phenol (BHPI-Cl) and 2-(1-(4-bromophenyl)-4,5-diphenyl-1H-imidazol-2-yl)phenol (BHPI-Br) were designed and synthesized by Debus-Radziszewski method through a one-pot multicomponent reaction in high yield. The synthesized compounds were fully characterized by 1H NMR, 13C NMR, FT-IR, FT-Raman, GC-Mass, and elemental analysis. The molecular structures in single crystal lattice were studied by X-ray crystallographic analysis. Because of the intramolecular hydrogen bonding, hydroxyphenyl group is planar to the central imidazole ring, while the other phenyl rings gave distorted conformations to the central heterocyclic ring. BHPI-Cl and BHPI-Br molecules showed intense ESIPT fluorescence at 480 nm, because the two twisted phenyl rings on 4- and 5-positions have reduced intermolecular interaction between adjacent molecules in each crystal through a head-to-tail packing manner. Quantum chemical calculations of energies were carried out by (TD-)DFT using B3LYP/6-31G(d, p) basis set to predict the electronic absorption spectra of the compounds, and they showed good agreement between the computational and the experimental values. The thermal analyses of the synthesized molecules were also carried out by TGA/DSC method.

Molecular-Level Processing of Si-(B)-C Materials with Tailored Nano/Microstructures.

PubMed

Schmidt, Marion; Durif, Charlotte; Acosta, Emanoelle Diz; Salameh, Chrystelle; Plaisantin, Hervé; Miele, Philippe; Backov, Rénal; Machado, Ricardo; Gervais, Christel; Alauzun, Johan G; Chollon, Georges; Bernard, Samuel

2017-12-01

The design of Si-(B)-C materials is investigated, with detailed insight into the precursor chemistry and processing, the precursor-to-ceramic transformation, and the ceramic microstructural evolution at high temperatures. In the early stage of the process, the reaction between allylhydridopolycarbosilane (AHPCS) and borane dimethyl sulfide is achieved. This is investigated in detail through solid-state NMR and FTIR spectroscopy and elemental analyses for Si/B ratios ranging from 200 to 30. Boron-based bridges linking AHPCS monomeric fragments act as crosslinking units, extending the processability range of AHPCS and suppressing the distillation of oligomeric fragments during the low-temperature pyrolysis regime. Polymers with low boron contents display appropriate requirements for facile processing in solution, leading to the design of monoliths with hierarchical porosity, significant pore volume, and high specific surface area after pyrolysis. Polymers with high boron contents are more appropriate for the preparation of dense ceramics through direct solid shaping and pyrolysis. We provide a comprehensive study of the thermal decomposition mechanisms, and a subsequent detailed study of the high-temperature behavior of the ceramics produced at 1000 °C. The nanostructure and microstructure of the final SiC-based ceramics are intimately linked to the boron content of the polymers. B 4 C/C/SiC nanocomposites can be obtained from the polymer with the highest boron content. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Amphiphilic chitosan derivatives as carrier agents for rotenone

NASA Astrophysics Data System (ADS)

Kamari, Azlan; Aljafree, Nurul Farhana Ahmad

2017-08-01

In the present study, the feasibility of amphiphilic chitosan derivatives, namely oleoyl carboxymethyl chitosan (OCMCs), N,N-dimethylhexadecyl carboxymethyl chitosan (DCMCs) and deoxycholic acid carboxymethyl chitosan (DACMCs) as carrier agents for rotenone in water-insoluble pesticide formulations was investigated. Fourier Transform Infrared (FTIR) Spectrometer, CHN-O Elemental Analyser (CHN-O) and Transmission Electron Microscope (TEM) were used to characterise amphiphilic chitosan derivatives. The critical micelle concentration (CMC) of amphiphilic chitosan derivatives was determined using a Fluorescence Spectrometer. A High Performance Liquid Chromatography (HPLC) was used to determine the ability of OCMCs, DCMCs and DACMCs to load and release rotenone in an in vitro system. Based on TEM analysis, results have shown that amphiphilic chitosan derivatives formed self-assembly and exhibited spherical shape. The CMC values determined for OCMCs, DCMCs and DACMCs were 0.093, 0.098 and 0.468 mg/mL, respectively. The encapsulation efficiency (EE) values for the materials were more than 97.0%, meanwhile the loading capacity (LC) values were greater than 0.90%. OCMCs, DCMCs and DACMCs micelles exhibited an excellent ability to control the release of rotenone, of which 90.0% of rotenone was released within 40 to 52 h. In conclusion, OCMCs, DCMCs and DACMCs possess several key features to act as effective carrier agents for rotenone. Overall, amphiphilic chitosan derivatives produced in this study were successfully increased the solubility of rotenone by 49.0 times higher than free rotenone.

TOF-SIMS Analysis of Red Color Inks of Writing and Printing Tools on Questioned Documents.

PubMed

Lee, Jihye; Nam, Yun Sik; Min, Jisook; Lee, Kang-Bong; Lee, Yeonhee

2016-05-01

Time-of-flight secondary ion mass spectrometry (TOF-SIMS) is a well-established surface technique that provides both elemental and molecular information from several monolayers of a sample surface while also allowing depth profiling or image mapping to be performed. Static TOF-SIMS with improved performances has expanded the application of TOF-SIMS to the study of a variety of organic, polymeric, biological, archaeological, and forensic materials. In forensic investigation, the use of a minimal sample for the analysis is preferable. Although the TOF-SIMS technique is destructive, the probing beams have microsized diameters so that only small portion of the questioned sample is necessary for the analysis, leaving the rest available for other analyses. In this study, TOF-SIMS and attenuated total reflectance Fourier transform infrared (ATR-FTIR) were applied to the analysis of several different pen inks, red sealing inks, and printed patterns on paper. The overlapping areas of ballpoint pen writing, red seal stamping, and laser printing in a document were investigated to identify the sequence of recording. The sequence relations for various cases were determined from the TOF-SIMS mapping image and the depth profile. TOF-SIMS images were also used to investigate numbers or characters altered with two different red pens. TOF-SIMS was successfully used to determine the sequence of intersecting lines and the forged numbers on the paper. © 2016 American Academy of Forensic Sciences.

Quantum, characterization and spectroscopic studies on Cu(II), Pd(II) and Pt(II) complexes of 1-(benzo[d]thiazol-2-yl)-3-phenylthiourea and its biological application as antimicrobial and antioxidant

NASA Astrophysics Data System (ADS)

Jambi, M. S.

2017-09-01

Divalent platinum, palladium and copper chelates of H2PhT have been isolated and identified. Their structures have been elucidated by partial elemental analyses, magnetic susceptibilities and spectroscopic estimations and additionally mass spectra. The FTIR and 1H NMR studies illustrated that H2PhT performs as mono-negative bi-dentate in Cu(II) and Pd(II) complexes while it behaves as neutral bi-dentate in both Pt(II) complexes. Both magnetic moments and spectral studies suggests a tetrahedral coordination geometry for [Cu(HPhT)(H2O)Cl] complex, a square planar geometry for both [Pd(HPhT)2] and [Pt(H2PhT)2Cl2] complexes and octahedral geometry for [Pt(H2PhT)2Cl2] complex. The molecular modeling are drawn and demonstrated both bond lengths and angles, chemical reactivity, MEP, NLO, Mulliken atomic charges, and binding energy (kcal/mol) for the investigated compounds. Theoretical infrared intensities and 1H NMR of H2PhT was computed utilizing DFT technique. An examination of the experimental and hypothetical spectra can be extremely valuable in making right assignments and analyzing the main chemical shift. DNA bioassay, antibacterial and antifungal activities of the investigated compounds have been determined.

Synthesis, characterization and cytotoxic activity of substituted benzyl iminoether Pt(II) complexes of the type cis- and trans-[PtCl2{E-N(H)=C(OMe)CH2-C6H4-p-R}2] (R=Me, OMe, F). X-ray structure of trans-[PtCl2{E-N(H)=C(OMe)CH2-C6H4-p-F}2].

PubMed

Mazzega Sbovata, Silvia; Bettio, Frazia; Marzano, Christine; Tassan, Augusto; Mozzon, Mirto; Bertani, Roberta; Benetollo, Franco; Michelin, Rino A

2008-04-01

New substituted benzyl iminoether derivatives of the type cis- and trans-[PtCl(2){E-N(H)C(OMe)CH(2)-C(6)H(4)-p-R}(2)] (R=Me (1a, 2a), OMe (3a, 4a), F (5a, 6a)) have been synthesized and characterized by elemental analyses, FT-IR spectroscopy and NMR techniques. The iminoether ligands are in the E configuration, which is stable in solution and in the solid state, as confirmed by the (1)H NMR data. Complex trans-[PtCl(2){E-N(H)C(OMe)CH(2)-C(6)H(4)-p-F}(2)] (6a) was also characterized by an X-ray diffraction study. Complexes 1a-6a have been tested against a panel of human tumor cell lines in order to evaluate their cytotoxic activity. cis-Isomers were significant more potent than the corresponding trans-isomers against all tumor cell lines tested; moreover, complexes 1a and 5a showed IC(50) values from about 2-fold to 6-fold lower than those exhibited by cisplatin, used as reference platinum anticancer drug.

Catalytic pyrolysis of car tire waste using expanded perlite.

PubMed

Kar, Y

2011-08-01

In this study, the non-catalytic and catalytic pyrolysis experiments were conducted on the sample of tire waste using expanded perlite as an additive material to determine especially the effect of temperature and catalyst-to-tire ratio on the products yields and the compositions and qualities of pyrolytic oils (NCPO and CPO). Non-catalytic studies, which were carried out under the certain conditions (a nitrogen flow of 100mL/min and a heating rate of 10°C/min), showed that the highest yield of pyrolytic oil (NCPO) was 60.02wt.% at 425°C. Then, the catalytic pyrolysis studies were carried out at catalyst-to-tire ratio range of 0.05-0.25 and the highest catalytic pyrolytic oil (CPO) yield was 65.11wt.% at the ratio of 0.10 with the yield increase of 8.48wt.% compared with the non-catalytic pyrolysis. Lastly, the pyrolytic oils were characterized with applying a various techniques such as elemental analyses and various chromatographic and spectroscopic techniques (GC-MS, (1)H NMR, FT-IR, etc.). The characterization results revealed that the pyrolytic oils which were complex mixtures of C(5)-C(15) organic compounds (predominantly aromatic compounds) and also the CPO compared to the NCPO was more similar to conventional fuels in view of the certain fuel properties. Copyright © 2011 Elsevier Ltd. All rights reserved.

Synthesis of novel Schiff's bases of highly potential biological activities and their structure investigation.

PubMed

Zayed, Ehab M; Zayed, M A

2015-05-15

Novel bisaldehyde-hydrazide Schiff's bases AS1 (2,2'-(ethane-1,2-diylbis(oxy))dibenzaldehyde terephthalohydrazide) and AS2 (N',N'″-(((ethane-1,2-diylbis(oxy))bis(2,1-phenylene))bis(methanylylidene))di(benzohydrazide)) were prepared as new macrocyclic compounds via condensation reactions. AS1 had been prepared by condensation between (2,2'-(ethane-1,2-diylbis(oxy))dibenzaldehyde) bisaldehyde and terephthalohydrazide in a ratio1:1. AS2 had been obtained by condensation between (2,2'-(ethane-1,2-diylbis(oxy))dibenzaldehyde) bisaldehyde and benzohydrazide in ratio 1:2. The structures of AS1 and AS2 were characterized by elemental analysis (EA), mass (MS), FT-IR and (1)H-NMR spectra, and thermal analyses (TG, DTG). The activation thermodynamic parameters such as ΔE(∗), ΔH(∗), ΔS(∗) and ΔG(∗) were calculated from the TG curves using Coats-Redfern method. It is important to investigate their molecular structures to know the active groups and weak bonds responsible for their biological activities. Consequently in the present work, the obtained thermal (TA) and mass (MS) practical results are confirmed by semi-empirical MO-calculations (MOCS) using PM3 procedure. Their biological activities had been tested in vitro against Escherichia coli, Proteus vulgaris, Bacillus subtilis and Staphylococcus aurous bacteria in order to assess their anti-microbial potential. Copyright © 2015 Elsevier B.V. All rights reserved.

Converting inert plastic waste into energetic materials: A study on the light-accelerated decomposition of plastic waste with the Fenton reaction.

PubMed

Chow, Cheuk-Fai; Wong, Wing-Leung; Chan, Ching-Wan; Chan, Chung-Sum

2018-05-01

Better treatment and management strategies than landfilling are needed to address the large quantities of unrecycled plastic waste generated by daily human activities. Waste-to-energy conversion is an ideal benchmark for developing future large-scale waste management technologies. The present study explores a new approach for producing energetic materials by converting inert plastic waste into energy (thermal and mechanical energies) via a light-controlled process through the simple chemical activation of plastic waste, including polyethylene, polypropylene, and polyvinyl chloride. The inert and non-polar polymer surfaces of the plastics were modified by generating a number of sulfonic groups (SO 3 - ) using chlorosulfuric acid, followed by grafting of Fe(III) catalyst onto the polymer chains to obtain activated polymer. Elemental analyses of these activated materials showed that the carbon-to-sulfur ratio ranged from 3:1 to 5:1. The FTIR spectra indicated the presence of CC bonds (v C=C : 1615-1630 cm -1 ) and SO bonds (v S=O : 1151-1167 cm -1 ) in the activated polymers after chemical reaction. These activated materials were energetic, as light could be used to convert them into thermal (1800-3200 J/g) and mechanical energies (380-560 kPa/g) using hydrogen peroxide as the oxidant under ambient conditions within 1 h. Copyright © 2018 Elsevier Ltd. All rights reserved.

As(III) and As(V) sorption on iron-modified non-pyrolyzed and pyrolyzed biomass from Petroselinum crispum (parsley).

PubMed

Jiménez-Cedillo, M J; Olguín, M T; Fall, C; Colin-Cruz, A

2013-03-15

The sorption of As(III) and As(V) from aqueous solutions onto iron-modified Petroselinum crispum (PCFe) and iron-modified carbonaceous material from the pyrolysis of P. crispum (PCTTFe) was investigated. The modified sorbents were characterized with scanning electron microscopy. The sorbent elemental composition was determined with energy-dispersive X-ray spectroscopy (EDS). The principal functional groups from the sorbents were determined with FT-IR. The specific surfaces and points of zero charge (pzc) of the materials were also determined. As(III) and As(V) sorption onto the modified sorbents were performed in a batch system. After the sorption process, the As content in the liquid and solid phases was determined with atomic absorption and neutron activation analyses, respectively. After the arsenic sorption processes, the desorption of Fe from PCFe and PCTTFe was verified with atomic absorption spectrometry. The morphology of PC changed after iron modification. The specific area and pzc differed significantly between the iron-modified non-pyrolyzed and pyrolyzed P. crispum. The kinetics of the arsenite and arsenate sorption processes were described with a pseudo-second-order model. The Langmuir-Freundlich model provided the isotherms with the best fit. Less than 0.02% of the Fe was desorbed from the PCFe and PCTTFe after the As(III) and As(V) sorption processes. Copyright © 2013 Elsevier Ltd. All rights reserved.

Study of structural, surface and hydrogen storage properties of boric acid mediated metal (sodium)-organic frameworks

NASA Astrophysics Data System (ADS)

Ozer, Demet; Köse, Dursun A.; Sahin, Onur; Oztas, Nursen A.

2018-04-01

Three boric acid mediated metal organic frameworks were synthesized by solution method with using succinic acid, fumaric acid and acetylene dicarboxylic acid as a ligand source and sodium as a metal source. The complexes were characterized by FT-IR, powder XRD, elemental analyses and single crystal measurements. The complexes with the formula, C4H18B2Na2O14, C4H16B2Na2O14 and C4H14B2Na2O14 were successfully obtained. BET surface area of complexes were calculated and found as 13.474 m2/g for catena-(tetrakis(μ2-hydroxo)-(μ2-trihydrogen borate)-(μ2-succinato)-di-sodium boric acid solvate), 1.692 m2/g for catena-(tetrakis(μ2-hydroxo)-(μ2-trihydrogen borate)-(μ2-fumarato)-di-sodium boric acid solvate) and 5.600 m2/g for catena-(tetrakis(μ2-hydroxo)-(μ2-trihydrogen borate)-(μ2-acetylenedicarboxylato)-di-sodium boric acid solvate). Hydrogen storage capacities of the complexes were also studied at 77 K 1 bar pressure and found as 0.108%, 0.033%, 0.021% by mass. When different ligands were used, the pore volume, pore width and surface area of the obtained complexes were changed. As a consequence, hydrogen storage capacities also changed.

Role of manganese dioxide in the recovery of oxide-sulphide zinc ore.

PubMed

Yang, Kun; Zhang, Libo; Zhu, Xingcai; Peng, Jinhui; Li, Shiwei; Ma, Aiyuan; Li, Haoyu; Zhu, Fei

2018-02-05

In this article, the role of MnO 2 in the recovery of oxide-sulphide zinc ore discussed. Through adopting various modern analysis techniques (such as X-ray diffraction pattern, X-ray photoelectron spectroscopy, scanning electron microscope, energy dispersive X-ray analysis, and fourier transform infrared spectroscopy), the function and mechanism of MnO 2 during the phase transformation process is found out. Thermodynamic mechanisms involved in the phase transformation process with or without addition of manganese dioxide investigated by exploiting the Equilib module of FactSage. What's more, XRD patterns, XPS spectra and SEM-EDAX analyses of zinc calcines verify well the calculations of FactSage. Results reveal that the addition of MnO 2 will produce an aggregation of ZnMn 2 O 4 , a valuable energy material, while roasting on its own, results in generating undesirable Zn 2 SiO 4 , the oxidation degree being relatively low. Moreover, XRD pattern of zinc calcine and FT-IR spectrum of yellow product collected in the calcination process prove that the sulphur-fixing value of the additive MnO 2 , which can promote transforming to the elemental sulphur. The volatile S can be collected through a simple guiding device. In this process, the emission of SO 2 effectively avoids, thus MnO 2 deems as a potential additive in the recovery of oxide-sulphide zinc ore. Copyright © 2017. Published by Elsevier B.V.

Spectroscopic and thermal properties of short wavelength metal (II) complexes containing α-isoxazolylazo-β-diketones as co-ligands

NASA Astrophysics Data System (ADS)

Huang, Fuxin; Wu, Yiqun; Gu, Donghong; Gan, Fuxi

2005-10-01

Two new azo dyes of α-isoxazolylazo-β-diketones and their Ni(II) and Cu(II) complexes with blue-violet light wavelength were synthesized using a coupling component, different diazo components and metal (II) ions (Ni 2+ and Cu 2+). Based on the elemental analysis, MS spectra and FT-IR spectral analyses, azo dyes were unequivocally shown to exist as hydrazoketo and azoenol forms which were respectively obtained from the solution forms and from the solid forms. The action of sodium methoxide (NaOMe) on azo dyes in solutions converts hydrazoketo form into azoenol form, so azo dyes are coordinated with metal (II) ions as co-ligands in the azoenol forms. The solubility of all the compounds in common organic solvents such as 2,2,3,3-tetrafluoro-1-propanol (TFP) or chloroform (CHCl 3) and absorption properties of spin-coating thin films were measured. The difference of absorption maxima from the complexes to their ligands was discussed. In addition, the TG analysis of the complexes was also determined, and their thermal stability was evaluated. It is found that these new metal (II) complexes had potential application for high-density digital versatile disc-recordable (HD-DVD-R) system due to their good solubility in organic solvents, reasonable and controllable absorption spectra in blue-violet light region and high thermal stability.

Comparison of the bulk geochemical features and thermal reactivity of kerogens from Mol (Boom Clay), Bure (Callovo-Oxfordian argillite) and Tournemire (Toarcian shales) underground research laboratories.

PubMed

Deniau, I; Devol-Brown, I; Derenne, S; Behar, F; Largeau, C

2008-01-25

Deep argillaceous formations are potential repositories for the long-term disposal of nuclear waste because of their low permeability and high sorption capacity with respect to radioelements and heavy metals. Such sedimentary rocks contain organic matter, mostly macromolecular and insoluble (kerogen). Upon temperature elevation related to high-level long-lived radioactive waste disposal, the kerogen may release significant quantities of gaseous and liquid effluents, especially oxygen-containing ones, which may influence the ability of the clay to retain radionuclides. The aim of the present study is to assess the global geochemical features and the thermal reactivity of the kerogens isolated from samples collected in the Bure and Tournemire sites, France (Callovo-Oxfordian Clay and Toarcian Shales, respectively) and to draw comparisons with data previously obtained for the Mol site, Belgium (Boom Clay). The study is based on a combination of elemental, spectroscopic (FTIR, solid state (13)C NMR) and pyrolytic (Rock-Eval pyrolysis, Curie point pyrolysis-gas chromatography/mass spectrometry) analyses. Different levels of maturity and resulting differences in the relative abundance of oxygen-containing groups were thus observed for the three kerogens. This is linked with differences in their ability to generate CO(2) and various oxygen-containing, low molecular weight, water-soluble compounds under thermal stress, decreasing from Mol to Bure and to Tournemire.

In vitro anticancer activities of Schiff base and its lanthanum complex

NASA Astrophysics Data System (ADS)

Neelima; Poonia, Kavita; Siddiqui, Sahabjada; Arshad, Md; Kumar, Dinesh

2016-02-01

Schiff base metal complexes are well-known to intercalate DNA. The La(III) complexes have been synthesized such that they hinder with the role of the topoisomerases, which control the topology of DNA during the cell-division cycle. Although several promising chemotherapeutics have been developed, on the basis of Schiff base metal complex DNA intercalating system they did not proceed past clinical trials due to their dose-limiting toxicity. Herein, we discuss an alternative compound, the La(III) complex, [La(L1)2Cl3]·7H2O based on a Schiff base ligand 2,3-dihydro-1H-indolo-[2,3-b]-phenazin-4(5H)-ylidene)benzothiazole-2-amine (L1), and report in vitro cell studies. Results of antitumor activity using cell viability assay, reactive oxygen species (ROS) generation and nuclear condensation in PC-3 (Human, prostate carcinoma) cells show that the metal complex is more potent than ligand. La(III) complexes have been synthesized by reaction of lanthanum(III) salt in 1:2 M ratio with ligands L1 and 3-(ethoxymethylene)-2,3-dihydro-1H-indolo[2,3-b]-phenazin-4(5H)-ylidene)benzathiazole-2-amine (L2) in methanol. The ligands and their La(III) complexes were characterized by molar conductance, magnetic susceptibility, elemental analyses, FT-IR, UV-Vis, 1H/13C NMR, thermogravimetric, XRD, and SEM analysis.

Synthesis of novel Schiff's bases of highly potential biological activities and their structure investigation

NASA Astrophysics Data System (ADS)

Zayed, Ehab M.; Zayed, M. A.

2015-05-01

Novel bisaldehyde-hydrazide Schiff's bases AS1 (2,2‧-(ethane-1,2-diylbis(oxy))dibenzaldehyde terephthalohydrazide) and AS2 (N‧,N‧″-(((ethane-1,2-diylbis(oxy))bis(2,1-phenylene))bis(methanylylidene))di(benzohydrazide)) were prepared as new macrocyclic compounds via condensation reactions. AS1 had been prepared by condensation between (2,2‧-(ethane-1,2-diylbis(oxy))dibenzaldehyde) bisaldehyde and terephthalohydrazide in a ratio1:1. AS2 had been obtained by condensation between (2,2‧-(ethane-1,2-diylbis(oxy))dibenzaldehyde) bisaldehyde and benzohydrazide in ratio 1:2. The structures of AS1 and AS2 were characterized by elemental analysis (EA), mass (MS), FT-IR and 1H-NMR spectra, and thermal analyses (TG, DTG). The activation thermodynamic parameters such as ΔE∗, ΔH∗, ΔS∗ and ΔG∗ were calculated from the TG curves using Coats-Redfern method. It is important to investigate their molecular structures to know the active groups and weak bonds responsible for their biological activities. Consequently in the present work, the obtained thermal (TA) and mass (MS) practical results are confirmed by semi-empirical MO-calculations (MOCS) using PM3 procedure. Their biological activities had been tested in vitro against Escherichia coli, Proteus vulgaris, Bacillus subtilis and Staphylococcus aurous bacteria in order to assess their anti-microbial potential.

Reactivity of tris(acetylacetonato) iron(III) with tridentate [ONO] donor Schiff base as an access to newer mixed-ligand iron(III) complexes

NASA Astrophysics Data System (ADS)

Bhattacharjee, Chira R.; Goswami, Pankaj; Pramanik, Harun A. R.; Paul, Pradip C.; Mondal, Paritosh

2011-05-01

Two new mixed-ligand iron(III) complexes, [Fe(L n)(acac)(C 2H 5OH)] incorporating coordinated ethanol from the reaction solvent were accessed from the reaction of [Fe(acac) 3] with [ONO] donor dibasic tridentate unsymmetrical Schiff base ligands derived from condensation of 2-hydroxy-1-napthaldehyde with 2-aminophenol (H 2L 1) or 2-aminobenzoic acid (H 2L 2). The thermal study (TGA-DTA) provided evidence for weakly bound ethanol which is readily substituted by neutral N-donor molecule imidazole, benzimidazole or pyridine to produce an array of newer complexes, [Fe(L n)(acac)X] ( n = 1, 2; X = Im, Bim, Py). The compounds were characterized by elemental analyses, FT-IR, UV-vis, solution electrical conductivity, FAB mass, 1H and 13C NMR spectroscopy. Room temperature magnetic susceptibility measurements ( μeff ˜ 5.8 B.M.) are consistent with spin-free octahedral iron(III) complexes. Cyclic voltammetry of ethanol complexes revealed a quasi-reversible one electron redox response (Δ Ep > 100 mV) for the Fe(III)/Fe(II) couple. Low half wave redox potential ( E1/2) values suggested easy redox susceptibility. The ground state geometries of the ethanol and imidazole complexes have been ascertained to be distorted octahedral by density functional theory using DMol3 program at BLYP/DNP level.

Methotrexate conjugated magnetic nanoparticle for targeted drug delivery and thermal therapy

NASA Astrophysics Data System (ADS)

Gupta, Jagriti; Bhargava, Parag; Bahadur, D.

2014-05-01

A simple soft chemical approach is used for the preparation of citrate functionalized iron oxide (Fe3O4) aqueous colloidal magnetic nanoparticles (CA-MNPs) of average size ˜10 nm. The CA-MNPs exhibit superparamagnetic behavior at room temperature with strong field dependent magnetic responsivity. The CA-MNPs can be conjugated with Methotrexate (MTX) drug through amide bonds between the carboxylic group on the surface of MNPs and amine group of MTX. The surface functionalization of Fe3O4 nanoparticles with citric acid and conjugation of MTX drug is evident from FTIR spectroscopy, zeta-potential measurement, and elemental and thermal analyses. From the drug release study, it has been observed that this bonding of MTX conjugated MNPs (MTX-MNPs) is cleaved by the intracellular enzymes in lysosome, and MTX is delivered largely inside target cancerous cells at lower pH, thereby reducing toxicity to normal cells. Also, it has been observed that the intercellular uptake of MTX-MNPs is higher compared to CA-MNPs. In addition, the aqueous colloidal stability, optimal magnetization, and good specific absorption rate (under external AC magnetic field) of CA-MNPs act as effective heating source for thermal therapy. Cytotoxicity study of MTX-MNPs shows the reduction of cellular viability for human cervical cancer cells (HeLa). Further, a synergistic effect of MTX-MNPs shows a more effective tumor cell death due to the combined effect of thermo-chemotherapy.