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Sample records for total reflection atr

  1. Characterization of Printing Inks Using DART-Q-TOF-MS and Attenuated Total Reflectance (ATR) FTIR.

    PubMed

    Williamson, Rhett; Raeva, Anna; Almirall, Jose R

    2016-05-01

    The rise in improved and widely accessible printing technology has resulted in an interest to develop rapid and minimally destructive chemical analytical techniques that can characterize printing inks for forensic document analysis. Chemical characterization of printing inks allows for both discrimination of inks originating from different sources and the association of inks originating from the same source. Direct analysis in real-time mass spectrometry (DART-MS) and attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR) were used in tandem to analyze four different classes of printing inks: inkjets, toners, offset, and intaglio. A total of 319 samples or ~ 80 samples from each class were analyzed directly on a paper substrate using the two methods. DART-MS was found to characterize the semi-volatile polymeric vehicle components, while ATR-FTIR provided chemical information associated with the bulk components of these inks. Complimentary data results in improved discrimination when both techniques are used in succession resulting in >96% discrimination for all toners, 95% for all inkjets, >92% for all offset, and >54% for all intaglio inks. PMID:27122410

  2. Unidirectional Excitation of Graphene Plasmon in Attenuated Total Reflection (ATR) Configuration

    NASA Astrophysics Data System (ADS)

    Dai, Wei; Wu, Yue-Chao; Liu, Fang-Li

    2016-04-01

    Graphene plasmon has been attracting interests from both theoretical and experimental research due to its gate tunability and potential applications in the terahertz frequency range. Here, we propose an effective scheme to unidirectionally excite the graphene plasmon by exploiting magneto-optical materials in the famous attenuated total reflection (ATR) configuration. We show that the graphene plasmon dispersion relation in such a device is asymmetric in different exciting directions, thus making it possible to couple the incident light unidirectionally to the propagating plasmon. The split of absorption spectrum of graphene clearly indicates that under a magnetic field for one single frequency, graphene plasmon can only be excited in one direction. The possible gate tunablity of excitation direction and the further application of the proposed scheme, such as optical isolator, also are discussed.

  3. Analysis of H2O in silicate glass using attenuated total reflectance (ATR) micro-FTIR spectroscopy

    USGS Publications Warehouse

    Lowenstern, Jacob B.; Pitcher, Bradley W.

    2013-01-01

    We present a calibration for attenuated total reflectance (ATR) micro-FTIR for analysis of H2O in hydrous glass. A Ge ATR accessory was used to measure evanescent wave absorption by H2O within hydrous rhyolite and other standards. Absorbance at 3450 cm−1 (representing total H2O or H2Ot) and 1630 cm−1 (molecular H2O or H2Om) showed high correlation with measured H2O in the glasses as determined by transmission FTIR spectroscopy and manometry. For rhyolite, wt%H2O=245(±9)×A3450-0.22(±0.03) and wt%H2Om=235(±11)×A1630-0.20(±0.03) where A3450 and A1630 represent the ATR absorption at the relevant infrared wavelengths. The calibration permits determination of volatiles in singly polished glass samples with spot size down to ~5 μm (for H2O-rich samples) and detection limits of ~0.1 wt% H2O. Basaltic, basaltic andesite and dacitic glasses of known H2O concentrations fall along a density-adjusted calibration, indicating that ATR is relatively insensitive to glass composition, at least for calc-alkaline glasses. The following equation allows quantification of H2O in silicate glasses that range in composition from basalt to rhyolite: wt%H2O=(ω×A3450/ρ)+b where ω = 550 ± 21, b = −0.19 ± 0.03, ρ = density, in g/cm3, and A3450 is the ATR absorbance at 3450 cm−1. The ATR micro-FTIR technique is less sensitive than transmission FTIR, but requires only a singly polished sample for quantitative results, thus minimizing time for sample preparation. Compared with specular reflectance, it is more sensitive and better suited for imaging of H2O variations in heterogeneous samples such as melt inclusions. One drawback is that the technique can damage fragile samples and we therefore recommend mounting of unknowns in epoxy prior to polishing. Our calibration should hold for any Ge ATR crystals with the same incident angle (31°). Use of a different crystal type or geometry would require measurement of several H2O-bearing standards to provide a crystal-specific calibration.

  4. Historical perspective and modern applications of Attenuated Total Reflectance-Fourier Transform Infrared Spectroscopy (ATR-FTIR).

    PubMed

    Blum, Marc-Michael; John, Harald

    2012-01-01

    Vibrational spectroscopy has a long history as an important spectroscopic method in chemical and pharmaceutical analysis. Instrumentation for infrared (IR) spectroscopy was revolutionized by the introduction of Fourier Transform Infrared (FTIR) spectrometers. In addition, easier sampling combined with better sample-to-sample reproducibility and user-to-user spectral variation became available with attenuated total reflectance (ATR) probes and their application for in situ IR spectroscopy. These innovations allow many new applications in chemical and pharmaceutical analysis, such as the use of IR spectroscopy in Process Analytical Chemistry (PAC), the quantitation of drugs in complex matrix formulations, the analysis of protein binding and function and in combination with IR microscopy to the emergence of IR imaging technologies. The use of ATR-FTIR instruments in forensics and first response to 'white powder' incidents is also discussed. A short overview is given in this perspective article with the aim to renew and intensify interest in IR spectroscopy. PMID:22113892

  5. A quantitative study for determination of sugar concentration using attenuated total reflectance terahertz (ATR-THz) spectroscopy

    NASA Astrophysics Data System (ADS)

    Suhandy, Diding; Suzuki, Tetsuhito; Ogawa, Yuichi; Kondo, Naoshi; Ishihara, Takeshi; Takemoto, Yuichiro

    2011-06-01

    The objective of our research was to use ATR-THz spectroscopy together with chemometric for quantitative study in food analysis. Glucose, fructose and sucrose are main component of sugar both in fresh and processed fruits. The use of spectroscopic-based method for sugar determination is well reported especially using visible, near infrared (NIR) and middle infrared (MIR) spectroscopy. However, the use of terahertz spectroscopy for sugar determination in fruits has not yet been reported. In this work, a quantitative study for sugars determination using attenuated total reflectance terahertz (ATR-THz) spectroscopy was conducted. Each samples of glucose, fructose and sucrose solution with different concentrations were prepared respectively and their absorbance spectra between wavenumber 20 and 450 cm-1 (between 0.6 THz and 13.5 THz) were acquired using a terahertz-based Fourier Transform spectrometer (FARIS-1S, JASCO Co., Japan). This spectrometer was equipped with a high pressure of mercury lamp as light source and a pyroelectric sensor made from deuterated L-alanine triglycine sulfate (DLTGS) as detector. Each spectrum was acquired using 16 cm-1 of resolution and 200 scans for averaging. The spectra of water and sugar solutions were compared and discussed. The results showed that increasing sugar concentration caused decreasing absorbance. The correlation between sugar concentration and its spectra was investigated using multivariate analysis. Calibration models for glucose, fructose and sucrose determination were developed using partial least squares (PLS) regression. The calibration model was evaluated using some parameters such as coefficient of determination (R2), standard error of calibration (SEC), standard error of prediction (SEP), bias between actual and predicted sugar concentration value and ratio prediction to deviation (RPD) parameter. The cross validation method was used to validate each calibration model. It is showed that the use of ATR-THz spectroscopy combined with appropriate chemometric can be a potential for a rapid determination of sugar concentrations.

  6. Attenuated total reflection Fourier transform infrared (ATR-FTIR) spectroscopic analysis of regenerated bone

    NASA Astrophysics Data System (ADS)

    Benetti, Carolina; Kazarain, Sergei G.; Alves, Marco A. V.; Blay, Alberto; Correa, Luciana; Zezell, Denise M.

    2014-03-01

    The cutting of bone is routinely required in medical procedures, especially in dental applications. In such cases, bone regeneration and new bone quality can determine the success of the treatment. This study investigated the main spectral differences of undamaged and healed bone using the ATR-FTIR spectroscopy technique. Three rabbits were submitted to a surgical procedure; a small piece of bone (3x3 mm2) was removed from both sides of their jaws using a high speed drill. After 15 days, the rabbits were euthanized and the jaws were removed. A bone slice was cut from each side of the jaw containing regions of undamaged and newly formed bone, resulting in six samples which were polished for spectroscopic comparison. The samples were analyzed by FTIR spectroscopy using a diamond ATR accessory. Spectral characteristics were compared and particular attention was paid to the proportion of phosphate to amide I bands and the width of the phosphate band. The results show that the ratio of phosphate to amide I is smaller in new bone tissue than in the undamaged bone, indicating a higher organic content in the newly formed bone. The analysis of the width of the phosphate band suggests a crystallinity difference between both tissues, since the width was higher in the new bone than in the natural bone. These results suggest that the differences observed in bone aging processes by FTIR spectroscopic can be applied to the study of healing processes.

  7. Attenuated total reflection (ATR) Fourier transform infrared (FT-IR) spectroscopy of oxidized polymer-modified bitumens.

    PubMed

    Yut, Iliya; Zofka, Adam

    2011-07-01

    Oxidative age hardening of bitumen results in increasing fatigue susceptibility of bituminous mixtures, thus reducing the service life of asphalt pavements. Polymer additives to bitumen have been shown to improve its viscoelastic properties and, in some cases, reduce the level of bitumen hardening. Fourier transform infrared (FT-IR) spectroscopy enables evaluation of oxidation levels in bitumen by measuring the concentration of oxygen-containing chemical functionalities. This paper summarizes the results of the investigation of oxidative age hardening of polymer-modified bitumens (PMB) caused by accelerated aging in laboratory conditions. The PMB samples are prepared with different concentrations of styrene-butadiene-based co-polymers. Next, the PMB samples are aged using standard procedures that employ air blowing at 163 °C for 85 min followed by conditioning the samples at 100 °C and 2.1 MPa pressure for 20 to 48 hours. The resultant changes in their chemical composition are evaluated by portable attenuated total reflection (ATR) spectrometer. Measurements of ketone, sulfoxide, and hydroxyl content in PMB samples indicated similar oxidation pathways to those of non-modified bitumens. In addition, no evidence of polymer degradation due to accelerated aging of PMB was found in this study. PMID:21740638

  8. Use of total internal reflection Raman (TIR) and attenuated total reflection infrared (ATR-IR) spectroscopy to analyze component separation in thin offset ink films after setting on coated paper surfaces.

    PubMed

    Kivioja, Antti; Hartus, Timo; Vuorinen, Tapani; Gane, Patrick; Jääskeläinen, Anna-Stiina

    2013-06-01

    The interactive behavior of ink constituents with porous substrates during and after the offset print process has an important effect on the quality of printed products. To help elucidate the distribution of ink components between the retained ink layer and the substrate, a variety of spectroscopic and microscopic analysis techniques have been developed. This paper describes for the first time the use of total internal reflection (TIR) Raman spectroscopy to analyze the penetration behavior of separated offset ink components (linseed oil, solid color pigment) in coated papers providing chemically intrinsic information rapidly, nondestructively, and with minimal sample preparation. In addition, the already widely applied technique of attenuated total reflection infrared spectroscopy (ATR-IR) was evaluated in parallel and compared. The results of the ATR-IR Raman clearly revealed an improvement in uppermost depth resolution compared with values previously published from other nondestructive techniques, and the method is shown to be capable of providing new knowledge of the setting of thin (0.25-2 μm) offset ink films, allowing the spreading and the penetration behavior on physically different paper coating surfaces to be studied. PMID:23735252

  9. Fluorescence, CD, attenuated total reflectance (ATR) FTIR, and sup 13 C NMR characterization of the structure and dynamics of synthetic melittin and melittin analogues in lipid environments

    SciTech Connect

    Weaver, A.J.; Prendergast, F.G. ); Kemple, M.D. ); Brauner, J.W.; Mendelsohn, R. )

    1992-02-11

    The structure and dynamics of synthetic melittin (MLT) and MLT analogues bound to monomyristoylphosphatidylcholine micelles, dimyristoylphosphatidylcholine vesicles, and diacylphosphatidylcholine films have been investigated by fluorescence, CD, attenuated total reflectance (ATR) FTIR, and {sup 13}C NMR spectroscopy. All of these methods provide information about peptide secondary structure and/or about the environment of the single tryptophan side chain in these lipid environments. ATR-FTIR data provide additional information about the orientation of helical peptide segments with respect to the bilayer plane. Steady-state fluorescence anisotropy, fluorescence lifetime, and {sup 13}C NMR relaxation data are used in concert to provide quantitative information about the dynamics of a single {sup 13}C{alpha}-labeled glycine incorporated into each of the MLT peptides at position 12. The cumulative structural and dynamic data are consistent with a model wherein the N-terminal {alpha}-helical segment of these peptides is oriented perpendicular to the bilayer plane. Correlation times for the lysolipid-peptide complexes provide evidence for binding of a single peptide monomer per micelle. A model for the membranolytic action of MLT and MLT-like peptides is proposed.

  10. Sensing cocaine in saliva with attenuated total reflection infrared (ATR-IR) spectroscopy combined with a one-step extraction method

    NASA Astrophysics Data System (ADS)

    Hans, Kerstin M.-C.; Gianella, Michele; Sigrist, Markus W.

    2012-03-01

    On-site drug tests have gained importance, e.g., for protecting the society from impaired drivers. Since today's drug tests are majorly only positive/negative, there is a great need for a reliable, portable and preferentially quantitative drug test. In the project IrSens we aim to bridge this gap with the development of an optical sensor platform based on infrared spectroscopy and focus on cocaine detection in saliva. We combine a one-step extraction method, a sample drying technique and infrared attenuated total reflection (ATR) spectroscopy. As a first step we have developed an extraction technique that allows us to extract cocaine from saliva to an almost infrared-transparent solvent and to record ATR spectra with a commercially available Fourier Transform-infrared spectrometer. To the best of our knowledge this is the first time that such a simple and easy-to-use one-step extraction method is used to transfer cocaine from saliva into an organic solvent and detect it quantitatively. With this new method we are able to reach a current limit of detection around 10 μg/ml. This new extraction method could also be applied to waste water monitoring and controlling caffeine content in beverages.

  11. Detection and quantification of soymilk in cow-buffalo milk using Attenuated Total Reflectance Fourier Transform Infrared spectroscopy (ATR-FTIR).

    PubMed

    Jaiswal, Pranita; Jha, Shyam Narayan; Borah, Anjan; Gautam, Anuj; Grewal, Manpreet Kaur; Jindal, Gaurav

    2015-02-01

    Milk consumption is steadily increasing, especially in India and China, due to rising income. To bridge the gap between supply and demand, unscrupulous milk vendors add milk-like products from vegetable sources (soymilk) to milk without declaration. A rapid detection technique is required to enforce the safety norms of food regulatory authorities. Fourier Transform Infrared (FTIR) spectroscopy has demonstrated potential as a rapid quality monitoring method and was therefore explored for detection of soymilk in milk. In the present work, spectra of milk, soymilk (SM), and milk adulterated with known quantity of SM were acquired in the wave number range of 4000-500cm(-1) using Attenuated Total Reflectance (ATR)-FTIR. The acquired spectra revealed differences amongst milk, SM and adulterated milk (AM) samples in the wave number range of 1680-1058cm(-1). This region encompasses the absorption frequency of amide-I, amide-II, amide-III, beta-sheet protein, α-tocopherol and Soybean Kunitz Trypsin Inhibitor. Principal component analysis (PCA) showed clustering of samples based on SM concentration at 5% level of significance and thus SM could be detected in milk using ATR-FTIR. The SM was best predicted in the range of 1472-1241cm(-1) using multiple linear regression with coefficient of determination (R(2)) of 0.99 and 0.92 for calibration and validation, respectively. PMID:25172681

  12. An attenuated total reflection (ATR) and Raman spectroscopic investigation into the effects of chloroquine on Plasmodium falciparum-infected red blood cells.

    PubMed

    Kozicki, M; Creek, D J; Sexton, A; Morahan, B J; Wesełucha-Birczyńska, A; Wood, B R

    2015-04-01

    Attenuated Total Reflection Fourier Transform Infrared (ATR-FTIR) and Raman spectroscopy were used to compare chloroquine (CQ)-treated and untreated cultured Plasmodium falciparum-infected human red blood cells (iRBCs). The studies were carried out in parallel from the same starting cultures using both spectroscopic techniques, in duplicate. ATR FTIR spectra showed modifications in the heme vibrational bands as well as increases in the CH2/CH3 stretching bands in the 3100-2800 cm(-1) region of CQ-treated iRBCs consistent with an increase in lipid content. Other changes consisted of secondary structural variations including shifts in the amide I and II modes, along with changes in RNA and carbohydrate bands. Raman microspectroscopy of single red blood cells using 532 nm revealed subtle changes in the positions and intensity of ν37 of the core size region marker band and ν4 in the pyrrole ring-stretching region between untreated and CQ-treated iRBCs. Similar patterns in the corresponding relations were also observed in the non-fundamental (overtone region) between the control and treated cells. These differences were consistent with higher levels of oxygenated hemoglobin (oxyHb) in the treated cells as shown in a Principle Component Analysis (PCA) loadings plot. The results obtained demonstrate that vibrational spectroscopic techniques can provide insight into the effect of quinolines on iRBCs and thus may assist understanding the sensitivity and resistance of new and existing anti-malarial drugs. PMID:25654140

  13. Adsorption of bovine serum albumin (BSA) onto lecithin studied by attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectroscopy.

    PubMed

    Tantipolphan, R; Rades, T; McQuillan, A J; Medlicott, N J

    2007-06-01

    The adsorption of bovine serum albumin (BSA) to lecithin was investigated by ATR-FTIR spectroscopy. Lecithin films were prepared by casting aliquots of 3.2 microg lecithin in methanol onto ZnSe ATR prisms. Surface morphology and the thickness of the films were investigated by laser scanning confocal electron microscopy and scanning electron microscopy and the thickness of the films used for adsorption studies was estimated to be 40 A. The dependency of the CO peak area on the lecithin mass in the calibration curve confirms that the thickness of the film is below the penetration depth of the infrared evanescent wave. Size exclusion HPLC and fluorescence spectroscopy show that BSA conformation in up to 1M NaCl and CaCl(2) solutions is similar to that in water with no aggregation or changes in protein conformation seen over 4h. The kinetics of BSA adsorption on the lecithin film from water, NaCl and CaCl(2) solutions demonstrates that ions promote the protein adsorption. BSA bound more in the presence of NaCl compared to CaCl(2) at equivalent concentrations. The adsorption appeared greatest at a 0.1M concentration for both NaCl and CaCl(2). The results are explained in terms of absorptive reactivity of BSA and lecithin surfaces upon salt addition. PMID:17240095

  14. Attenuated Total Reflection Mid-Infrared (ATR-MIR) Spectroscopy and Chemometrics for the Identification and Classification of Commercial Tannins.

    PubMed

    Ricci, Arianna; Parpinello, Giuseppina P; Olejar, Kenneth J; Kilmartin, Paul A; Versari, Andrea

    2015-11-01

    Attenuated total reflection Fourier transform infrared (FT-IR) spectroscopy was used to characterize 40 commercial tannins, including condensed and hydrolyzable chemical classes, provided as powder extracts from suppliers. Spectral data were processed to detect typical molecular vibrations of tannins bearing different chemical groups and of varying botanical origin (univariate qualitative analysis). The mid-infrared region between 4000 and 520 cm(-1) was analyzed, with a particular emphasis on the vibrational modes in the fingerprint region (1800-520 cm(-1)), which provide detailed information about skeletal structures and specific substituents. The region 1800-1500 cm(-1) contained signals due to hydrolyzable structures, while bands due to condensed tannins appeared at 1300-900 cm(-1) and exhibited specific hydroxylation patterns useful to elucidate the structure of the flavonoid monomeric units. The spectra were investigated further using principal component analysis for discriminative purposes, to enhance the ability of infrared spectroscopy in the classification and quality control of commercial dried extracts and to enhance their industrial exploitation. PMID:26647047

  15. Comparison between ATR-IR, Raman, concatenated ATR-IR and Raman spectroscopy for the determination of total antioxidant capacity and total phenolic content of Chinese rice wine.

    PubMed

    Wu, Zhengzong; Xu, Enbo; Long, Jie; Pan, Xiaowei; Xu, Xueming; Jin, Zhengyu; Jiao, Aiquan

    2016-03-01

    The application of attenuated total reflectance infrared spectroscopy (ATR-IR), Raman spectroscopy (RS) and combination of ATR-IR and RS for measurements of total antioxidant capacity (TAC) and total phenolic content (TPC) of Chinese rice wine (CRW) were investigated in this study. Synergy interval partial least-squares (SiPLS), support vector machine (SVM) and principal component analysis (PCA) were applied to process the merged data from two individual instruments. It was observed that the performances of models based on the RS spectra were better than those based on the ATR-IR spectra. In addition, SVM models based on the efficient information extracted from ATR-IR and RS spectra were superior to PLS models based on the same information and PLS models based on ATR-IR or RS spectra. The overall results demonstrated that integrating ATR-IR and RS was possible and could improve the prediction accuracy of TAC and TPC in CRWs. PMID:26471606

  16. Optimized data analysis algorithm for on-site chemical identification using a hand-held attenuated total reflection Fourier transform infrared (ATR FT-IR) spectrometer.

    PubMed

    Ron, Izhar; Zaltsman, Amalia; Kendler, Shai

    2013-12-01

    On-site identification of organic compounds in the presence of interfering materials using a field-portable attenuated total reflection Fourier transform infrared (ATR FT-IR) spectrometer is presented. Identification is based on an algorithm that compares the analyte's infrared absorption spectrum with the reference spectra. The comparison is performed at several predetermined frequencies, and a similarity value (distance) between the measured and the reference spectra is calculated either at each frequency individually, or, alternatively, the average distance for all frequencies is calculated. The examined frequencies are selected to give the best contrast between the target materials of interest. In this study, the algorithm was optimized to identify three common chemical warfare agents (CWAs): O-ethyl S-[2-(diisopropylamino)ethyl] methylphosphonothioic acid (VX), sarin (GB), and sulfur mustard (bis(2-chloroethyl) sulfide) (HD), in the presence of field-related interfering materials (fuels, water, and dust). Receiver operating characteristics analysis was performed in order to determine the probabilities for detection (PD) and for false alerts (PF). Challenging the algorithm with a set of data that contains mixtures of CWAs and interfering materials resulted in PD of 90% and PF of 0%, 0%, and 1% for VX, GB, and HD, respectively, using the average distance approach, which was found to be much more effective than analyzing each frequency individually. This finding was validated for all possible combinations of 2-7 peaks per material. It is suggested that this algorithm provides a reliable mean for the identification of a predetermined set of target analytes and interfering materials. PMID:24359653

  17. Identification of natural dyes on laboratory-dyed wool and ancient wool, silk, and cotton fibers using attenuated total reflection (ATR) Fourier transform infrared (FT-IR) spectroscopy and Fourier transform Raman spectroscopy.

    PubMed

    Bruni, Silvia; De Luca, Eleonora; Guglielmi, Vittoria; Pozzi, Federica

    2011-09-01

    Attenuated total reflection (ATR) infrared and Fourier transform (FT) Raman spectra were obtained from wool threads dyed in the laboratory with natural dyes used in antiquity, following a procedure similar to ancient methods for dyeing wool. The ATR spectra were primarily dominated by the signals of the wool, making it difficult to identify the dye on the fibers only by visual inspection of the infrared spectrum. However, the Raman spectra showed more significant characteristics attributable to the dyes as previously studied in the literature on modern synthetic dyes. A library-search method was thus applied to the second derivatives of both the ATR and Raman spectra to verify the possibility of identifying the dye. Two libraries were constructed, one consisting of the ATR spectra of undyed wool (raw, washed, and mordanted) and the transmission spectra of pure dyes and the other consisting of the Raman spectra of undyed wool and of pure dyes. Correlation and first-derivative correlation search algorithms were used. The results presented here suggest that the two types of spectroscopy are complementary in this kind of work, allowing the almost complete identification of historic dyes on wool. In fact, through the combined use of the two searches, most dyes were identified with a good index of similarity and within the first five hits. Only for annatto was identification totally impossible using either technique. Subsequently the same method was applied to wool, silk, and cotton threads taken from ancient Caucasian and Chinese textiles. PMID:21929856

  18. 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. PMID:26725502

  19. Self-assembling of oleic acid ( cis-9-octadecenoic acid) and linoleic acid ( cis-9, cis-12-octadecadienoic acid) in ethanol studied by time-dependent attenuated total reflectance (ATR) infrared (IR) and two-dimensional (2D) correlation spectroscopy

    NASA Astrophysics Data System (ADS)

    Pi, Fuwei; Shinzawa, Hideyuki; Czarnecki, Mirosław A.; Iwahashi, Makio; Suzuki, Masao; Ozaki, Yukihiro

    2010-06-01

    The dynamic behavior of liquid oleic and linoleic acids in ethanol has been explored by applying attenuated total reflectance (ATR) infrared (IR) spectroscopy. Fine spectral features are obtained with two-dimensional (2D) correlation spectroscopy. When the solution mixture was exposed to the open atmosphere, the complexes between the carboxylic acids and ethanol begin to dissociate and it starts the formation of dimers of the carboxylic acids. As the evaporation proceeds, the dimeric molecules undergo the self-assembling to form tightly packed quasi-smectic liquid crystal structure. The hetero-system 2D correlation spectra developed with two sets of time-dependent ATR-IR spectra of oleic and linoleic acids reveal that linoleic acid molecules aggregate faster as compared with oleic acid ones during the self-assembling mostly due to the difference in the number of the C dbnd C bonds.

  20. Applying Attenuated Total Reflection-Mid-Infrared (ATR-MIR) Spectroscopy to Detect Hairtail Surimi in Mixed Surimi and Their Surimi Products.

    PubMed

    You, Zhao-hong; Liu, Zi-hao; Gong, Chao-yong; Yang, Xiao-ling; Cheng, Fang

    2015-10-01

    ATR-MIR spectroscopic analysis was used to classify sliver carp surimi and surimi products adulterated with different levels of hairtail surimi. Five chemometric methods, including SIMCA (soft independent modeling class of analogies), KNN (K-nearest neighbor), SVR (support vector machines regression), PLSDA (partial least squares discriminate analysis) and ID3 (interative dicremiser version 3) Decision tree were used to build the classifying models. And the performances of the models were compared. Results showed that for both cooked and uncooked mixed surimi samples, better classifications were obtained using SIMCA model, the percentage of the correct classification reached 96.59% and 96.43%, and the corresponding RMSECV were 0.185 7 and 0.189 8, r value were 0.988 0 and 0.994 1 respectively. The results of this study demonstrated for the first time that ATR-MIR spectroscopy combined with chemometrics method can be used to classify sliver carp surimi and surimi products adulterated with different levels of hairtail surimi. PMID:26904846

  1. Effects of pH and metal ions on the conformation of bovine serum albumin in aqueous solution An attenuated total reflection (ATR) FTIR spectroscopic study

    NASA Astrophysics Data System (ADS)

    Qing, Huai; Yanlin, He; Fenlin, Sheng; Zuyi, Tao

    1996-11-01

    The Hummel-Dreyer gel permeation technique has been applied to investigate the binding of bovine serum albumin (BSA) with Zn 2+ and Cd 2+, and has provided evidence for the existence of two different types of binding sites in the BSA molecule. The effects of pH and the presence of metal ions Zn 2- and Cd 2+ on the conformation of BSA were investigated using ATR FTIR Spectroscopy. The results demonstrated that there were different conformational states in BSA at pH 5.0 and 9.0. Furthermore, we observed the spectral changes of BSA in the amide I region and major metal ion (Zn 2+ and Cd 2+) binding sites which were C?O and C?N groups of BSA.

  2. Quantitative evaluation by attenuated total reflectance infrared (ATR-FTIR) spectroscopy of the chemical composition of decayed wood preserved in waterlogged conditions.

    PubMed

    Pizzo, Benedetto; Pecoraro, Elisa; Alves, Ana; Macchioni, Nicola; Rodrigues, José Carlos

    2015-01-01

    This paper reports on the assessment of lignin and holocellulose by means of ATR-FTIR analysis and multivariate PLS regression. The analysis was conducted on 59 samples coming from different excavations where wood had been preserved in waterlogged conditions. A range of results from different wood species (Alnus sp.p., Cupressus sempervirens, Larix decidua, Picea abies, Pinus sp.p., Quercus sp.p., Ulmus sp.p.), states of preservation, waterlogged environments, and burial times are presented. A calibration model was selected after comparing different reference data (samples extracted and not-extracted, and ash-rich and ash-free bases of calculation for the calibration values), and two different post-acquisition spectroscopic manipulations (both in terms of normalisation procedures and of spectral ranges used for the calibration). Results showed that the best models were different depending on which considered component (lignin or holocellulose) was measured and to which data set (softwood or hardwood) the samples belonged. It is shown that the predictive ability of the models is affected by high ash content (too contaminated samples had to be excluded in order to attain good results, because of excessive overlapping of bands related to the inorganic fraction) but not by the preliminary extraction of sample. Furthermore, the stability of best models is also demonstrated and a procedure of external validation carried out on an external set of samples confirmed the general validity of the identified models. PMID:25281067

  3. Development and use of an attenuated total reflectance/fourier transform infrared (ATR/FT-IR) spectral database to identify foreign matter in cotton.

    PubMed

    Himmelsbach, David S; Hellgeth, John W; McAlister, David D

    2006-10-01

    The presence of foreign matter in cotton seriously affects the cotton grade and thus the price per bale paid by the spinner to the grower, the efficiency of the spinning and ginning operations, and the quality of the final woven product. Rapid identification of the nature of the extraneous matter in cotton at each stage of cleaning and processing is necessary to permit actions to eliminate or reduce its presence and improve efficiency and quality. Although several instruments are being successfully employed for the measurement of contamination in cotton fibers based on particle size/weight, no commercial instrument is capable of accurate qualitative identification of contaminants. To this end, ATR/FT-IR spectra of retrieved foreign matter were collected and subsequently rapidly matched to an authentic spectrum in a spectral database. The database includes contaminants typically classified as "trash", cotton plant parts (hull, shale, seed-coat fragments, bract, cacyx, leaf, bark, sticks, and stems) and grass plant parts (leaf and stem); "foreign objects and materials", synthetic materials (plastic bags, film, rubber, bale wrapping and strapping); organic materials (other fibers, yarns, paper, feathers, and leather); plus entomological and physiological sugars and inorganic materials (sand and rust). The spectral matching resulted in consistently high-score identification of the foreign matter based on chemical composition, irrespective of its particle size. The method is envisioned to be employed with stand-alone rugged infrared instrumentation to provide specific identification of extraneous materials in cotton as opposed to only general classification of the type by particle size or shape. PMID:17002401

  4. 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.

  5. Direct determination of sorbitol and sodium glutamate by attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR) in the thermostabilizer employed in the production of yellow-fever vaccine.

    PubMed

    de Castro, Eduardo da S G; Cassella, Ricardo J

    2016-05-15

    Reference methods for quality control of vaccines usually require treatment of the samples before analysis. These procedures are expensive, time-consuming, unhealthy and require careful manipulation of the sample, making them a potential source of analytical errors. This work proposes a novel method for the quality control of thermostabilizer samples of the yellow fever vaccine employing attenuated total reflectance Fourier transform infrared spectrometry (ATR-FTIR). The main advantage of the proposed method is the possibility of direct determination of the analytes (sodium glutamate and sorbitol) without any pretreatment of the samples. Operational parameters of the FTIR technique, such as the number of accumulated scans and nominal resolution, were evaluated. The best conditions for sodium glutamate were achieved when 64 scans were accumulated using a nominal resolution of 4cm(-1). The measurements for sodium glutamate were performed at 1347cm(-)(1) (baseline correction between 1322 and 1369cm(-1)). In the case of sorbitol, the measurements were done at 890cm(-1) (baseline correction between 825 and 910cm(-1)) using a nominal resolution of 2cm(-1) with 32 accumulated scans. In both cases, the quantitative variable was the band height. Recovery tests were performed in order to evaluate the accuracy of the method and recovery percentages in the range 93-106% were obtained. Also, the methods were compared with reference methods and no statistical differences were observed. The limits of detection and quantification for sodium glutamate were 0.20 and 0.62% (m/v), respectively, whereas for sorbitol they were 1 and 3.3% (m/v), respectively. PMID:26992492

  6. Structural effects of insulin-loading into HII mesophases monitored by electron paramagnetic resonance (EPR), small angle X-ray spectroscopy (SAXS), and attenuated total reflection Fourier transform spectroscopy (ATR-FTIR).

    PubMed

    Mishraki, Tehila; Ottaviani, Maria Francesca; Shames, Alexander I; Aserin, Abraham; Garti, Nissim

    2011-06-30

    Insulin entrapment within a monoolein-based reverse hexagonal (H(II)) mesophase was investigated under temperature-dependent conditions at acidic (pH 3) and basic (pH 8) conditions. Studying the structure of the host H(II) system and the interactions of insulin under temperature-dependent conditions has great impact on the enhancement of its thermal stabilization and controlled release for the purposes of transdermal delivery. Small angle X-ray spectroscopy (SAXS) measurements show that pH variation and/or insulin entrapment preserve the hexagonal structure and do not influence the lattice parameter. Attenuated total reflection Fourier transform spectroscopy (ATR-FTIR) spectra indicate that, although insulin interacts with hydroxyl groups of GMO in the interface region, it is not affected by pH variations. Hence different microenvironments within the H(II) mesophase were monitored by a computer-aided electron paramagnetic resonance (EPR) analysis using 5-doxylstearic acid (5-DSA) as a pH-dependent probe. The microviscosity, micropolarity, order of systems, and distribution of the probes in different microenvironments were influenced by three factors: temperature, pH, and insulin solubilization. When the temperature is increased, microviscosity and order parameters decreased at both pH 3 and 8, presenting different decrease trends. It was found that, at pH 3, the protein perturbs the lipid structure while "pushing aside" the un-ionized 5-DSA probe to fit into the narrow water cylinders. At the interface region (pH 8), the probe was distributed in two differently structured environments that significantly modifies by increasing temperature. Insulin loading within the H(II) mesophase decreased the order and microviscosity of both the microenvironments and increased their micropolarity. Finally, the EPR analysis also provides information about the unfolding/denaturation of insulin within the channel at high temperatures. PMID:21591776

  7. Attenuated total reflectance spectroscopy with chirped-pulse upconversion.

    PubMed

    Shirai, Hideto; Duchesne, Constance; Furutani, Yuji; Fuji, Takao

    2014-12-01

    Chirped-pulse upconversion technique has been applied to attenuated total reflectance (ATR) infrared spectroscopy. An extremely broadband infrared pulse was sent to an ATR diamond prism and the reflected pulse was converted to the visible by using four-wave mixing in krypton gas. Absorption spectra of liquids in the range from 200 to 5500 cm(-1) were measured with a visible spectrometer on a single-shot basis. The system was applied to observe the dynamics of exchanging process of two solvents, water and acetone, which give clear vibrational spectral contrast. We observed that the exchange was finished within ∼ 10 ms. PMID:25606893

  8. Infrared polarimetry using attenuated total reflection

    NASA Astrophysics Data System (ADS)

    Deibler, Lynn L.; Smith, Matthew H.

    1999-10-01

    Most organic materials are quite opaque to IR radiation, making it nearly impossible to measure the polarization properties at these wavelengths. By placing the highly absorbing organic material on a high index of refraction prism and making use of the evanescent field present at the interface for angles exceeding the critical angle, it is possible to measure the organic material's polarization characteristics. Attenuated Total Reflection (ATR) devices have been constructed in-house for use in our IR polarimeter operating over the spectral range of 3-14 microns. Single bounce internal reflection ZnSe prisms are used in our devices to measure the polarization characteristics of highly absorbing materials. Using attenuated total reflection along with a dual rotating retarder polarimeter, it is possible to determine the full Mueller Matrix, and thus determine the linear and circular diattenuation and retardance. With this information we can determine the complex index of refraction, dichroic ratio, and isotropic ratio of materials which are opaque in the IR region. With this knowledge of the material polarization properties, it may be possible to determine the orientation of the molecules in films made of long helical organic molecules and determine the enantiomeric purity of stereo-isomers. The theoretical performance of these devices with a focus on the organic chemical applications has been determined and compared with experiments. In this paper we present a summary of the theoretical basis for the measurements and make comparisons with our measurements.

  9. Nondestructive Determination of the Age of 20th-Century Oil-Binder Ink Prints Using Attenuated Total Reflection Fourier Transform Infrared Spectroscopy (ATR FT-IR): A Case Study with Postage Stamps from the Łódź Ghetto.

    PubMed

    Bower, Nathan W; Blanchet, Conor J K; Epstein, Michael S

    2016-01-01

    The ability to determine the production date for a painting or print would be of great benefit in the forensic detection of fakes and forgeries as well as in art history and conservation. Changes in the pigments used at different times have been invaluable in detecting incongruities that suggest fraud, but relatively little work has been published that uses the chemical changes in oil binders as they dry to determine when an ink print or an oil painting was made. Using attenuated total reflectance-Fourier transform infrared (ATR FT-IR) spectroscopy and samples with known dates, we calibrate the drying of oil binders in inks and paints and cross-validate the paints with pyrolysis-gas chromatography-mass spectrometry (Py-GC-MS). We apply the ink calibration to a case study involving the age determination of possible philatelic counterfeits from a World War II Jewish Ghetto in Occupied Poland, obtaining a date of 1946 ± 6 (1 s, n = 9) for the genuine stamps, and 1963 ± 16 (1 s, n = 19) for the various reproductions. PMID:26767642

  10. Terahertz time domain attenuated total reflection spectroscopy with an integrated prism system.

    PubMed

    Nakanishi, Atsushi; Kawada, Yoichi; Yasuda, Takashi; Akiyama, Koichiro; Takahashi, Hironori

    2012-03-01

    We demonstrated attenuated total reflection (ATR) spectroscopy with an integrated prism system that included a terahertz emitter, a terahertz receiver, and an ATR prism. The ATR prism had two internal off-axis parabolic mirrors for, respectively, collimating and focusing the terahertz waves. The Fresnel loss at each interface was reduced, and the total propagation efficiency was 3.36 times larger than when using a non-integrated prism system. The refractive index of water samples calculated from the experimental data showed good agreement with values reported in the literature. PMID:22462902

  11. Rapid determination of total trans fat content--an attenuated total reflection infrared spectroscopy international collaborative study.

    PubMed

    Mossoba, M M; Adam, M; Lee, T; Bastyr, J

    2001-01-01

    Interest in trans fat labeling has prompted efforts to develop new, more efficient methods for rapidly and accurately determining trans fat content of foods. A novel and rapid (5 min) attenuated total reflection-Fourier transform infrared (ATR-FTIR) spectroscopic procedure was recently developed and applied to food products. This procedure was voted official method AOCS Cd 14d-99 by the American Oil Chemists' Society in 1999 after testing in a 12 laboratory international collaborative study. The results of the study are described in this paper. Analytical ATR-FTIR results exhibited high accuracy in the range 5-40% trans; results tended to have <2% high bias relative to the gravimetrically determined values. The precision of this internal reflection method was found to be superior to the precision of transmission infrared official methods. It is recommended that the applicability of the ATR-FTIR method be limited to trans levels of >5% (as percent of total fat). PMID:11501916

  12. Surface-enhanced, multi-dimensional attenuated total reflectance spectroscopy

    NASA Astrophysics Data System (ADS)

    Kraack, Jan Philip; Lotti, Davide; Hamm, Peter

    2015-08-01

    Ultrafast two-dimensional infrared spectroscopy (2D IR) spectroscopy is performed in attenuated total reflectance (ATR) geometry with the Kretschmann configuration in order to measure femtosecond to picosecond dynamics of self-assembled monolayers on gold-coated solid-liquid interfaces. In the monolayers low-absorbing (<200 M-1 cm-1) nitrile functional groups are used as local vibrational probes to monitor vibrational relaxation and spectral diffusion in dependence of different environments of the nitrile group. By comparing spectral diffusion dynamics of the vibrational probe in bulk solution and in the monolayer we find that the dynamics are slowed down by more than a factor of 20 upon immobilization of the sample. Moreover, spectral diffusion dynamics are affected by the local environment within the monolayers as evidenced by 2D ATR IR experiments on mixed monolayers with different aliphatic and aromatic co-adsorbates. The results are interpreted in terms of absent excitation energy-transfer as well as solvation dynamics around the nitrile vibrational probe. Our results demonstrate that 2D ATR IR spectroscopy offers the possibility to obtain ultrafast dynamics from sub-monolayer coverages of even low-absorbing vibrational probes such as nitrile functional groups.

  13. Total sulfur determination in residues of crude oil distillation using FT-IR/ATR and variable selection methods

    NASA Astrophysics Data System (ADS)

    Müller, Aline Lima Hermes; Picoloto, Rochele Sogari; Mello, Paola de Azevedo; Ferrão, Marco Flores; dos Santos, Maria de Fátima Pereira; Guimarães, Regina Célia Lourenço; Müller, Edson Irineu; Flores, Erico Marlon Moraes

    2012-04-01

    Total sulfur concentration was determined in atmospheric residue (AR) and vacuum residue (VR) samples obtained from petroleum distillation process by Fourier transform infrared spectroscopy with attenuated total reflectance (FT-IR/ATR) in association with chemometric methods. Calibration and prediction set consisted of 40 and 20 samples, respectively. Calibration models were developed using two variable selection models: interval partial least squares (iPLS) and synergy interval partial least squares (siPLS). Different treatments and pre-processing steps were also evaluated for the development of models. The pre-treatment based on multiplicative scatter correction (MSC) and the mean centered data were selected for models construction. The use of siPLS as variable selection method provided a model with root mean square error of prediction (RMSEP) values significantly better than those obtained by PLS model using all variables. The best model was obtained using siPLS algorithm with spectra divided in 20 intervals and combinations of 3 intervals (911-824, 823-736 and 737-650 cm-1). This model produced a RMSECV of 400 mg kg-1 S and RMSEP of 420 mg kg-1 S, showing a correlation coefficient of 0.990.

  14. Attenuated total reflectance spectroscopy of plant leaves: A tool for ecological and botanical studies

    USGS Publications Warehouse

    Ribeiro da Luz, B.

    2006-01-01

    ??? Attenuated total reflectance (ATR) spectra of plant leaves display complex absorption features related to organic constituents of leaf surfaces. The spectra can be recorded rapidly, both in the field and in the laboratory, without special sample preparation. ??? This paper explores sources of ATR spectral variation in leaves, including compositional, positional and temporal variations. Interspecific variations are also examined, including the use of ATR spectra as a tool for species identification. ??? Positional spectral variations generally reflected the abundance of cutin and the epicuticular wax thickness and composition. For example, leaves exposed to full sunlight commonly showed more prominent cutin- and wax-related absorption features compared with shaded leaves. Adaxial vs. abaxial leaf surfaces displayed spectral variations reflecting differences in trichome abundance and wax composition. Mature vs. young leaves showed changes in absorption band position and intensity related to cutin, polysaccharide, and possibly amorphous silica development on and near the leaf surfaces. ??? Provided that similar samples are compared (e.g. adaxial surfaces of mature, sun-exposed leaves) same-species individuals display practically identical ATR spectra. Using spectral matching procedures to analyze an ATR database containing 117 individuals, including 32 different tree species, 83% of the individuals were correctly identified. ?? The Authors (2006).

  15. Attenuated total reflectance spectroscopy of plant leaves: a tool for ecological and botanical studies.

    PubMed

    da Luz, Beatriz Ribeiro

    2006-01-01

    Attenuated total reflectance (ATR) spectra of plant leaves display complex absorption features related to organic constituents of leaf surfaces. The spectra can be recorded rapidly, both in the field and in the laboratory, without special sample preparation. This paper explores sources of ATR spectral variation in leaves, including compositional, positional and temporal variations. Interspecific variations are also examined, including the use of ATR spectra as a tool for species identification. Positional spectral variations generally reflected the abundance of cutin and the epicuticular wax thickness and composition. For example, leaves exposed to full sunlight commonly showed more prominent cutin- and wax-related absorption features compared with shaded leaves. Adaxial vs. abaxial leaf surfaces displayed spectral variations reflecting differences in trichome abundance and wax composition. Mature vs. young leaves showed changes in absorption band position and intensity related to cutin, polysaccharide, and possibly amorphous silica development on and near the leaf surfaces. Provided that similar samples are compared (e.g. adaxial surfaces of mature, sun-exposed leaves) same-species individuals display practically identical ATR spectra. Using spectral matching procedures to analyze an ATR database containing 117 individuals, including 32 different tree species, 83% of the individuals were correctly identified. PMID:16995918

  16. Attenuated Total Reflection FTIR spectroscopy of Ultrathin Dielectrics Films

    NASA Astrophysics Data System (ADS)

    Liu, Ran

    2003-03-01

    Characterization of ultrathin dielectric films and surface layers becomes extremely crucial in the semiconductor industry. Although the standard transmission and reflection Fourier Transformed Infrared (FTIR) spectroscopy provides rich structural and chemical information, the lack of sensitivity in comparison with other surface techniques such as X-ray Photoelectron Spectroscopy (XPS) and Auger Electron Spectroscopy (AES) calls for application of new IR sampling technique for ultrathin layer analysis. This paper will demonstrate the powerfulness of Attenuated Total Reflection (ATR) as a unique FTIR probing method that is capable of analyzing dielectric films with thickness down to 1 nm. Examples will be given in areas of characterization of regular (SiO_2, SiON), low-k (SiOF), and high-k (HfO_2, HfSiO_x, SrTiO_3) films on Si.

  17. Analysis of thin-film polymers using attenuated total internal reflection-Raman microspectroscopy.

    PubMed

    Tran, Willie; Tisinger, Louis G; Lavalle, Luis E; Sommer, André J

    2015-01-01

    Two methods commonly employed for molecular surface analysis and thin-film analysis of microscopic areas are attenuated total reflection infrared (ATR-IR) microspectroscopy and confocal Raman microspectroscopy. In the former method, the depth of the evanescent probe beam can be controlled by the wavelength of light, the angle of incidence, or the refractive index of the internal reflection element. Because the penetration depth is proportional to the wavelength of light, one could interrogate a smaller film thickness by moving from the mid-infrared region to the visible region employing Raman spectroscopy. The investigation of ATR Raman microspectroscopy, a largely unexplored technique available to Raman microspectroscopy, was carried out. A Renishaw inVia Raman microscope was externally modified and used in conjunction with a solid immersion lens (SIL) to perform ATR Raman experiments. Thin-film polymer samples were analyzed to explore the theoretical sampling depth for experiments conducted without the SIL, with the SIL, and with the SIL using evanescent excitation. The feasibility of micro-ATR Raman was examined by collecting ATR spectra from films whose thickness measured from 200 to 60 nm. Films of these thicknesses were present on a much thicker substrate, and features from the underlying substrate did not become visible until the thin film reached a thickness of 68 nm. PMID:25587997

  18. Recent Developments in Solid-Phase Extraction for Near and Attenuated Total Reflection Infrared Spectroscopic Analysis.

    PubMed

    Huck, Christian W

    2016-01-01

    A review with more than 100 references on the principles and recent developments in the solid-phase extraction (SPE) prior and for in situ near and attenuated total reflection (ATR) infrared spectroscopic analysis is presented. New materials, chromatographic modalities, experimental setups and configurations are described. Their advantages for fast sample preparation for distinct classes of compounds containing different functional groups in order to enhance selectivity and sensitivity are discussed and compared. This is the first review highlighting both the fundamentals of SPE, near and ATR spectroscopy with a view to real sample applicability and routine analysis. Most of real sample analyses examples are found in environmental research, followed by food- and bioanalysis. In this contribution a comprehensive overview of the most potent SPE-NIR and SPE-ATR approaches is summarized and provided. PMID:27187347

  19. Quantification of bovine immunoglobulin G using transmission and attenuated total reflectance infrared spectroscopy.

    PubMed

    Elsohaby, Ibrahim; McClure, J Trenton; Riley, Christopher B; Shaw, R Anthony; Keefe, Gregory P

    2016-01-01

    In this study, we evaluated and compared the performance of transmission and attenuated total reflectance (ATR) infrared (IR) spectroscopic methods (in combination with quantification algorithms previously developed using partial least squares regression) for the rapid measurement of bovine serum immunoglobulin G (IgG) concentration, and detection of failure of transfer of passive immunity (FTPI) in dairy calves. Serum samples (n = 200) were collected from Holstein calves 1-11 days of age. Serum IgG concentrations were measured by the reference method of radial immunodiffusion (RID) assay, transmission IR (TIR) and ATR-IR spectroscopy-based assays. The mean IgG concentration measured by RID was 17.22 g/L (SD ±9.60). The mean IgG concentrations predicted by TIR and ATR-IR spectroscopy methods were 15.60 g/L (SD ±8.15) and 15.94 g/L (SD ±8.66), respectively. RID IgG concentrations were positively correlated with IgG levels predicted by TIR (r = 0.94) and ATR-IR (r = 0.92). The correlation between 2 IR spectroscopic methods was 0.94. Using an IgG concentration <10 g/L as the cut-point for FTPI cases, the overall agreement between TIR and ATR-IR methods was 94%, with a corresponding kappa value of 0.84. The sensitivity, specificity, positive predictive value, negative predictive value, and accuracy for identifying FTPI by TIR were 0.87, 0.97, 0.91, 0.95, and 0.94, respectively. Corresponding values for ATR-IR were 0.87, 0.95, 0.86, 0.95, and 0.93, respectively. Both TIR and ATR-IR spectroscopic approaches can be used for rapid quantification of IgG level in neonatal bovine serum and for diagnosis of FTPI in dairy calves. PMID:26699522

  20. Frustrated total internal reflection acoustic field sensor

    DOEpatents

    Kallman, Jeffrey S.

    2000-01-01

    A frustrated total internal reflection acoustic field sensor which allows the acquisition of the acoustic field over an entire plane, all at once. The sensor finds use in acoustic holography and acoustic diffraction tomography. For example, the sensor may be produced by a transparent plate with transparent support members tall enough to support one or more flexible membranes at an appropriate height for frustrated total internal reflection to occur. An acoustic wave causes the membrane to deflect away from its quiescent position and thus changes the amount of light that tunnels through the gap formed by the support members and into the membrane, and so changes the amount of light reflected by the membrane. The sensor(s) is illuminated by a uniform tight field, and the reflection from the sensor yields acoustic wave amplitude and phase information which can be picked up electronically or otherwise.

  1. Secondary cell wall development in cotton fibers as examined with attenuated total reflection Fourier transform infrared spectroscopy

    Technology Transfer Automated Retrieval System (TEKTRAN)

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

  2. Total internal reflection laser tools and methods

    DOEpatents

    Zediker, Mark S.; Faircloth, Brian O.; Kolachalam, Sharath K.; Grubb, Daryl L.

    2016-02-02

    There is provided high power laser tools and laser heads that utilize total internal reflection ("TIR") structures to direct the laser beam along a laser beam path within the TIR structure. The TIR structures may be a TIR prism having its hypotenuse as a TIR surface.

  3. Attenuated total reflectance-FT-IR imaging for rapid and automated detection of gunshot residue.

    PubMed

    Bueno, Justin; Lednev, Igor K

    2014-04-01

    An alternative approach for the nondestructive, rapid and selective detection of gunshot residue (GSR) was investigated. A cloth substrate containing GSR particles expelled during a firearm discharge was used as an analog for the clothing of a shooting victim or a suspect discharging a firearm. An established and efficient procedure for GSR collection (tape lifting) was utilized to recover GSR particles from the cloth substrate. Microscopic-attenuated total reflectance (ATR) Fourier transform (FT) infrared (IR) spectroscopic imaging rapidly and automatically scanned large areas of the tape collection substrate and detected varying morphologies (microscopic and macroscopic) and chemical compositions (organic and inorganic) of GSR. The "spectroscopic fingerprint" of each GSR type provided unique virbrational modes, which were not characteristic of the tape collection substrate or the cloth debris which was also recovered. ATR images (maps) targeted the detection of these unique chemical markers over the mapped area. The hues of the ATR images were determined by the intensity of the signal for the chemical marker of each analyte. The spatial resolution of the technique was determined to be 4.7 ?m. Therefore, all GSR particles sized 4.7 ?m or larger will be resolved and detected on the tape substrate using micro-ATR imaging. PMID:24588255

  4. Total Internal Reflection Fluorescence (TIRF) Microscopy

    PubMed Central

    Fish, Kenneth N.

    2015-01-01

    Total internal reflection fluorescence (TIRF) microscopy (TIRFM) is an elegant optical technique that provides for the excitation of fluorophores in an extremely thin axial region (‘optical section’). The method is based on the principle that when excitation light is totally internally reflected in a transparent solid (e.g., coverglass) at its interface with liquid an electromagnetic field, called the evanescent wave, is generated in the liquid at the solid-liquid interface and is the same frequency as the excitation light. Since the intensity of the evanescent wave exponentially decays with distance from the surface of the solid, only fluorescent molecules within a few hundred nanometers of the solid are efficiently excited. This unit will briefly review the history, optical theory, and the different hardware configurations used in TIRFM. In addition, it will provide experimental details and methodological considerations for studying receptors at the plasma membrane in neurons. PMID:19816922

  5. Micro- and macro-attenuated total reflection Fourier transform infrared spectroscopic imaging. Plenary Lecture at the 5th International Conference on Advanced Vibrational Spectroscopy, 2009, Melbourne, Australia.

    PubMed

    Kazarian, Sergei G; Chan, K L Andrew

    2010-05-01

    Fourier transform infrared (FT-IR) spectroscopic imaging has become a very powerful method in chemical analysis. In this review paper we describe a variety of opportunities for obtaining FT-IR images using the attenuated total reflection (ATR) approach and provide an overview of fundamental aspects, accessories, and applications in both micro- and macro-ATR imaging modes. The advantages and versatility of both ATR imaging modes are discussed and the spatial resolution of micro-ATR imaging is demonstrated. Micro-ATR imaging has opened up many new areas of study that were previously precluded by inadequate spatial resolution (polymer blends, pharmaceutical tablets, cross-sections of blood vessels or hair, surface of skin, single live cells, cancerous tissues). Recent applications of ATR imaging in polymer research, biomedical and forensic sciences, objects of cultural heritage, and other complex materials are outlined. The latest advances include obtaining spatially resolved chemical images from different depths within a sample, and surface-enhanced images for macro-ATR imaging have also been presented. Macro-ATR imaging is a valuable approach for high-throughput analysis of materials under controlled environments. Opportunities exist for chemical imaging of dynamic aqueous systems, such as dissolution, diffusion, microfluidics, or imaging of dynamic processes in live cells. PMID:20482963

  6. [Application of Fourier transform attenuated total reflection infrared spectroscopy in analysis of pulp and paper industry].

    PubMed

    Zhang, Yong; Cao, Chun-yu; Feng, Wen-ying; Xu, Ming; Su, Zhen-hua; Liu, Xiao-meng; Lü, Wei-jun

    2011-03-01

    As one of the most powerful tools to investigate the compositions of raw materials and the property of pulp and paper, infrared spectroscopy has played an important role in pulp and paper industry. However, the traditional transmission infrared spectroscopy has not met the requirements of the producing processes because of its disadvantages of time consuming and sample destruction. New technique would be needed to be found. Fourier transform attenuated total reflection infrared spectroscopy (ATR-FTIR) is an advanced spectroscopic tool for nondestructive evaluation and could rapidly, accurately estimate the production properties of each process in pulp and paper industry. The present review describes the application of ATR-FTIR in analysis of pulp and paper industry. The analysis processes will include: pulping, papermaking, environmental protecting, special processing and paper identifying. PMID:21595211

  7. Raman scattering and attenuated-total-reflection studies of surface-plasmon polaritons

    SciTech Connect

    Kurosawa, K.; Pierce, R.M.; Ushioda, S.; Hemminger, J.C.

    1986-01-15

    We have made in situ measurements of attenuated total reflection (ATR) and Raman scattering from a layered structure consisting of a glass prism, a thin silver film, an MgF2 spacer, and a liquid mixture whose refractive index is matched to that of MgF2. When the incident angle of the laser beam coincides with the ATR angle, the surface-plasmon polariton (SPP) of the silver film is excited resonantly and the Raman scattering intensity of the liquid shows a maximum. The same effect is observed at the frequency of the Stokes scattered light. By measuring the decrease of the Raman scattering intensity of the liquid with increase of the thickness of the MgF2 spacer layer, we have determined the decay length (l/sub d/) of the SPP field into the liquid. The measured value of l/sub d/ = 1539 A agrees with the calculated value, 1534 A.

  8. Infrared Attenuated Total Reflectance Spectroscopy: An Innovative Strategy for Analyzing Mineral Components in Energy Relevant Systems

    PubMed Central

    Müller, Christian Menno; Pejcic, Bobby; Esteban, Lionel; Piane, Claudio Delle; Raven, Mark; Mizaikoff, Boris

    2014-01-01

    The direct qualitative and quantitative determination of mineral components in shale rocks is a problem that has not been satisfactorily resolved to date. Infrared spectroscopy (IR) is a non-destructive method frequently used in mineral identification, yet challenging due to the similarity of spectral features resulting from quartz, clay, and feldspar minerals. This study reports on a significant improvement of this methodology by combining infrared attenuated total reflection spectroscopy (IR-ATR) with partial least squares (PLS) regression techniques for classifying and quantifying various mineral components present in a number of different shale rocks. The developed multivariate classification model was calibrated using pure component mixtures of the most common shale minerals (i.e., kaolinite, illite, montmorillonite, calcite, and quartz). Using this model, the IR spectra of 11 real-world shale samples were analyzed and evaluated. Finally, the performance of the developed IR-ATR method was compared with results obtained via X-ray diffraction (XRD) analysis. PMID:25358261

  9. Potential Modulation on Total Internal Reflection Ellipsometry.

    PubMed

    Liu, Wei; Niu, Yu; Viana, A S; Correia, Jorge P; Jin, Gang

    2016-03-15

    Electrochemical-total internal reflection ellipsometry (EC-TIRE) has been proposed as a technique to observe the redox reactions on the electrode surface due to its high phase sensitivity to the electrolyte/electrode interface. In this paper, we mainly focus on the influence of the potential modulation on the TIRE response. The analysis suggests that both dielectric constant variation of gold and the electric double layer transformation would modulate the reflection polarization of the surface. For a nonfaradaic process, the signal of TIRE would be proportional to the potential modulation. To testify the analysis, linear sweep voltammetry and open circuit measurement have been performed. The results strongly support the system analysis. PMID:26889871

  10. Attenuated total reflectance spectroscopy of simultaneous processes: Corrosion inhibition of cuprous oxide by benzotriazole

    NASA Astrophysics Data System (ADS)

    Bratescu, Maria Antoaneta; Allred, Daniel B.; Saito, Nagahiro; Sarikaya, Mehmet; Takai, Osamu

    2008-03-01

    Attenuated total reflectance (ATR) spectroscopy was used to perform in situ studies of the corrosion inhibition of cuprous oxide (Cu 2O) by benzotriazole (BTA) in aqueous solution at concentrations from 1 to 20 μM. Because two separate processes occur simultaneously, that of Cu 2O corrosion and corrosion inhibition by BTA adsorption, the spectral information was subjected to deconvolution by a conjugate gradient minimization algorithm. Under these conditions, a solution phase concentration of 7-10 μM BTA nearly completely inhibited the corrosion of Cu 2O in deionized water. Using a Langmuir adsorption model, this represented only 25% of the maximally covered surface area.

  11. Atomic Scale Flatness of Chemically Cleaned Silicon Surfaces Studied by Infrared Attenuated-Total-Reflection Spectroscopy

    NASA Astrophysics Data System (ADS)

    Sawara, Kenichi; Yasaka, Tatsuhiro; Miyazaki, Seiichi; Hirose, Masataka

    1992-07-01

    Hydrogen-terminated Si(111) and Si(100) surfaces obtained by aqueous HF or pH-modified (pH{=}5.3) buffered-HF (BHF) treatments have been characterized by a Fourier transform infrared (FT-IR) attenuated-total-reflection (ATR) technique. The BHF treatment provides better surface flatness than the HF treatment. Pure water rinse is effective for improving the Si(111) surface flatness, while this is not the case for Si(100) because the pure water acts as an alkaline etchant and promotes the formation of (111) microfacets or microdefects on the (100) surface.

  12. Preliminary Method for Direct Quantification of Colistin Methanesulfonate by Attenuated Total Reflectance Fourier Transform Infrared Spectroscopy

    PubMed Central

    Niece, Krista L.

    2015-01-01

    Colistin use has increased in response to the advent of infections caused by multidrug-resistant organisms. It is administered parenterally as an inactive prodrug, colistin methanesulfonate (CMS). Various formulations of CMS and labeling conventions can lead to confusion about colistin dosing, and questions remain about the pharmacokinetics of CMS. Since CMS does not have strong UV absorbance, current methods employ a laborious process of chemical conversion to colistin followed by precolumn derivatization to detect formed colistin by high-performance liquid chromatography. Here, we report a method for direct quantification of colistin methanesulfonate by attenuated total reflectance Fourier transform infrared spectroscopy (ATR FTIR). PMID:26124160

  13. Attenuated total reflection design for in situ FT-IR spectroelectrochemical studies

    SciTech Connect

    Visser, Hendrik; Curtright, Aimee E.; McCusker, James K.; Sauer, Kenneth

    2000-11-10

    A versatile spectroelectrochemical apparatus is introduced to study the changes in IR spectra of organic and inorganic compounds upon oxidation or reduction. The design is based on an attenuated total reflection (ATR) device, which permits the study of a wide spectral range of 16,700 cm-1 (600 nm) - 250 cm-1 with a small opaque region of 2250 - 1900 cm-1. In addition, an IR data collection protocol is introduced to deal with electrochemically non-reversible background signals. This method is tested with ferrocene in acetonitrile, producing results that agree with those in the literature.

  14. Frustrated total internal reflection of laser eigenstates

    SciTech Connect

    Balcou, P.; Dutriaux, L.; Bretenaker, F.; Le Floch, A.

    1996-07-01

    The role of frustrated total internal reflection in the dynamics of laser eigenstates is investigated theoretically and experimentally. We first derive the Jones matrix of a frustrating element for a realistic Gaussian beam in a single-pass geometry. We point out the existence of three different angular regimes, namely, a pure frustration regime, an intermediate regime, and a quasi-Fabry{endash}Perot regime. We then explore in each case the nature and the competition between the laser polarization eigenstates. A novel spiraling behavior of the laser parameters is demonstrated when the frustrating gap is varied, along with puzzling polarization-flipping effects, that may modify strongly the conditions that optimize the laser-output power. Experimental results agree with a theoretical model. {copyright} {ital 1996 Optical Society of America.}

  15. Development of an ultra-compact mid-infrared attenuated total reflectance spectrophotometer

    NASA Astrophysics Data System (ADS)

    Kim, Dong Soo; Lee, Tae-Ro; Yoon, Gilwon

    2014-07-01

    Mid-infrared spectroscopy has been an important tool widely used for qualitative analysis in various fields. However, portable or personal use is size and cost prohibitive for either Fourier transform infrared or attenuated total reflectance (ATR) spectrophotometers. In this study, we developed an ultra-compact ATR spectrophotometer whose frequency band was 5.5-11.0 μm. We used miniature components, such as a light source fabricated by semiconductor technology, a linear variable filter, and a pyro-electric array detector. There were no moving parts. Optimal design based on two light sources, a zippered configuration of the array detector and ATR optics could produce absorption spectra that might be used for qualitative analysis. A microprocessor synchronized the pulsed light sources and detector, and all the signals were processed digitally. The size was 13.5×8.5×3.5 cm3 and the weight was 300 grams. Due to its low cost, our spectrophotometer can replace many online monitoring devices. Another application could be for a u-healthcare system installed in the bathroom or attached to a smartphone for monitoring substances in body fluids.

  16. Far- and Deep-UV Spectroscopy of Semiconductor Nanoparticles Measured Based on Attenuated Total Reflectance spectroscopy.

    PubMed

    Tanabe, Ichiro; Yamada, Yosuke; Ozaki, Yukihiro

    2016-02-01

    Far- and deep-ultraviolet spectra (150-300 nm) of semiconductor nanoparticles (zinc oxide and zinc sulfide) are successfully measured by using attenuated total reflectance (ATR) spectroscopy, and analyzed using finite-difference time-domain (FDTD) simulations. The obtained spectra show good consistency with earlier synchrotron-radiation spectra and with theoretical calculations. The FDTD simulation results show that the present system collected the correct spectra. In the present system, the obtained spectra are affected by the real part n of the complex refractive index more strongly than the imaginary part k. It is also revealed both experimentally and theoretically that spectral intensities of the semiconductor nanoparticles are approximately one tenth those of liquid samples. These results provide insights into the far- and deep-ultraviolet spectroscopy based on the ATR system, and show the general applicability of our original ATR spectroscopy to semiconductor nanoparticles. The system needs neither high vacuum nor much space, and enables rapid and systematic investigation of the electronic states of various materials. PMID:26691240

  17. Detection of sibutramine in adulterated dietary supplements using attenuated total reflectance-infrared spectroscopy.

    PubMed

    Deconinck, E; Cauwenbergh, T; Bothy, J L; Custers, D; Courselle, P; De Beer, J O

    2014-11-01

    Sibutramine is one of the most occurring adulterants encountered in dietary supplements with slimming as indication. These adulterated dietary supplements often contain a herbal matrix. When customs intercept these kind of supplements it is almost impossible to discriminate between the legal products and the adulterated ones, due to misleading packaging. Therefore in most cases these products are confiscated and send to laboratories for analysis. This results inherently in the confiscation of legal, non-adulterated products. Therefore there is a need for easy to use equipment and techniques to perform an initial screening of samples. Attenuated total reflectance-infrared (ATR-IR) spectroscopy was evaluated for the detection of sibutramine in adulterated dietary supplements. Data interpretation was performed using different basic chemometric techniques. It was found that the use of ATR-IR combined with the k-Nearest Neighbours (k-NN) was able to detect all adulterated dietary supplements in an external test set and this with a minimum of false positive results. This means that a small amount of legal products will still be confiscated and analyzed in a laboratory to be found negative, but no adulterated samples will pass the initial ATR-IR screening. PMID:25173110

  18. ATR-FTIR Spectroscopy in the Undergraduate Chemistry Laboratory: Part I--Fundamentals and Examples

    ERIC Educational Resources Information Center

    Schuttlefield, Jennifer D.; Grassian, Vicki H.

    2008-01-01

    Attenuated total reflectance-Fourier transform infrared (ATR-FTIR) spectroscopy is a useful technique for measuring the infrared spectra of solids and liquids as well as probing adsorption on particle surfaces. Several examples of the use of FTIR-ATR spectroscopy in different undergraduate chemistry laboratory courses are presented here. These

  19. ATR-FTIR Spectroscopy in the Undergraduate Chemistry Laboratory: Part I--Fundamentals and Examples

    ERIC Educational Resources Information Center

    Schuttlefield, Jennifer D.; Grassian, Vicki H.

    2008-01-01

    Attenuated total reflectance-Fourier transform infrared (ATR-FTIR) spectroscopy is a useful technique for measuring the infrared spectra of solids and liquids as well as probing adsorption on particle surfaces. Several examples of the use of FTIR-ATR spectroscopy in different undergraduate chemistry laboratory courses are presented here. These…

  20. Prisms with total internal reflection as solar reflectors

    DOEpatents

    Rabl, Arnulf; Rabl, Veronika

    1978-01-01

    An improved reflective wall for radiant energy collection and concentration devices is provided. The wall is comprised of a plurality of prisms whose frontal faces are adjacent and which reflect the desired radiation by total internal reflection.

  1. Surface-Active Lipid Linings under Shear Load--A Combined in-Situ Neutron Reflectivity and ATR-FTIR Study.

    PubMed

    Schwörer, Felicitas; Trapp, Marcus; Ballauff, Matthias; Dahint, Reiner; Steitz, Roland

    2015-10-27

    We study shear effects in solid-supported lipid membrane stacks by simultaneous combined in-situ neutron reflectivity (NR) and attenuated total reflection Fourier transform infrared spectroscopy (ATR-FTIR). The stacks mimic the terminal surface-active phospholipid (SAPL) coatings on cartilage in mammalian joints. Piles of 11 bilayer membranes of 1,2-dimyristoyl-sn-glycero-3-phosphocholine (DMPC) are immobilized at the interface of the solid silicon support and the liquid D2O backing phase. We replace the natural hyaluronic acid (HA) component of synovial fluid by a synthetic substitute, namely, poly(allylamine hydrochloride) (PAH), at identical concentration. We find the oligolamellar DMPC bilayer films strongly interacting with PAH resulting in a drastic increase of the membranes d spacing (by a factor of ∼5). Onset of shear causes a buckling-like deformation of the DMPC bilayers perpendicular to the applied shear field. With increasing shear rate we observe substantially enhanced water fractions in the membrane slabs which we attribute to increasing fragmentation caused by Kelvin-Helmholtz-like instabilities parallel to the applied shear field. Both effects are in line with recent theoretical predictions on shear-induced instabilities of lipid bilayer membranes in water (Hanasaki, I.; Walther, J. H.; Kawano, S.; Koumoutsakos, P. Phys. Rev. E 2010, 82, 051602). With the applied shear the interfacial lipid linings transform from their gel state Pβ' to their fluid state Lα. Although in chain-molten state with reduced bending rigidity the lipid layers do not detach from their solid support. We hold steric bridging of the fragmented lipid bilayer membranes by PAH molecules responsible for the unexpected mechanical stability of the DMPC linings. PMID:26388226

  2. Detection of Citrus Huanglongbing by Fourier Transform Infrared-Attenuated Total Reflection (FTIR-ATR) Spectroscopy

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Citrus Huanglongbing (HLB, also known as citrus greening disease) was discovered in Florida in 2005 and is spreading rapidly amongst the citrus growing regions of the state. Detection via visual symptoms of the disease is not a long term viable option. New techniques are being developed to test fo...

  3. Application of attenuated total reflectance Fourier transform infrared spectroscopy in the mineralogical study of a landslide area, Hungary

    NASA Astrophysics Data System (ADS)

    Udvardi, Beatrix; Kovács, István János; Kónya, Péter; Földvári, Mária; Füri, Judit; Budai, Ferenc; Falus, György; Fancsik, Tamás; Szabó, Csaba; Szalai, Zoltán; Mihály, Judith

    2014-11-01

    This study demonstrates that the unpolarized attenuated total reflectance Fourier transform infrared spectroscopy (ATR FTIR) is a practical and quick tool to distinguish different types of sediments in landslide-affected areas, and potentially other types of physical environments too. Identification and quantification of minerals by ATR FTIR is implemented on a set of powdered natural sediments from a loess landslide (Kulcs, Hungary). A protocol including sample preparation, analytical conditions and evaluation of sediment ATR spectra is outlined in order to identify and estimate major minerals in sediments. The comparison of the defined FTIR parameters against qualitative and quantitative results of X-ray diffraction and thermal analysis was used to validate the use of ATR FTIR spectroscopy for the considered sediments. The infrared band areas and their ratios (water/carbonates; silicates/carbonates; kaolinite) appear to be the most sensitive parameters to identify strongly weathered sediments such as paleosols and red clays which most likely facilitate sliding and could form sliding zones. The effect of grain size and orientation of anisotropic minerals on the wave number and intensity of some major absorption bands is also discussed.

  4. Attenuated total internal reflectance infrared microspectroscopy as a detection technique for capillary electrophoresis.

    PubMed

    Patterson, Brian M; Danielson, Neil D; Sommer, André J

    2004-07-01

    A novel detector for capillary electrophoresis (CE) using single-bounce attenuated total internal reflectance (ATR) Fourier transform infrared (FT-IR) microspectroscopy is presented. The terminus of the CE capillary is placed approximately 1 microm from the internal reflectance crystal at the focus of an ATR infrared microscope. Using pressure driven flow injection, concentration and volume detection limits have been determined for 25- and 10-microm-i.d. silica capillaries. Upon injection of 820 pL of succinylcholine chloride in a 10-microm capillary, a concentration detection limit of approximately 0.5 parts per thousand (ppt), or 410 pg, is found. The injection volume detection limit using a 108 ppt solution is 2.0 pL (216 pg). Sample separations using a programmed series of pressure, voltage, and again pressure on 25-, 50-, and 75-microm-i.d. capillaries are shown. CE separations of citrate and nitrate, as well as succinylcholine chloride with sodium salicylate using acetone as a neutral marker, are demonstrated. Several advantages of this CE-FT-IR technique include: (1) minimization of postcolumn broadening as a result of a small detector volume; (2) the ability to signal average spectra of the same aliquot, thereby improving the signal-to-noise in a stopped-flow environment; and (3) simplicity of design. PMID:15228361

  5. Attenuated total reflection micro FTIR characterisation of pigment-binder interaction in reconstructed paint films.

    PubMed

    Mazzeo, R; Prati, S; Quaranta, M; Joseph, E; Kendix, E; Galeotti, M

    2008-09-01

    The interaction of pigments and binding media may result in the production of metal soaps on the surface of paintings which modifies their visible appearance and state of conservation. To characterise more fully the metal soaps found on paintings, several historically accurate oil and egg yolk tempera paint reconstructions made with different pigments and naturally aged for 10 years were submitted to attenuated total reflectance Fourier transform infrared (ATR FTIR) microspectroscopic analyses. Standard metal palmitates were synthesised and their ATR spectra recorded in order to help the identification of metal soaps. Among the different lead-based pigments, red lead and litharge seemed to produce a larger amount of carboxylates compared with lead white, Naples yellow and lead tin yellow paints. Oil and egg tempera litharge and red lead paints appeared to be degraded into lead carbonate, a phenomenon which has been observed for the first time. The formation of metal soaps was confirmed on both oil and egg tempera paints based on zinc, manganese and copper and in particular on azurite paints. ATR mapping analyses showed how the areas where copper carboxylates were present coincided with those in which azurite was converted into malachite. Furthermore, the key role played by manganese in the production of metals soaps on burnt and raw sienna and burnt and raw umber paints has been observed for the first time. The formation of copper, lead, manganese, cadmium and zinc metal soaps was also identified on egg tempera paint reconstructions even though, in this case, the overlapping of the spectral region of the amide II band with that of metal carboxylates made their identification difficult. PMID:18454281

  6. Metallic attenuated total reflection infrared hollow fibers for robust optical transmission systems

    SciTech Connect

    Jing, Chengbin; Guo, Hong; Hu, Zhigao; Yang, Pingxiong; Chu, Junhao; Liu, Aiyun; Shi, Yiwei

    2014-07-07

    A durable metallic attenuated total reflection (ATR) hollow fiber (bore size: 1.45 mm, wall thickness: 50 μm) was designed and fabricated based on a nickel capillary tube and hexagonal germanium dioxide (GeO{sub 2}). The anomalous dispersion of the hexagonal GeO{sub 2} layer grown inside a nickel tube achieves low-loss light transmission at two peak-power wavelengths for CO{sub 2} laser devices (10.2 and 10.6 μm). An 11–28 W, 10.2 or 10.6 μm CO{sub 2} laser power was steadily delivered via a fiber elastically bent from 0° to 90° (radius: 45 cm) for over 40 min (transmission loss: 0.22 to 4.2 dB/m). Theoretically fitting the measured temperatures showed that front-end clipping caused greater thermal loading than the distributed mode absorption. The maximum external temperature of a nickel ATR fiber is much lower than that of a silica glass ATR fiber owing to their different heat dissipation abilities. The HE{sub 11} mode purity of the output beam profiles decreased from 90.3% to 44.7% as the bending angle increased from 0° to 90°. Large core sizes and wall roughnesses (scattering loss 0.04 dB/m) contributed to mode mixing and excess losses that were above the value predicted by the classical Marcatili and Schmeltzer equation (0.024–0.037 dB/m).

  7. Development of a time-resolved attenuated total reflectance spectrometer in far-ultraviolet region.

    PubMed

    Morisawa, Yusuke; Higashi, Noboru; Takaba, Kyoko; Kariyama, Naomi; Goto, Takeyoshi; Ikehata, Akifumi; Ozaki, Yukihiro

    2012-07-01

    A far-ultraviolet transient absorption spectrometer based on time-resolved attenuated total reflectance (ATR) has been developed and tested for aqueous solutions of phenol and tryptophan in the region 170-185 nm. In this region, a stable tunable laser was not available, and therefore, white light from a laser-driven Xe lamp source was used. The time resolution, which was determined by the time response of a continuous light detector, was 40 ns. A new ATR cell where a sample liquid is exchanged continuously by a flow system was designed to reduce efficiently the stray light from the excitation light. We have tested the performance of the instrument by using aqueous solutions of phenol and tryptophan, whose photochemistry is already well known. Phenol and tryptophan have very strong absorptions due to a ?-?? transition near 180 nm. Even for dilute solutions (10(-3) mol dm(-3)), we could observe decreases in their concentrations due to photochemistry that occurred upon their irradiation with a fourth harmonic generation laser pulse produced by an Nd:YAG laser. The sensitivity of the spectrometer was about 10(-4) abs, which corresponded to a concentration variation of 10(-3) mol dm(-3) for phenol and tryptophan. PMID:22852667

  8. Evaluation of drug crystallinity in aqueous suspension using terahertz time-domain attenuated total reflection spectroscopy.

    PubMed

    Takebe, Gen; Kawada, Yoichi; Akiyama, Koichiro; Takahashi, Hironori; Takamoto, Hisayoshi; Hiramatsu, Mitsuo

    2013-11-01

    Terahertz pulsed spectroscopy has recently been demonstrated to be a novel technique for the investigation of the solid-state properties of pharmaceutical materials. In this study, we directly measured the crystallinity of a drug suspended in water, using a terahertz pulsed attenuated total reflection (ATR) method. The dihydropyridine calcium channel blocker nifedipine is classified as a poorly soluble drug; its most stable crystalline form is known as form I. Transmission spectra, collected from 0.2 to 2.0 THz (6.6 to 66 cm(-1) ), of nifedipine crystals had a strong absorption peak at 1.2 THz (40 cm(-1) ) at room temperature. When the nifedipine crystals were mixed with poloxamer 188 and suspended in water, the resulting spectra measured using the ATR method had a peak at the same frequency as in the spectra obtained in transmission mode. Furthermore, the peak area was proportional to the amount of crystals. The upward sloping baseline in the spectra, corresponding to water absorption, decreased stepwise with increasing amounts of crystalline particles. We confirmed that the spectra gave excellent quantitative results, using partial least-squares regression analysis. The results suggest the possibility of using this method for qualitative and quantitative assessments of crystalline drugs in suspension. PMID:24037861

  9. [Attenuated Total Reflection Infrared Spectroscopy for Degradation Profile of High Density Polyethylene after Weathering Aging].

    PubMed

    Guo, Jun-jun; Yan, Hua; Bao, He-bin; Wang, Xue-mei; Hu, Zhi-de; Yang, Jian-jian

    2015-06-01

    High density polyethylene (HDPE) was widely used as rotational packaging case in the material reserve field. The chemical changes of HDPE, exposed to particular climatic conditions of tropic marine atmosphere for one year-long in Wanning Hainan, were elucidated by the attenuated total reflection infrared spectroscopy (ATR-FTIR). The structural changes were studied qualitatively, mainly from the polymeric chain breaking, branching and oxidation to distinguish the degradation profile. The variations of crystallinity & carbonyl index were also studied quantitatively according to the characteristic peaks intensity & area ratio. Finally, the relationships between structural changes and mechanical properties were investigated. The results showed that the polymeric chain breaking & branching play a leading role before 3 months in the aging progress. Then oxidation phenomena gradually takes place during 3-6 months. The chain branching & oxidation were predominant factors after 6 months. Nine months later, the oxidation was saturated gradually. Furthermore, the aging process is positively correlated to the temperature and irradiation. After 12 months aging, the carbonyl index increased by 112 times and crystallinity was 10% higher than before. The tensile/bending modulus deceased faster than tensile/bending strength of HDPE. The linear degree of tensile modulus and carbonyl index was 0.97. The degree of linearity of tensile strength and crystallinity calculated by feature bands (720-730 cm(-1)) was 0.96. It showed that the mechanical properties of HDPE can be speculated from the structural changes by ATR-FTIR. PMID:26601359

  10. Attenuated total reflectance Fourier-transform infrared spectroscopic investigation of silicon heterojunction solar cells.

    PubMed

    Holovský, Jakub; De Wolf, Stefaan; Jiříček, Petr; Ballif, Christophe

    2015-07-01

    Silicon heterojunction solar cells critically depend on the detailed properties of their amorphous/crystalline silicon interfaces. We report here on the use of attenuated total reflectance Fourier-transform infrared (ATR-FTIR) spectroscopy to gain precise insight into the vibrational properties of the surfaces and ultrathin layers present in such solar cells. We fabricate ATR prisms from standard silicon wafers similar to those used for device fabrication. In this fashion, we acquire very-high sensitivity FTIR information on device-relevant structures. Our method has no requirement for minimum layer thickness, enabling the study of the impact of the different fabrication process steps on the film microstructure. We discuss the necessary requirements for the method implementation and give a comprehensive overview of all observed vibration modes. In particular, we study vibrational signatures of Si-H(X), Si-H(X)(Si(Y)O(Z)), B-H, hydroxyl groups, and hydrocarbons on the Si(111) surface. We observe subtle effects in the evolution of the chemical state of the surface during sample storage and process-related wafer handling and discuss their effect on the electronic properties of the involved interfaces. PMID:26233357

  11. ATR-FTIR Spectroscopy in the Undergraduate Chemistry Laboratory: Part II--A Physical Chemistry Laboratory Experiment on Surface Adsorption

    ERIC Educational Resources Information Center

    Schuttlefield, Jennifer D.; Larsen, Sarah C.; Grassian, Vicki H.

    2008-01-01

    Attenuated total reflectance-Fourier transform infrared (ATR-FTIR) spectroscopy is a useful technique for measuring the infrared spectra of solids and liquids as well as probing adsorption on particle surfaces. The use of FTIR-ATR spectroscopy in organic and inorganic chemistry laboratory courses as well as in undergraduate research was presented…

  12. ATR-FTIR Spectroscopy in the Undergraduate Chemistry Laboratory: Part II--A Physical Chemistry Laboratory Experiment on Surface Adsorption

    ERIC Educational Resources Information Center

    Schuttlefield, Jennifer D.; Larsen, Sarah C.; Grassian, Vicki H.

    2008-01-01

    Attenuated total reflectance-Fourier transform infrared (ATR-FTIR) spectroscopy is a useful technique for measuring the infrared spectra of solids and liquids as well as probing adsorption on particle surfaces. The use of FTIR-ATR spectroscopy in organic and inorganic chemistry laboratory courses as well as in undergraduate research was presented

  13. The effect of breast cancer on the Fourier transform infrared attenuated total reflection spectra of human hair

    PubMed Central

    Lyman, Donald J; Fay, Sheila G

    2014-01-01

    Changes in the Synchrotron x-ray diffraction pattern of scalp hair were shown to occur in patients with breast cancer. A preliminary Fourier transform infrared (FT-IR) spectroscopy study of scalp hair using attenuated total reflection (ATR) supported the concept that these changes are due to an increase in the lipid content of the hair fibre. This study was undertaken to determine whether the ATR-FT-IR spectrum obtained using a single hair fibre ATR cell could be used in the detection of breast cancer. In addition, variable angle ATR-FT-IR difference spectra were obtained to investigate the location and the molecular structure of this lipid material in the hair fibre, which appears to be an indicator of breast cancer. Patients with breast cancer showed an increase in the peak height ratio of the 1446–1456 cm−1 C–H bending absorption bands of the ATR-FT-IR spectra of a single hair fibre. Peak height ratios > 1.0 were indicative of breast cancer. The spectra of scalp hair of subjects with breast cancer also showed a slight shift in C–H bending absorption from 1446 to 1448 cm−1 and from 1456 to 1458 cm−1 that could result from the formation of secondary structures by the increased lipid material. Variable angle difference spectra indicated that this increased lipid material is located in the cuticle–cortex interface area and appears to be similar to the lipids normally found here. An alteration in hair biosynthesis in the follicle caused by breast cancer signalling molecules, or biomarkers, is most likely involved. ATR-FT-IR spectral analysis of a long hair fibre containing a distal portion formed when the breast cancer was present and a proximal portion formed after the breast cancer was removed showed that hair fibre synthesis had become normal after the removal of the cancer. This study demonstrates the potential of ATR-FT-IR analysis of a hair fibre in the early detection of breast cancer and in studying how hair acts as a biosensor for breast cancer. PMID:24605137

  14. High-sensitivity infrared attenuated total reflectance sensors for in situ multicomponent detection of volatile organic compounds in water.

    PubMed

    Lu, Rui; Li, Wen-Wei; Mizaikoff, Boris; Katzir, Abraham; Raichlin, Yosef; Sheng, Guo-Ping; Yu, Han-Qing

    2016-02-01

    In situ detection of volatile organic compounds (VOCs) in aqueous environments is imperative for ensuring the quality and safety of water supplies, yet it remains a challenging analytical task. We present a high-sensitivity method for in situ analysis of multicomponent VOCs at low concentrations based on the use of infrared attenuated total reflection (IR-ATR) spectroscopy. This protocol uses a unique ATR waveguide, which comprises a planar silver halide (AgClxBr1-x) fiber with cylindrical extensions at both ends to increase the number of internal reflections, and a polymer coating that traps VOCs and excludes water molecules. Depending on the type of VOC and measurement scenario, IR spectra with specific frequency windows, scan times and spectral resolutions are obtained, from which concentration information is derived. This protocol allows simultaneous detection of multiple VOCs at concentrations around 10 p.p.b., and it enables accurate quantification via a single measurement within 5 min without the need for sample collection or sample pretreatment. This IR-ATR sensor technology will be useful for other applications; we have included a procedure for the analysis of protein conformation changes in Supplementary Methods as an example. PMID:26820794

  15. Total Internal Reflection Accounts for the Bright Color of the Saharan Silver Ant

    PubMed Central

    Aron, Serge

    2016-01-01

    The Saharan silver ant Cataglyphis bombycina is one of the terrestrial living organisms best adapted to tolerate high temperatures. It has recently been shown that the hairs covering the ant’s dorsal body part are responsible for its silvery appearance. The hairs have a triangular cross-section with two corrugated surfaces allowing a high optical reflection in the visible and near-infrared (NIR) range of the spectrum while maximizing heat emissivity in the mid-infrared (MIR). Those two effects account for remarkable thermoregulatory properties, enabling the ant to maintain a lower thermal steady state and to cope with the high temperature of its natural habitat. In this paper, we further investigate how geometrical optical and high reflection properties account for the bright silver color of C. bombycina. Using optical ray-tracing models and attenuated total reflection (ATR) experiments, we show that, for a large range of incidence angles, total internal reflection (TIR) conditions are satisfied on the basal face of each hair for light entering and exiting through its upper faces. The reflection properties of the hairs are further enhanced by the presence of the corrugated surface, giving them an almost total specular reflectance for most incidence angles. We also show that hairs provide an almost 10-fold increase in light reflection, and we confirm experimentally that they are responsible for a lower internal body temperature under incident sunlight. Overall, this study improves our understanding of the optical mechanisms responsible for the silver color of C. bombycina and the remarkable thermoregulatory properties of the hair coat covering the ant’s body. PMID:27073923

  16. Total Internal Reflection Accounts for the Bright Color of the Saharan Silver Ant.

    PubMed

    Willot, Quentin; Simonis, Priscilla; Vigneron, Jean-Pol; Aron, Serge

    2016-01-01

    The Saharan silver ant Cataglyphis bombycina is one of the terrestrial living organisms best adapted to tolerate high temperatures. It has recently been shown that the hairs covering the ant's dorsal body part are responsible for its silvery appearance. The hairs have a triangular cross-section with two corrugated surfaces allowing a high optical reflection in the visible and near-infrared (NIR) range of the spectrum while maximizing heat emissivity in the mid-infrared (MIR). Those two effects account for remarkable thermoregulatory properties, enabling the ant to maintain a lower thermal steady state and to cope with the high temperature of its natural habitat. In this paper, we further investigate how geometrical optical and high reflection properties account for the bright silver color of C. bombycina. Using optical ray-tracing models and attenuated total reflection (ATR) experiments, we show that, for a large range of incidence angles, total internal reflection (TIR) conditions are satisfied on the basal face of each hair for light entering and exiting through its upper faces. The reflection properties of the hairs are further enhanced by the presence of the corrugated surface, giving them an almost total specular reflectance for most incidence angles. We also show that hairs provide an almost 10-fold increase in light reflection, and we confirm experimentally that they are responsible for a lower internal body temperature under incident sunlight. Overall, this study improves our understanding of the optical mechanisms responsible for the silver color of C. bombycina and the remarkable thermoregulatory properties of the hair coat covering the ant's body. PMID:27073923

  17. Analytical model for the excitation of leaky surface plasmon polaritons in the attenuated total reflection configuration

    NASA Astrophysics Data System (ADS)

    Jia, Hongwei; Xie, Yunya; Liu, Haitao; Zhong, Ying

    2016-05-01

    We propose a fully-analytical model for the excitation of leaky surface plasmon polariton (SPP) in the attenuated total reflection (ATR) configuration under illumination by a finite-width beam of electromagnetic wave. The model is built up on the basis of the general unconjugated-form reciprocity theorem and is able to predict the excitation amplitude and phase of the leaky SPP at a quantitative level. The validity of the model is carefully supported through a comparison with the numerical results obtained with the mode orthogonality. With the model a physical understanding of the resonant excitation of the leaky SPP is achieved and the optimal parameters such as the incidence angle and the beam width to ensure an efficient SPP excitation are demonstrated for design tasks.

  18. Application of micro-attenuated total reflectance Fourier transform infrared spectroscopy to ink examination in signatures written with ballpoint pen on questioned documents.

    PubMed

    Nam, Yun Sik; Park, Jin Sook; Lee, Yeonhee; Lee, Kang-Bong

    2014-05-01

    Questioned documents examined in a forensic laboratory sometimes contain signatures written with ballpoint pen inks; these signatures were examined to assess the feasibility of micro-attenuated total reflectance (ATR) Fourier transform infrared (FTIR) spectroscopy as a forensic tool. Micro-ATR FTIR spectra for signatures written with 63 ballpoint pens available commercially in Korea were obtained and used to construct an FTIR spectral database. A library-searching program was utilized to identify the manufacturer, blend, and model of each black ballpoint pen ink based upon their FTIR peak intensities, positions, and patterns in the spectral database. This FTIR technique was also successfully used in determining the sequence of homogeneous line intersections from the crossing lines of two ballpoint pen signatures. We have demonstrated with a set of sample documents that micro-ATR FTIR is a viable nondestructive analytical method that can be used to identify the origin of the ballpoint pen ink used to mark signatures. PMID:24661236

  19. Epidermal in vivo and in vitro studies by attenuated total reflection mid-infrared spectroscopy using flexible silver halide fibre-probes

    NASA Astrophysics Data System (ADS)

    Heise, H. M.; Küpper, L.; Pittermann, W.; Stücker, M.

    2003-06-01

    Dermatology studies focussing on the stratum corneum were carried out by infrared attenuated total reflection (ATR) spectroscopy using flexible fibre-optic probes made from square cross-section polycrystalline silver halide material. We compared the upper horny layer of human and bovine udder skin (BUS). As a substitute for human in vivo tests, the in vitro model of the isolated perfused bovine udder skin (BUS-model) has been used. For depth profiling of endogenous and topically applied compounds, subsequent stripping of corneocyte layers by adhesive tape application was carried out in combination with in situ fibre-probe ATR-measurements. The non-invasive measurement technique was also applied to patients with various skin abnormalities. Owing to the remote sensing capability, the technique presented is promising, since it opens the field for new medical and cosmetic applications, which are otherwise not possible with conventional sampling compartment based ATR-accessories.

  20. Total reflection infrared spectroscopy of water-ice and frozen aqueous NaCl solutions.

    PubMed

    Walker, Rachel L; Searles, Keith; Willard, Jesse A; Michelsen, Rebecca R H

    2013-12-28

    Liquid-like and liquid water at and near the surface of water-ice and frozen aqueous sodium chloride films were observed using attenuated total reflection infrared spectroscopy (ATR-IR). The concentration of NaCl ranged from 0.0001 to 0.01 M and the temperature varied from the melting point of water down to 256 K. The amount of liquid brine at the interface of the frozen films with the germanium ATR crystal increased with salt concentration and temperature. Experimental spectra are compared to reflection spectra calculated for a simplified morphology of a uniform liquid layer between the germanium crystal and the frozen film. This morphology allows for the amount of liquid observed in an experimental spectrum to be converted to the thickness of a homogenous layer with an equivalent amount of liquid. These equivalent thickness ranges from a nanometer for water-ice at 260 K to 170 nm for 0.01 M NaCl close to the melting point. The amounts of brine observed are over an order of magnitude less than the total liquid predicted by equilibrium thermodynamic models, implying that the vast majority of the liquid fraction of frozen solutions may be found in internal inclusions, grain boundaries, and the like. Thus, the amount of liquid and the solutes dissolved in them that are available to react with atmospheric gases on the surfaces of snow and ice are not well described by thermodynamic equilibrium models which assume the liquid phase is located entirely at the surface. PMID:24387384

  1. Total reflection infrared spectroscopy of water-ice and frozen aqueous NaCl solutions

    SciTech Connect

    Walker, Rachel L.; Searles, Keith; Willard, Jesse A.; Michelsen, Rebecca R. H.

    2013-12-28

    Liquid-like and liquid water at and near the surface of water-ice and frozen aqueous sodium chloride films were observed using attenuated total reflection infrared spectroscopy (ATR-IR). The concentration of NaCl ranged from 0.0001 to 0.01 M and the temperature varied from the melting point of water down to 256 K. The amount of liquid brine at the interface of the frozen films with the germanium ATR crystal increased with salt concentration and temperature. Experimental spectra are compared to reflection spectra calculated for a simplified morphology of a uniform liquid layer between the germanium crystal and the frozen film. This morphology allows for the amount of liquid observed in an experimental spectrum to be converted to the thickness of a homogenous layer with an equivalent amount of liquid. These equivalent thickness ranges from a nanometer for water-ice at 260 K to 170 nm for 0.01 M NaCl close to the melting point. The amounts of brine observed are over an order of magnitude less than the total liquid predicted by equilibrium thermodynamic models, implying that the vast majority of the liquid fraction of frozen solutions may be found in internal inclusions, grain boundaries, and the like. Thus, the amount of liquid and the solutes dissolved in them that are available to react with atmospheric gases on the surfaces of snow and ice are not well described by thermodynamic equilibrium models which assume the liquid phase is located entirely at the surface.

  2. Determination of the polymorphic forms of bicifadine hydrochloride by differential scanning calorimetry-thermogravimetric analysis, X-ray powder diffraction, attenuated total reflectance-infrared spectroscopy, and attenuated total reflectance-near-infrared spectroscopy.

    PubMed

    McArdle, Patrick; Gilligan, Karen; Cunningham, Desmond; Ryder, Alan

    2005-11-01

    The pharmaceutical compound bicifadine hydrochloride, which has been found to crystallize in two polymorphic forms, has been characterized by thermal analysis, X-ray powder diffraction (XRPD), infrared (IR) spectroscopy, and near-infrared (NIR) spectroscopy. A series of 22 sample mixtures of polymorph 1 and polymorph 2 were prepared and calibration models for the quantitation of these binary mixtures have been developed for each of the XRPD, attenuated total reflectance (ATR)-IR, and ATR-NIR analytical techniques. The quantitative results were obtained using a partial least squares (PLS) algorithm, which predicted the concentration of polymorph 1 from the XRPD spectra with a root mean standard error of prediction (RMSEP) of 4.4%, from the IR spectra with a RMSEP of 3.8%, and from the NIR spectra with a RMSEP of 1.4%. The studies indicate that when analyses are carried out on equivalent sets of spectra, NIR spectroscopy offers significant advantages in quantitative accuracy as a tool for the determination of polymorphs in the solid state and is also more convenient to use than both the ATR-IR and XRPD methods. Density functional theory (DFT) B3LYP calculations and IR spectral simulation have been used to determine the nature of the vibrational modes that are the most sensitive in the analysis. PMID:16316514

  3. Hygrothermal degradation of 3-glycidoxypropyltrimethoxysilane films studied by neutron and X-ray reflectivity and attenuated total reflection infrared spectroscopy.

    SciTech Connect

    Tallant, David Robert; Garcia, Manuel Joseph; Majewski, Jaroslaw; Kent, Michael Stuart; Yim, Hyun

    2005-05-01

    Thin films of organosilanes have great technological importance in the areas of adhesion promotion, durability, and corrosion resistance. However, it is well-known that water can degrade organosilane films, particularly at elevated temperatures. In this work, X-ray and neutron reflectivity (XR and NR) were combined with attenuated total reflection infrared (ATR-IR) spectroscopy to study the chemical and structural changes within thin films of (3-glycidoxypropyl)trimethoxysilane (GPS) after exposure for various periods of time to air saturated with either D{sub 2}O or H{sub 2}O at 80 C. For NR and XR, ultrathin ({approx}100 {angstrom}) films were prepared by spin-coating. Both D{sub 2}O and H{sub 2}O provide neutron scattering contrast with GPS. Variations in the neutron scattering length density (SLD) profiles (a function of mass density and atomic composition) with conditioning time were measured after drying the samples out and also swelled with H{sub 2}O or D{sub 2}O vapor at room temperature. For samples that were dried out prior to measurement, little or no change was observed for H{sub 2}O conditioning up to 3.5 days, but large changes were observed after 30 days of conditioning. The range of conditioning time for this structural change was narrowed to between 4 and 10 days with XR. The SLD profiles indicated that the top portion of the GPS film was transformed into a thick low-density layer after conditioning, but the bottom portion showed little structural change. A previous NR study of as-prepared GPS films involving swelling with deuterated nitrobenzene showed that the central portion of the film has much lower cross-link density than the region nearest the substrate. The present data show that the central portion also swells to a much greater extent with water and hydrolyzes more rapidly. The chemical degradation mechanism was identified by IR as hydrolysis of siloxane bonds. For ATR-IR, GPS films were prepared by dip-coating, which resulted in a greater and more variable thickness than for the spin-coated samples. The IR spectra revealed an increase in vicinal silanol generation over the first 3 days of conditioning followed by geminal silanol generation. Thus, the structural change detected by NR and XR roughly coincided with the onset of geminal silanol generation. Finally, little change in the reflectivity data was observed for films conditioned with D{sub 2}O at 80 C for 1 month. This indicates that hydrolysis of Si-O-Si is much slower with D{sub 2}O than with H{sub 2}O.

  4. Attenuated total reflectance-fourier transform infrared microspectroscopy of copper(II) complexes with reduced dextran derivatives

    NASA Astrophysics Data System (ADS)

    Nikolić, G. S.; Cakić, M.; Mitić, Ž.; Ilić, B.; Premović, P.

    2009-09-01

    Dextran is a water-soluble, extracellular neutral polysaccharide with a linear flexible chain of α-(1 → 6)-linked α-D-glucopyranose units, in a single compounds. In alkali solutions Cu(II) ion forms complexes with reduced low-molar dextran (RLMD). The metal content and the solution composition depended on pH. The complexing process begins in weak alkali solution (pH > 7), and involves OH groups in C2 and C3 dextran monomer units. Synthesized copper(II) complexes with RLMD, of average molar mass M w = 5000 g/mol were investigated by attenuated total reflectance-Fourier transform infrared (ATR-FTIR) spectroscopy and FTIR imaging microscopy. ATR-FTIR microspectroscopic data of synthesized complexes are rare in literature. The changes in intensity and width of the IR bands in region 1500-1000 cm-1 were related to changes in conformation and short-range interactions of the ligand dextran. FTIR microscopy images shows more and less ordered structures of the Cu(II)-RLMD complexes. ATR-FTIR microspectroscopic data shows homogeneity of the Cu(II)-RLMD samples and green color of the samples confirm existence of Cu(II) ions.

  5. Investigating the secondary structures for long oligonucleotides using attenuated-total-reflection nanoplasmon-enhanced Raman scattering

    NASA Astrophysics Data System (ADS)

    Chiu, K.-C.; Yu, L.-Y.; Lin, C.-Y.; Chen, S.-J.

    2007-09-01

    This study utilizes a nanoplasmon-enhanced Raman scattering based on the attenuated-total-reflection (ATR) method to investigate the secondary structures of long oligonucleotides and their influence on the DNA hybridization. It is found that the ring-breathing modes of adenine, thymine, guanine, and cytosine in Raman fingerprint associated with three 60mer oligonucleotides with prominent secondary structures are lower than those observed for the two oligonucleotides with no obvious secondary structures. It is also determined that increasing the DNA hybridization temperature from 35 °C to 45 °C reduces secondary structure effects. The kinetics of biomolecular interaction analysis can be performed by using surface plasmons resonance biosensor, but the structural information of the oligonucleotides can not observed directly. The ATR-Raman spectrum can provide the structural information of the oligonucleotide monolayer on the sensing surface with the help of a silver patterned nanostructure film based on the finite-difference time-domain simulation and the e-beam lithography fabrication adapted as an ATR-Raman active substrate.

  6. The Advantages of an Attenuated Total Internal Reflection Infrared Microspectroscopic Imaging Approach for Kidney Biopsy Analysis

    PubMed Central

    Gulley-Stahl, Heather J.; Bledsoe, Sharon B.; Evan, Andrew P.; Sommer, André J.

    2011-01-01

    The benefits of an ATR-FTIR imaging approach for kidney biopsy analysis are described. Biopsy sections collected from kidney stone formers are analyzed at the initial stages of stone development to provide insights into stone growth and formation. The majority of tissue analysis currently conducted with IR microspectroscopy is performed with a transflection method. The research presented in this manuscript demonstrates that ATR overcomes many of the disadvantages of transflection or transmission measurements for tissue analysis including an elimination of spectral artifacts. When kidney biopsies with small mineral inclusions are analyzed with a transflection approach, specular reflection, and the Christiansen effect (anomalous dispersion) can occur leading to spectral artifacts. Another effect specific to the analysis of mineral inclusions present in kidney biopsies is known as the reststrahlen effect where the inclusions become strong reflectors near an absorption band. ATR eliminates these effects by immersing the sample in a high index medium. Additionally, the focused beam size for ATR is decreased by a factor of four when a germanium internal reflection element is used, allowing the acquisition of spectra from small mineral inclusions several micrometers in diameter. If quantitative analysis of small mineral inclusions is ultimately desired, ATR provides the photometrically accurate spectra necessary for quantification. PMID:20132593

  7. MIR-ATR sensor for process monitoring

    NASA Astrophysics Data System (ADS)

    Geörg, Daniel; Schalk, Robert; Methner, Frank-Jürgen; Beuermann, Thomas

    2015-06-01

    A mid-infrared attenuated total reflectance (MIR-ATR) sensor has been developed for chemical reaction monitoring. The optical setup of the compact and low-priced sensor consists of an IR emitter as light source, a zinc selenide (ZnSe) ATR prism as boundary to the process, and four thermopile detectors, each equipped with an optical bandpass filter. The practical applicability was tested during esterification of ethanol and formic acid to ethyl formate and water as a model reaction with subsequent distillation. For reference analysis, a Fourier transform mid-infrared (FT-MIR) spectrometer with diamond ATR module was applied. On-line measurements using the MIR-ATR sensor and the FT-MIR spectrometer were performed in a bypass loop. The sensor was calibrated by multiple linear regression in order to link the measured absorbance in the four optical channels to the analyte concentrations. The analytical potential of the MIR-ATR sensor was demonstrated by simultaneous real-time monitoring of all four chemical substances involved in the esterification and distillation process. The temporal courses of the sensor signals are in accordance with the concentration values achieved by the commercial FT-MIR spectrometer. The standard error of prediction for ethanol, formic acid, ethyl formate, and water were 0.38 mol L  -  1, 0.48 mol L  -  1, 0.38 mol L  -  1, and 1.12 mol L  -  1, respectively. A procedure based on MIR spectra is presented to simulate the response characteristics of the sensor if the transmission ranges of the filters are varied. Using this tool analyte specific bandpass filters for a particular chemical reaction can be identified. By exchanging the optical filters, the sensor can be adapted to a wide range of processes in the chemical, pharmaceutical, and beverage industries.

  8. Evaluation of various polyethylene as potential dosimeters by attenuated total reflectance-Fourier-transform infrared spectroscopy

    NASA Astrophysics Data System (ADS)

    Halperin, Fred; Collins, Greta; DiCicco, Michael; Logar, John

    2014-12-01

    Various types of polyethylene (PE) have been evaluated in the past for use as a potential dosimeter, chiefly via the formation of an unsaturated transvinylene (TV) double-bond resulting from exposure to ionizing radiation. The utilization of attenuated total reflectance Fourier-transform infrared (ATR-FTIR) spectroscopy in characterizing TV formation in irradiated PE for a potential dosimeter has yet to be fully developed. In this initial investigation, various PE films/sheets were exposed to ionizing radiation in a high-energy 5 megaelectron volt (MeV) electron beam accelerator in the 10-500 kilogray (kGy) dose range, followed by ATR-FTIR analysis of TV peak formation at the 965 cm-1 wavenumber. There was an upward trend in TV formation for low-density polyethylene (LDPE) films and high-density polyethylene (HDPE) sheets as a function of absorbed dose in the 10-50 kGy dose range, however, the TV response could not be equated to a specific absorbed dose. LDPE film displayed a downward trend from 50 kGy to 250 kGy and then scattering up to 500 kGy; HDPE sheets demonstrated an upward trend in TV formation up to 500 kGy. For ultra-high molecular weight polyethylene (UHMWPE) sheets irradiated up to 150 kGy, TV response was equivalent to non-irradiated UHMWPE, and a minimal upward trend was observed for 200 kGy to 500 kGy. The scatter of the data for the irradiated PE films/sheets is such that the TV response could not be equated to a specific absorbed dose. A better correlation of the post-irradiation TV response to absorbed dose may be attained through a better understanding of variables.

  9. [Attenuated total reflection-fourier transform infrared spectroscopic study of dried shark fin products].

    PubMed

    Han, Wan-qing; Luo, Hai-ying; Xian, Yan-ping; Luo, Dong-hui; Mu, Torng-na; Guo, Xin-dong

    2015-02-01

    Sixty-four pieces of shark fin dried products (including real, fake and artificial shark fin products) and real products coated with gelatin were rapidly and nondestructively analyzed by attenuated total reflection-Fourier transform infrared spectroscopy (ATR-FTIR). The characteristic of IR spectrograms among the above four kinds of samples were systematically studied and comparied, the results showed that the spectrograms of the same kind of samples were repeatable, and different kinds of shark fin products presented significant differences in the spectrograms, which mainly manifested as the specific absorption peaks of amido bonds in protein (1650, 1544 cm(-1)) and skeletal vibration in polysaccharide (1050 cm(-1)). The spectrograms of real shark fins were characterized by the strong absorption peaks of protein characteristic amide I and II absorbent (1650, 1544 cm(-1)) and relatively weak C--O--C vibration absorbent (1050 cm(-1)) owing to the high content of protein and relatively low level of polysaccharide. For fake shark fin products that were molded form by mixing together with the offcut of shark, collagen and other substances, the introduction of non-protein materials leaded to the weaker amido bonds absorbent than real products along with a 30 cm(-1) blue shift of amide I absorbent. Opposite to the real sample, the relatively strong absorption peak of polysaccharide (approximately 1047 cm(-1)) and barely existed amide absorbent were the key features of the spectrogram of artificial samples, which was synthersized by polysaccharide like sodium alginate. Real samples coated with gelatin, the peak strength of protein and polysaccharide were decreased simultaneously when the data collection was taken at the surface of sample, while the spectrogram presented no significant difference to real samples when the data was collected in the section. The results above indicated that by analyzing the characteristic of IR spectrograms and the value range of Apro/Apol collected by ATR-FTIR method could perform the undamaged and rapid identification for shark fins. PMID:25970896

  10. Measuring Photochemical Kinetics in Submonolayer Films by Transient ATR Spectroscopy on a Multimode Planar Waveguide

    SciTech Connect

    Simon, Anne M.; Marucci, Nicole E.; Saavedra, S. Scott

    2011-07-15

    Understanding the kinetics of reactions in molecular thin films can aid in the molecular engineering of organic photovoltaics and biosensors. Using two analytical methods, transient absorbance spectroscopy (TAS) and attenuated total reflectance (ATR), in a relatively simple arrangement when compared with previous TAS/ATR instruments to interrogate molecular structure and photochemistry at interfaces. The multimode planar waveguide geometry provides a significant path length enhancement relative to a conventional transmission geometry, making it feasible to perform measurements on low-surface-coverage films. This work demonstrates that TAS/ATR can be used to probe structure and photochemical kinetics in molecular films at extremely low surface coverages.

  11. Determination of antioxidant capacity and phenolic content of chocolate by attenuated total reflectance-Fourier transformed-infrared spectroscopy.

    PubMed

    Hu, Yaxi; Pan, Zhi Jie; Liao, Wen; Li, Jiaqi; Gruget, Pierre; Kitts, David D; Lu, Xiaonan

    2016-07-01

    Antioxidant capacity and phenolic content of chocolate, containing different amounts of cacao (35-100%), were determined using attenuated total reflectance (ATR)-Fourier transformed-infrared (FT-IR) spectroscopy (4000-550cm(-1)). Antioxidant capacities were first characterized using DPPH (2,2-diphenyl-1-picrylhydrazyl) and ORAC (oxygen radical absorbance capacity) assays. Phenolic contents, including total phenol and procyanidins monomers, were quantified using the Folin-Ciocalteu assay and high performance liquid chromatography coupled with photodiode array detector (HPLC-DAD), respectively. Five partial least-squares regression (PLSR) models were constructed and cross-validated using FT-IR spectra from 18 types of chocolate and corresponding reference values determined using DPPH, ORAC, Folin-Ciocalteu, and HPLC assays. The models were validated using seven unknown samples of chocolate. PLSR models showed good prediction capability for DPPH [R(2)-P (prediction)=0.88, RMSEP (root mean squares error of prediction)=12.62μmol Trolox/g DFW], ORAC (R(2)-P=0.90, RMSEP=37.92), Folin-Ciocalteu (R(2)-P=0.88, RMSEP=5.08), and (+)-catechin (R(2)-P=0.86, RMSEP=0.10), but lacked accuracy in the prediction of (-)-epicatechin (R(2)-P=0.72, RMSEP=0.57). ATR-FT-IR spectroscopy can be used for rapid prediction of antioxidant capacity, total phenolic content, and (+)-catechin in chocolate. PMID:26920292

  12. Broad Band Intra-Cavity Total Reflection Chemical Sensor

    DOEpatents

    Pipino, Andrew C. R.

    1998-11-10

    A broadband, ultrahigh-sensitivity chemical sensor is provided that allows etection through utilization of a small, extremely low-loss, monolithic optical cavity. The cavity is fabricated from highly transparent optical material in the shape of a regular polygon with one or more convex facets to form a stable resonator for ray trajectories sustained by total internal reflection. Optical radiation enters and exits the monolithic cavity by photon tunneling in which two totally reflecting surfaces are brought into close proximity. In the presence of absorbing material, the loss per pass is increased since the evanescent waves that exist exterior to the cavity at points where the circulating pulse is totally reflected, are absorbed. The decay rate of an injected pulse is determined by coupling out an infinitesimal fraction of the pulse to produce an intensity-versus-time decay curve. Since the change in the decay rate resulting from absorption is inversely proportional to the magnitude of absorption, a quantitative sensor of concentration or absorption cross-section with 1 part-per-million/pass or better sensitivity is obtained. The broadband nature of total internal reflection permits a single device to be used over a broad wavelength range. The absorption spectrum of the surrounding medium can thereby be obtained as a measurement of inverse decay time as a function of wavelength.

  13. Gaining Insight into Antibubbles via Frustrated Total Internal Reflection

    ERIC Educational Resources Information Center

    Suhr, Wilfried

    2012-01-01

    The interest in the phenomenon of frustrated total internal reflection dates back to the time of Newton. Because of its technological relevance, it has become a standard topic covered by advanced courses in physics. In practical courses optical setups especially designed to demonstrate the phenomenon are commonly used. As an alternative, this…

  14. Evaluation of the moisture prediction capability of near-infrared and attenuated total reflectance fourier transform infrared spectroscopy using superdisintegrants as model compounds.

    PubMed

    Uppaluri, Sai G; Bompelliwar, Sai K; Johnson, Paul R; Gupta, Mali R; Al-Achi, Antoine; Stagner, William C; Haware, Rahul V

    2014-12-01

    The superdisintegrants (SDs) moisture content measurement by near-infrared (NIR) spectroscopy and attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectroscopy has been evaluated against thermogravimetric analysis as a reference method. SDs with varying moisture content were used to build calibration and independent model verification data sets. Calibration models were developed based on the water-specific NIR and ATR-FTIR spectral regions using partial least-square regression methods. Because of the NIR water low molar absorptivity, NIR spectroscopy handled higher moisture content (∼81%, w/w) than ATR-FTIR (∼25%, w/w). A two-way ANOVA test was performed to compare R(2) values obtained from measured and predicted moisture content (5%-25%, w/w) of SDs. No statistically significant difference was observed between the predictability of NIR and ATR-FTIR methods (p = 0.3504). However, the interactions between the two independent variables, SDs, and analytical methods were statistically significant (p = 0.0002), indicating that the predictability of the analytical method is material dependent. Thus, it would be important to recognize this highly dependent material and analytical method interaction when using NIR moisture analysis in process analytical technology to analyze and control critical quality and performance attributes of raw materials during processing with the goal of ensuring final product quality attributes. PMID:25332106

  15. Cell-substrate contacts illuminated by total internal reflection fluorescence.

    PubMed

    Axelrod, D

    1981-04-01

    A technique for exciting fluorescence exclusively from regions of contact between cultured cells and the substrate is presented. The technique utilizes the evanescent wave of a totally internally reflecting laser beam to excite only those fluorescent molecules within one light wavelength or less of the substrate surface. Demonstrations of this technique are given for two types of cell cultures: rat primary myotubes with acetylcholine receptors labeled by fluorescent alpha-bungarotoxin and human skin fibroblasts labeled by a fluorescent lipid probe. Total internal reflection fluorescence examination of cells appears to have promising applications, including visualization of the membrane and underlying cytoplasmic structures at cell-substrate contacts, dramatic reduction of autofluorescence from debris and thick cells, mapping of membranes topography, and visualization of reversible bound fluorescent ligands at membrane receptors. PMID:7014571

  16. Multiple-channel, total-reflection optic with controllable divergence

    DOEpatents

    Gibson, D.M.; Downing, R.G.

    1997-02-18

    An apparatus and method for providing focused x-ray, gamma-ray, charged particle and neutral particle, including neutron, radiation beams with a controllable amount of divergence are disclosed. The apparatus features a novel use of a radiation blocking structure, which, when combined with multiple-channel total reflection optics, increases the versatility of the optics by providing user-controlled output-beam divergence. 11 figs.

  17. Multiple-channel, total-reflection optic with controllable divergence

    DOEpatents

    Gibson, David M.; Downing, Robert G.

    1997-01-01

    An apparatus and method for providing focused x-ray, gamma-ray, charged particle and neutral particle, including neutron, radiation beams with a controllable amount of divergence are disclosed. The apparatus features a novel use of a radiation blocking structure, which, when combined with multiple-channel total reflection optics, increases the versatility of the optics by providing user-controlled output-beam divergence.

  18. Attenuated total reflectance fourier transform infrared analysis of fly ash geopolymer gel aging.

    PubMed

    Rees, Catherine A; Provis, John L; Lukey, Grant C; van Deventer, Jannie S J

    2007-07-17

    Structural changes in fly ash geopolymers activated with different sodium hydroxide and silicate concentrations are investigated using attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectroscopy over a period of 200 days. A strong correlation is found between the concentration of silicate monomer in the activating solution and the position of the main Si-O-T stretching band in the FTIR spectrum, which gives an indication of the relative changes in the gel Si/Al ratio. The FTIR spectra of geopolymer samples with activating solution concentrations of up to 1.2 M SiO2 indicate that an Al-rich gel forms before the final gel composition is reached. The time required for the system to reach a steady gel composition depends on the silicate activating solution concentration and speciation. Geopolymers activated with solutions containing predominantly high-order silicate species rapidly reach a steady gel composition without first forming an Al-rich gel. A minimum silicate monomer concentration of approximately 0.6 M is required to shift the geopolymer synthesis mechanism from hydroxide activation to silicate activation. Silicate speciation in the activating solutions also affects zeolite formation and geopolymer microstructures, with a more homogeneous microstructure and less zeolite formation observed at a higher SiO2 content. PMID:17590027

  19. Fourier Transform Infrared with Attenuated Total Reflectance Applied to the Discrimination of Freshwater Planktonic Coccoid Green Microalgae

    PubMed Central

    de Moraes, Guilherme Pavan; Vieira, Armando Augusto Henriques

    2014-01-01

    Despite the recent advances on fine taxonomic discrimination in microorganisms, namely using molecular biology tools, some groups remain particularly problematic. Fine taxonomy of green algae, a widely distributed group in freshwater ecosystems, remains a challenge, especially for coccoid forms. In this paper, we propose the use of the Fourier Transform Infrared (FTIR) spectroscopy as part of a polyphasic approach to identify and classify coccoid green microalgae (mainly order Sphaeropleales), using triplicated axenic cultures. The attenuated total reflectance (ATR) technique was tested to reproducibility of IR spectra of the biological material, a primary requirement to achieve good discrimination of microalgal strains. Spectral window selection was also tested, in conjunction with the first derivative treatment of spectra, to determine which regions of the spectrum provided better separation and clustering of strains. The non-metric multidimensional scaling (NMDS), analysis of similarities (ANOSIM) and hierarchical clusters (HCA), demonstrated a correct discrimination and classification of closely related strains of chlorophycean coccoid microalgae, with respect to currently accepted classifications. FTIR-ATR was highly reproducible, and provided an excellent discrimination at the strain level. The best separation was achieved by analyzing the spectral windows of 1500–1200 cm−1 and 900–675 cm−1, which differs from those used in previously studies for the discrimination of broad algal groups, and excluding spectral regions related to storage compounds, which were found to give poor discrimination. Furthermore, hierarchical cluster analyses have positioned the strains tested into clades correctly, reproducing their taxonomic orders and families. This study demonstrates that FTIR-ATR has great potential to complement classical approaches for fine taxonomy of coccoid green microalgae, though a careful spectrum region selection is needed. PMID:25541701

  20. Exploration of attenuated total reflectance mid-infrared spectroscopy and multivariate calibration to measure immunoglobulin G in human sera.

    PubMed

    Hou, Siyuan; Riley, Christopher B; Mitchell, Cynthia A; Shaw, R Anthony; Bryanton, Janet; Bigsby, Kathryn; McClure, J Trenton

    2015-09-01

    Immunoglobulin G (IgG) is crucial for the protection of the host from invasive pathogens. Due to its importance for human health, tools that enable the monitoring of IgG levels are highly desired. Consequently there is a need for methods to determine the IgG concentration that are simple, rapid, and inexpensive. This work explored the potential of attenuated total reflectance (ATR) infrared spectroscopy as a method to determine IgG concentrations in human serum samples. Venous blood samples were collected from adults and children, and from the umbilical cord of newborns. The serum was harvested and tested using ATR infrared spectroscopy. Partial least squares (PLS) regression provided the basis to develop the new analytical methods. Three PLS calibrations were determined: one for the combined set of the venous and umbilical cord serum samples, the second for only the umbilical cord samples, and the third for only the venous samples. The number of PLS factors was chosen by critical evaluation of Monte Carlo-based cross validation results. The predictive performance for each PLS calibration was evaluated using the Pearson correlation coefficient, scatter plot and Bland-Altman plot, and percent deviations for independent prediction sets. The repeatability was evaluated by standard deviation and relative standard deviation. The results showed that ATR infrared spectroscopy is potentially a simple, quick, and inexpensive method to measure IgG concentrations in human serum samples. The results also showed that it is possible to build a united calibration curve for the umbilical cord and the venous samples. PMID:26003699

  1. Detection of counterfeit Scotch whisky samples using mid-infrared spectrometry with an attenuated total reflectance probe incorporating polycrystalline silver halide fibres.

    PubMed

    McIntyre, Allyson C; Bilyk, Madeleine L; Nordon, Alison; Colquhoun, Gary; Littlejohn, David

    2011-04-01

    Two methods of analysis were developed to permit detection of counterfeit Scotch whisky samples using a novel attenuated total reflectance (ATR) diamond-tipped immersion probe for mid-infrared (MIR) spectrometry. The first method allowed determination of the ethanol concentration (35-45% (v/v)) in situ without dilution of the samples; the results obtained compared well with the supplied concentrations (average relative error of 1.2% and 0.8% for univariate and multivariate partial least squares (PLS) calibration, respectively). The second method involved analysis of dried residues of the whisky samples and caramel solutions on the diamond ATR crystal; principal component analysis (PCA) of the spectra was used to classify the samples and investigate the colorant added. Seventeen test whisky samples were successfully categorised as either authentic or counterfeit in a blind study when both MIR methods were used. PMID:21435480

  2. Investigating the structural changes of β-amyloid peptide aggregation using attenuated-total-reflection surface-enhanced Raman spectroscopy

    NASA Astrophysics Data System (ADS)

    Chiu, K.-C.; Yu, L.-Y.; Yih, J.-N.; Chen, S.-J.

    2007-02-01

    This study utilizes a surface-enhanced Raman spectroscopy (SERS) based on the attenuated-total-reflection (ATR) method to investigate that the structural information of the biomolecular monolayer on sensing surface can be dynamically observed with a higher signal-to-noise ratio signal. The secondary structures of long oligonucleotides and their influence on the DNA hybridization on the sensing surface are investigated. The SERS spectrum provides the structural information of the oligonucleotides with the help of a silver colloidal nanoparticle monolayer by control of the size and distribution of the nanoparticles adapted as a Raman active substrate. It is found that the ring-breathing modes of adenine, thymine, guanine, and cytosine in Raman fingerprint associated with three 60mer oligonucleotides with prominent secondary structures are lower than those observed for the two oligonucleotides with no obvious secondary structures. It is also determined that increasing the DNA hybridization temperature from 35°C to 45°C reduces secondary structure effects. The ATR-SERS biosensing technique will be used to provide valuable structural information regarding the short-term reversible interactions and long-term polymerization events in the Aβ aggregates on the sensing surface.

  3. Discrimination of the hard keratins animal horn and chelonian shell using attenuated total reflection-infrared spectroscopy.

    PubMed

    Biscardi, Brianna; Welsh, Wendy; Kennedy, Anthony

    2012-05-01

    The ability to discriminate between objects manufactured from animal horn and chelonian (turtle, tortoise, or terrapin) shell is important from a cultural and archeological perspective such that it may allow conservators to determine the appropriate treatment and long-term care solution. It would also aid curators in identifying and cataloging items manufactured from these materials. Discrimination and classification is also a valuable tool for those involved in tracking the illegal trade in restricted materials of this nature. Attenuated total reflection infrared (ATR-IR) spectroscopy, using a single reflection diamond internal reflection element (IRE), coupled with discrimination analysis was used to analyze a total of thirty-nine samples (29 calibration samples, 10 validation samples). A discrimination analysis model was constructed using Mahalanobis distances to classify spectra into one of two classes. The model was then subsequently used to successfully classify all validation samples and correctly identify them as animal horn or chelonian shell based on second-derivative spectra of the amide I and II regions. This technique requires minimal to no sample preparation and may be used to nondestructively identify very small samples successfully without performing detailed secondary structural curve-fitting routines. This model should be a valuable resource to museums, conservators, and wildlife management programs for rapidly and reliably discriminating between animal horn and chelonian shell. PMID:22524968

  4. Coverslip Cleaning and Functionalization for Total Internal Reflection Fluorescence Microscopy.

    PubMed

    Kudalkar, Emily M; Deng, Yi; Davis, Trisha N; Asbury, Charles L

    2016-01-01

    Total internal reflection fluorescence (TIRF) microscopy allows visualization of biological events at the single-molecule level by restricting excitation to a precise focal plane near the coverslip and eliminating out-of-focus fluorescence. The quality of TIRF imaging relies on a high signal-to-noise ratio and therefore it is imperative to prevent adherence of molecules to the glass coverslip. Nonspecific interactions can make it difficult to distinguish true binding events and may also interfere with accurate quantification of background noise. In addition, nonspecific binding of the fluorescently tagged protein will lower the effective working concentration, thereby altering values used to calculate affinity constants. To prevent spurious interactions, we thoroughly clean the surface of the coverslip and then functionalize the glass either by applying a layer of silane or by coating with a lipid bilayer. PMID:27140911

  5. Total Internal Reflection Fluorescence Quantification of Receptor Pharmacology

    PubMed Central

    Fang, Ye

    2015-01-01

    Total internal reflection fluorescence (TIRF) microscopy has been widely used as a single molecule imaging technique to study various fundamental aspects of cell biology, owing to its ability to selectively excite a very thin fluorescent volume immediately above the substrate on which the cells are grown. However, TIRF microscopy has found little use in high content screening due to its complexity in instrumental setup and experimental procedures. Inspired by the recent demonstration of label-free evanescent wave biosensors for cell phenotypic profiling and drug screening with high throughput, we had hypothesized and demonstrated that TIRF imaging is also amenable to receptor pharmacology profiling. This paper reviews key considerations and recent applications of TIRF imaging for pharmacology profiling. PMID:25922915

  6. Frustrated Total Internal Reflection applied to Quantum Tunneling

    NASA Astrophysics Data System (ADS)

    Hull, Nathaniel; Yan, Jia-An

    The objective of this project is to demonstrate an optical phenomenon, frustrated total internal reflection (FTIR), by numerically solving the time-dependent Schrodinger equation (TDSE) in quantum mechanics, and to illustrate the correlations between FTIR and the quantum tunneling in one-dimensional quantum structures. We will use a MATLAB program to numerically propagate a Gaussian wave packet to penetrate finite square barriers. The transmission coefficient is then calculated as a function of the distance between two rectangular barriers/wells. The results will be useful to elucidate the correlations between optical FTIR and quantum tunneling. This work was supported by the FCSM Undergraduate Research Committee, the FCSM Fisher General Endowment and the FDRC Grant (OSPR No. 140269) at Towson University.

  7. Single-Molecule Total Internal Reflection Fluorescence Microscopy.

    PubMed

    Kudalkar, Emily M; Davis, Trisha N; Asbury, Charles L

    2016-01-01

    The advent of total internal reflection fluorescence (TIRF) microscopy has permitted visualization of biological events on an unprecedented scale: the single-molecule level. Using TIRF, it is now possible to view complex biological interactions such as cargo transport by a single molecular motor or DNA replication in real time. TIRF allows for visualization of single molecules by eliminating out-of-focus fluorescence and enhancing the signal-to-noise ratio. TIRF has been instrumental for studying in vitro interactions and has also been successfully implemented in live-cell imaging. Visualization of cytoskeletal structures and dynamics at the plasma membrane, such as endocytosis, exocytosis, and adhesion, has become much clearer using TIRF microscopy. Thanks to recent advances in optics and commercial availability, TIRF microscopy is becoming an increasingly popular and user-friendly technique. In this introduction, we describe the fundamental properties of TIRF microscopy and the advantages of using TIRF for single-molecule investigation. PMID:27140922

  8. A 'pocket guide' to total internal reflection fluorescence.

    PubMed

    Martin-Fernandez, M L; Tynan, C J; Webb, S E D

    2013-10-01

    The phenomenon of total internal reflection fluorescence (TIRF) was placed in the context of optical microscopy by Daniel Axelrod over three decades ago. TIRF microscopy exploits the properties of an evanescent electromagnetic field to optically section sample regions in the close vicinity of the substrate where the field is induced. The first applications in cell biology targeted investigation of phenomena at the basolateral plasma membrane. The most notable application of TIRF is single-molecule experiments, which can provide information on fluctuation distributions and rare events, yielding novel insights on the mechanisms governing the molecular interactions that underpin many fundamental processes within the cell. This short review intends to provide a 'one stop shop' explanation of the electromagnetic theory behind the remarkable properties of the evanescent field, guide the reader through the principles behind building or choosing your own TIRF system and consider how the most popular applications of the method exploit the evanescent field properties. PMID:23889125

  9. A laser output coupler using frustrated total internal reflection.

    PubMed

    Steele, E L; Davis, W C; Treuthart, R L

    1966-01-01

    A unique component has been developed, constructed, and incorporated into an optically pumped ruby laser system. Without using thin film optical coatings, this component allows a known fraction of the radiation to be coupled from a laser system while simultaneously serving as the partial reflector at the output end of the laser. The output coupler, herein described, utilizes a frustrated total internal reflection configuration and is fabricated of fused silica with an air gap 0.483 micro in thickness as the critically controlled element. Techniques have been developed for establishing and maintaining the spacing of the silica members to a predetermined fraction of the ruby emission wavelength of 6943 A. The measured transmission, reflection, and scattering loss characteristics of the coupler are discussed. In addition, schematic diagrams and photographs of the operating coupler are shown. This coupler has withstood repeated Q-spoiled bursts of laser radiation without damage. However, equivalent radiation pulses have consistently destroyed dielectric reflectors. Thus, more reproducible laser experiments can be performed with this coupler than with conventional optically coated reflectors. PMID:20048777

  10. Ultrasound-enhanced attenuated total reflection mid-infrared spectroscopy in-line probe: acquisition of cell spectra in a bioreactor.

    PubMed

    Koch, Cosima; Brandstetter, Markus; Wechselberger, Patrick; Lorantfy, Bettina; Plata, Maria Reyes; Radel, Stefan; Herwig, Christoph; Lendl, Bernhard

    2015-02-17

    This article presents a novel method for selective acquisition of Fourier transform infrared (FT-IR) spectra of microorganisms in-line during fermentation, using Saccharomyces cerevisiae as an example. The position of the cells relative to the sensitive region of the attenuated total reflection (ATR) FT-IR probe was controlled by combing a commercially available ATR in-line probe with contact-free, gentle particle manipulation by ultrasonic standing waves. A prototype probe was successfully constructed, assembled, and tested in-line during fed-batch fermentations of S. cerevisiae. Control over the position of the cells was achieved by tuning the ultrasound frequency: 2.41 MHz was used for acquisition of spectra of the cells (pushing frequency f(p)) and 1.87 MHz, for retracting the cells from the ATR element, therefore allowing spectra of the medium to be acquired. Accumulation of storage carbohydrates (trehalose and glycogen) inside the cells was induced by a lack of a nitrogen source in the feed medium. These changes in biochemical composition were visible in the spectra of the cells recorded in-line during the application of f(p) and could be verified by reference spectra of dried cell samples recorded off-line with a FT-IR microscope. Comparison of the cell spectra with spectra of trehalose, glycogen, glucose, and mannan, i.e., the major carbohydrates present in S. cerevisiae, and principal components analysis revealed that the changes observed in the cell spectra correlated well with the bands specific for trehalose and glycogen. This proves the applicability and capability of ultrasound-enhanced in-line ATR mid-IR spectroscopy as a real-time PAT method for the in situ monitoring of cellular biochemistry during fermentation. PMID:25582569

  11. 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

  12. Ultrasound-Enhanced Attenuated Total Reflection Mid-infrared Spectroscopy In-Line Probe: Acquisition of Cell Spectra in a Bioreactor

    PubMed Central

    2015-01-01

    This article presents a novel method for selective acquisition of Fourier transform infrared (FT-IR) spectra of microorganisms in-line during fermentation, using Saccharomyces cerevisiae as an example. The position of the cells relative to the sensitive region of the attenuated total reflection (ATR) FT-IR probe was controlled by combing a commercially available ATR in-line probe with contact-free, gentle particle manipulation by ultrasonic standing waves. A prototype probe was successfully constructed, assembled, and tested in-line during fed-batch fermentations of S. cerevisiae. Control over the position of the cells was achieved by tuning the ultrasound frequency: 2.41 MHz was used for acquisition of spectra of the cells (pushing frequency fp) and 1.87 MHz, for retracting the cells from the ATR element, therefore allowing spectra of the medium to be acquired. Accumulation of storage carbohydrates (trehalose and glycogen) inside the cells was induced by a lack of a nitrogen source in the feed medium. These changes in biochemical composition were visible in the spectra of the cells recorded in-line during the application of fp and could be verified by reference spectra of dried cell samples recorded off-line with a FT-IR microscope. Comparison of the cell spectra with spectra of trehalose, glycogen, glucose, and mannan, i.e., the major carbohydrates present in S. cerevisiae, and principal components analysis revealed that the changes observed in the cell spectra correlated well with the bands specific for trehalose and glycogen. This proves the applicability and capability of ultrasound-enhanced in-line ATR mid-IR spectroscopy as a real-time PAT method for the in situ monitoring of cellular biochemistry during fermentation. PMID:25582569

  13. 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

    2016-01-01

    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

  14. Kinetic modeling of dissolution and crystallization of slurries with attenuated total reflectance UV-visible absorbance and near-infrared reflectance measurements.

    PubMed

    Hsieh, Chun H; Billeter, Julien; McNally, Mary Ellen P; Hoffman, Ronald M; Gemperline, Paul J

    2013-06-01

    Slurries are often used in chemical and pharmaceutical manufacturing processes but present challenging online measurement and monitoring problems. In this paper, a novel multivariate kinetic modeling application is described that provides calibration-free estimates of time-resolved profiles of the solid and dissolved fractions of a substance in a model slurry system. The kinetic model of this system achieved data fusion of time-resolved spectroscopic measurements from two different kinds of fiber-optic probes. Attenuated total reflectance UV-vis (ATR UV-vis) and diffuse reflectance near-infrared (NIR) spectra were measured simultaneously in a small-scale semibatch reactor. A simplified comprehensive kinetic model was then fitted to the time-resolved spectroscopic data to determine the kinetics of crystallization and the kinetics of dissolution for online monitoring and quality control purposes. The parameters estimated in the model included dissolution and crystal growth rate constants, as well as the dissolution rate order. The model accurately estimated the degree of supersaturation as a function of time during conditions when crystallization took place and accurately estimated the degree of undersaturation during conditions when dissolution took place. PMID:23565977

  15. Application of the Polynomial-Based Least Squares and Total Least Squares Models for the Attenuated Total Reflection Fourier Transform Infrared Spectra of Binary Mixtures of Hydroxyl Compounds.

    PubMed

    Shan, Peng; Peng, Silong; Zhao, Yuhui; Tang, Liang

    2016-03-01

    An analysis of binary mixtures of hydroxyl compound by Attenuated Total Reflection Fourier transform infrared spectroscopy (ATR FT-IR) and classical least squares (CLS) yield large model error due to the presence of unmodeled components such as H-bonded components. To accommodate these spectral variations, polynomial-based least squares (LSP) and polynomial-based total least squares (TLSP) are proposed to capture the nonlinear absorbance-concentration relationship. LSP is based on assuming that only absorbance noise exists; while TLSP takes both absorbance noise and concentration noise into consideration. In addition, based on different solving strategy, two optimization algorithms (limited-memory Broyden-Fletcher-Goldfarb-Shanno (LBFGS) algorithm and Levenberg-Marquardt (LM) algorithm) are combined with TLSP and then two different TLSP versions (termed as TLSP-LBFGS and TLSP-LM) are formed. The optimum order of each nonlinear model is determined by cross-validation. Comparison and analyses of the four models are made from two aspects: absorbance prediction and concentration prediction. The results for water-ethanol solution and ethanol-ethyl lactate solution show that LSP, TLSP-LBFGS, and TLSP-LM can, for both absorbance prediction and concentration prediction, obtain smaller root mean square error of prediction than CLS. Additionally, they can also greatly enhance the accuracy of estimated pure component spectra. However, from the view of concentration prediction, the Wilcoxon signed rank test shows that there is no statistically significant difference between each nonlinear model and CLS. PMID:26810185

  16. Total internal reflection photoacoustic spectroscopy for the detection of ?-hematin.

    PubMed

    Goldschmidt, Benjamin S; Sudduth, Amanda S M; Samson, Edward B; Whiteside, Paul J D; Bhattacharyya, Kiran D; Viator, John A

    2012-06-01

    Evanescent field sensing methods are currently used to detect many different types of disease markers and biologically important chemicals such as the HER2 breast cancer receptor. Hinoue et al. used Total Internal Reflection Photoacoustic Spectroscopy (TIRPAS) as a method of using the evanescent field to detect an optically opaque dye at a sample interface. Although their methods were successful at detecting dyes, the results at that time did not show a very practical spectroscopic technique, which was due to the less than typical sensitivity of TIRPAS as a spectroscopy modality given the low power (? 1 to 2 W) lasers being used. Contrarily, we have used an Nd:YAG laser with a five nanosecond pulse that gives peak power of 1 MW coupled with the TIRPAS system to increase the sensitivity of this technique for biological material sensing. All efforts were focused on the eventual detection of the optically absorbing material, hemozoin, which is created as a byproduct of a malarial infection in blood. We used an optically analogous material, ?-hematin, to determine the potential for detection in the TIRPAS system. In addition, four properties which control the sensitivity were investigated to increase understanding about the sensor's function as a biosensing method. PMID:22734742

  17. Around-the-objective total internal reflection fluorescence microscopy.

    PubMed

    Burghardt, Thomas P; Hipp, Andrew D; Ajtai, Katalin

    2009-11-10

    Total internal reflection fluorescence (TIRF) microscopy uses the evanescent field on the aqueous side of a glass/aqueous interface to selectively illuminate fluorophores within approximately 100 nm of the interface. Applications of the method include epi-illumination TIRF, where the exciting light is refracted by the microscope objective to impinge on the interface at incidence angles beyond critical angle, and prism-based TIRF, where exciting light propagates to the interface externally to the microscope optics. The former has higher background autofluorescence from the glass elements of the objective where the exciting beam is focused, and the latter does not collect near-field emission from the fluorescent sample. Around-the-objective TIRF, developed here, creates the evanescent field by conditioning the exciting laser beam to propagate through the submillimeter gap created by the oil immersion high numerical aperture objective and the glass coverslip. The approach eliminates background light due to the admission of the laser excitation to the microscopic optics while collecting near-field emission from the dipoles excited by the approximately 50 nm deep evanescent field. PMID:19904308

  18. Absolute position total internal reflection microscopy with an optical tweezer

    PubMed Central

    Liu, Lulu; Woolf, Alexander; Rodriguez, Alejandro W.; Capasso, Federico

    2014-01-01

    A noninvasive, in situ calibration method for total internal reflection microscopy (TIRM) based on optical tweezing is presented, which greatly expands the capabilities of this technique. We show that by making only simple modifications to the basic TIRM sensing setup and procedure, a probe particle’s absolute position relative to a dielectric interface may be known with better than 10 nm precision out to a distance greater than 1 μm from the surface. This represents an approximate 10× improvement in error and 3× improvement in measurement range over conventional TIRM methods. The technique’s advantage is in the direct measurement of the probe particle’s scattering intensity vs. height profile in situ, rather than relying on assumptions, inexact system analogs, or detailed knowledge of system parameters for calibration. To demonstrate the improved versatility of the TIRM method in terms of tunability, precision, and range, we show our results for the hindered near-wall diffusion coefficient for a spherical dielectric particle. PMID:25512542

  19. Measurement uncertainty in Total Reflection X-ray Fluorescence

    NASA Astrophysics Data System (ADS)

    Floor, G. H.; Queralt, I.; Hidalgo, M.; Marguí, E.

    2015-09-01

    Total Reflection X-ray Fluorescence (TXRF) spectrometry is a multi-elemental technique using micro-volumes of sample. This work assessed the components contributing to the combined uncertainty budget associated with TXRF measurements using Cu and Fe concentrations in different spiked and natural water samples as an example. The results showed that an uncertainty estimation based solely on the count statistics of the analyte is not a realistic estimation of the overall uncertainty, since the depositional repeatability and the relative sensitivity between the analyte and the internal standard are important contributions to the uncertainty budget. The uncertainty on the instrumental repeatability and sensitivity factor could be estimated and as such, potentially relatively straightforward implemented in the TXRF instrument software. However, the depositional repeatability varied significantly from sample to sample and between elemental ratios and the controlling factors are not well understood. By a lack of theoretical prediction of the depositional repeatability, the uncertainty budget can be based on repeat measurements using different reflectors. A simple approach to estimate the uncertainty was presented. The measurement procedure implemented and the uncertainty estimation processes developed were validated from the agreement with results obtained by inductively coupled plasma - optical emission spectrometry (ICP-OES) and/or reference/calculated values.

  20. Data Analysis for Total Internal Reflection Fluorescence Microscopy.

    PubMed

    Asbury, Charles L

    2016-01-01

    In the microscopes we use to analyze total internal reflection fluorescence (TIRF), the emitted fluorescence is split chromatically, using dichroic filters, into either two or three different colors ("channels"). In our two-color instrument, the green emission wavelengths (405-488 nm; for imaging green fluorescent protein [GFP]-tagged proteins) and far-red emission wavelengths (650-800 nm; for imaging Alexa-647-labeled microtubules) are projected onto the upper and lower halves, respectively, of a single camera. A single filter can be swapped to collect near-red wavelengths (561-640 nm; for imaging mCherry, or Alexa-568-labeled microtubules) instead of far-red. Our three-color instrument is very similar except that the green, near-red, and far-red color ranges are projected onto three separate cameras. In either case, the different colors can be imaged simultaneously. Typically, we collect images at 10 frames/sec for ∼200 sec. We have developed a series of semiautomated image analysis programs, written in LabView, to obtain the brightness, residence time, and mobility of individual particles bound to single microtubules. The basic analysis steps are straightforward and could also be implemented using ImageJ or Matlab. For convenience, this protocol describes the analysis of a single microtubule. Data from many microtubules across many experimental trials are needed to obtain robust conclusions that are independent of stochastic and trial-to-trial variability. PMID:27140913

  1. Combined study of biphasic and zero-order release formulations with dissolution tests and ATR-FTIR spectroscopic imaging.

    PubMed

    Wray, Patrick; Li, Jing; Li, Ling Qiao; Kazarian, Sergei G

    2014-07-01

    In this study of multi-layer tablets, the dissolution of biphasic and zero-order release formulations has been studied primarily using attenuated total reflection-Fourier transform infrared (ATR-FTIR) spectroscopic imaging as well as UV-Vis detection of dissolved drug in the effluent stream and USP dissolution testing. Bilayer tablets, containing the excipients microcrystalline cellulose (MCC) and glucose, were used for biphasic release with nicotinamide and buflomedil as model drugs. ATR-FTIR spectroscopic imaging showed the changing component distributions during dissolution. Further experiments studied monolithic and barrier-layered tablets containing hydroxypropyl methylcellulose, MCC and buflomedil dissolving in a USP I apparatus. These data were compared with UV-Vis dissolution profiles obtained online with the ATR flow-through cell. ATR-FTIR imaging data of the biphasic formulations demonstrated that the drug release was affected by excipient ratios and effects such as interference between tablet sections. Tablets placed in the ATR-FTIR flow-through cell exhibited zero-order UV-Vis dissolution profile data at high flow rates, similar to barrier-layered formulations studied using the USP I apparatus. ATR-FTIR spectroscopic imaging provided information regarding the dissolution mechanisms in multi-layer tablets which could assist formulation development. The ability to relate data from USP dissolution tests with that from the ATR-FTIR flow-through cell could help spectroscopic imaging complement dissolution methods used in the industry. PMID:24801351

  2. Development of a method for the determination of Fusarium fungi on corn using mid-infrared spectroscopy with attenuated total reflection and chemometrics.

    PubMed

    Kos, Gregor; Lohninger, Hans; Krska, Rudolf

    2003-03-01

    A novel method, which enables the determination of fungal infection with Fusarium graminearum on corn within minutes, is presented. The ground sample was sieved and the particle size fraction between >250 and 100 microm was used for mid-infrared/attenuated total reflection (ATR) measurements. The sample was pressed onto the ATR crystal, and reproducible pressure was applied. After the spectra were recorded, they were subjected to principle component analysis (PCA) and classified using cluster analysis. Observed changes in the spectra reflected changes in protein, carbohydrate, and lipid contents. Ergosterol (for the total fungal biomass) and the toxin deoxynivalenol (DON; a secondary metabolite) of Fusarium fungi served as reference parameters, because of their relevance for the examination of corn based food and feed. The repeatability was highly improved by sieving prior to recording the spectra, resulting in a better clustering in PCA score/score plots. The developed method enabled the separation of samples with a toxin content of as low as 310 microg/kg from noncontaminated (blank) samples. Investigated concentration ranges were 880-3600 microg/kg for ergosterol and 310-2596 microg/kg for DON. The percentage of correctly classified samples was up to 100% for individual samples compared with a number of blank samples. PMID:12641243

  3. Quo Vadis total reflection X-ray fluorescence?

    NASA Astrophysics Data System (ADS)

    Pahlke, Siegfried

    2003-12-01

    The multielement trace analytical method 'total reflection X-ray fluorescence' (TXRF) has become a successfully established method in the semiconductor industry, particularly, in the ultra trace element analysis of silicon wafer surfaces. TXRF applications can fulfill general industrial requirements on daily routine of monitoring wafer cleanliness up to 300 mm diameter under cleanroom conditions. Nowadays, TXRF and hyphenated TXRF methods such as 'vapor phase decomposition (VPD)-TXRF', i.e. TXRF with a preceding surface and acid digestion and preconcentration procedure, are automated routine techniques ('wafer surface preparation system', WSPS). A linear range from 10 8 to 10 14 [atoms/cm 2] for some elements is regularly controlled. Instrument uptime is higher than 90%. The method is not tedious and can automatically be operated for 24 h/7 days. Elements such as S, Cl, K, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Br, Sn, Sb, Ba and Pb are included in the software for standard peak search. The detection limits of recovered elements are between 1×10 11 and 1×10 7 [atoms/cm 2] depending upon X-ray excitation energy and the element of interest. For the determination of low Z elements, i.e. Na, Al and Mg, TXRF has also been extended but its implementation for routine analysis needs further research. At present, VPD-TXRF determination of light elements is viable in a range of 10 9 [atoms/cm 2]. Novel detectors such as silicon drift detectors (SDD) with an active area of 5 mm 2, 10 mm 2 or 20 mm 2, respectively, and multi-array detectors forming up to 70 mm 2 are commercially available. The first SDD with 100 mm 2 (!) area and integrated backside FET is working under laboratory conditions. Applications of and comparison with ICP-MS, HR-ICP-MS and SR-TXRF, an extension of TXRF capabilities with an extremely powerful energy source, are also reported.

  4. Comparison of direct-total-reflection X-ray fluorescence, sweeping-total-reflection X-ray fluorescence and vapor phase decomposition-total-reflection X-ray fluorescence applied to the characterization of metallic contamination on semiconductor wafers

    NASA Astrophysics Data System (ADS)

    Danel, Adrien; Cabuil, Nicolas; Lardin, Thierry; Despois, Dominique; Veillerot, Marc; Geoffroy, Charles; Yamagami, Motoyuki; Kohno, Hiroshi

    2008-12-01

    The issues related to the matching between the 3 modes of Total-reflection X-Ray Fluorescence available on the latest generation of commercial equipment: Direct-Total-reflection X-Ray Fluorescence, Sweeping-Total-reflection X-Ray Fluorescence and Vapor Phase Decomposition-Total-reflection X-Ray Fluorescence, are discussed for quantitative analysis of metallic contamination on Si wafers. Direct-Total-reflection X-Ray Fluorescence and Sweeping-Total-reflection X-Ray Fluorescence agrees very well (+/- 20% for light elements, transition metals and heavy metals), but due to a poor surface coverage with Direct-Total-reflection X-Ray Fluorescence, the matching is correct on a whole wafer only for uniform contaminations. Vapor Phase Decomposition-Total-reflection X-Ray Fluorescence might agree with other Total-reflection X-Ray Fluorescence modes only if the collection of contaminants following the oxide decomposition step is 100% completed. This is not achieved for 2 situations: noble metals which plate on bare Si, and solid particles partially digested during the Vapor Phase Decomposition and collection protocol. Furthermore, even if the collection of contaminants is well completed, quantification after Vapor Phase Decomposition depends on the shape of the dried residues and the Total-reflection X-Ray Fluorescence incident angle. With the incident angle selected to maximize the signal to noise ratio for ultra trace applications, i.e. about 0.5 times the Si critical angle, an increase of the quantification by a factor up to 10 is often seen after Vapor Phase Decomposition because of particle-like shape of the metals against film-like shape for the initial distribution. Taking into account advantages and drawbacks of each Total-reflection X-Ray Fluorescence mode, a proposal for the use of Total-reflection X-Ray Fluorescence in advanced Integrated Circuit manufacturing is given and illustrated by practical results from a R&D pilot line and a mass production plant.

  5. Oxidation of carbon monoxide at a platinum film electrode studied by Fourier transform infrared spectroscopy with attenuated total reflection technique

    SciTech Connect

    Zhu, Yimin; Uchida, Hiroyuki; Watanabe, Masahiro

    1999-12-07

    Fourier transform infrared reflection absorption spectroscopy with the attenuated total reflection technique (ATR-FTIR), coupled with cyclic voltammetry (CV) measurement, is used to observe the oxidation process of adsorbed CO at Pt film sputtered on a silicon prism. The interesting bipolar shape of the linearly bonded CO band is observed at high coverage of CO, although no CO band is included in the reference spectrum. This asymmetric shape is ascribed to Fano resonance. In addition to a linear CO and bridged CO, a new absorption band presumably assigned to a carboxyl radical, was detected. This band may be formed by a heterogeneous reaction between adsorbed CO and H{sub 2}O on the Pt surface in the hydrogen adsorption potential region. The adsorbed carboxyl radical was oxidized at a less positive potential than the adsorbed CO, which can be ascribed to a presumable origin for the pre-peak that appeared in a CV reading prior to the oxidation of such a linear or bridged CO. This oxidation led to the rearrangement of CO ad-layers, especially at high coverage of CO. In the case of the low coverage of CO, the conversion from the bridged CO to the linear CO is ascribed to the potential induced electronic effects of the electrode surface on the adsorption states. A consumption of adsorbed H{sub 2}O and a production of CO{sub 2} were also clearly indicated by the spectroscopy when COOH of CO disappeared from the surface.

  6. Determination of detector rotation angle in the experiment based on the total internal reflection using an equilateral right angle prism

    NASA Astrophysics Data System (ADS)

    Hendro, Viridi, S.; Pratama, Y.

    2015-04-01

    We present a relation between incident angle and rotation angle detector in the Total Internal Reflection (TIR) experiments when using a right angle prism. In the TIR method, the light coming toward the prism will experience reflection and out of the prism at a certain angle direction. Results of analysis of the geometry and Snell's law shows that the angular position of the detector is not only determined by the angle of incidence of light alone but also by the size of the prism and the detector position from the rotation axis of goniometer. The experimental results show relation between the angle of detector and angle of goniometer. When the prism rotated 45 °, position of goniometer detector is 2×45 °. However, when the prism rotated at an angle instead of 45 °, detector position µ is not always equal to twice the rotation angle goniometer ψ, so that this relationship needs to be corrected. This correction is also determined by the value of the refractive index of the prism is used. By knowing the relationship between detector position and the incident angle of light, this formulation can be used to control the position of the sample and the detector in the experiments based on ATR.

  7. Simultaneous probing of bulk liquid phase and catalytic gas-liquid-solid interface under working conditions using attenuated total reflection infrared spectroscopy

    SciTech Connect

    Meemken, Fabian; Müller, Philipp; Hungerbühler, Konrad; Baiker, Alfons

    2014-08-15

    Design and performance of a reactor set-up for attenuated total reflection infrared (ATR-IR) spectroscopy suitable for simultaneous reaction monitoring of bulk liquid and catalytic solid-liquid-gas interfaces under working conditions are presented. As advancement of in situ spectroscopy an operando methodology for gas-liquid-solid reaction monitoring was developed that simultaneously combines catalytic activity and molecular level detection at the catalytically active site of the same sample. Semi-batch reactor conditions are achieved with the analytical set-up by implementing the ATR-IR flow-through cell in a recycle reactor system and integrating a specifically designed gas feeding system coupled with a bubble trap. By the use of only one spectrometer the design of the new ATR-IR reactor cell allows for simultaneous detection of the bulk liquid and the catalytic interface during the working reaction. Holding two internal reflection elements (IRE) the sample compartments of the horizontally movable cell are consecutively flushed with reaction solution and pneumatically actuated, rapid switching of the cell (<1 s) enables to quasi simultaneously follow the heterogeneously catalysed reaction at the catalytic interface on a catalyst-coated IRE and in the bulk liquid on a blank IRE. For a complex heterogeneous reaction, the asymmetric hydrogenation of 2,2,2-trifluoroacetophenone on chirally modified Pt catalyst the elucidation of catalytic activity/enantioselectivity coupled with simultaneous monitoring of the catalytic solid-liquid-gas interface is shown. Both catalytic activity and enantioselectivity are strongly dependent on the experimental conditions. The opportunity to gain improved understanding by coupling measurements of catalytic performance and spectroscopic detection is presented. In addition, the applicability of modulation excitation spectroscopy and phase-sensitive detection are demonstrated.

  8. Simultaneous probing of bulk liquid phase and catalytic gas-liquid-solid interface under working conditions using attenuated total reflection infrared spectroscopy.

    PubMed

    Meemken, Fabian; Müller, Philipp; Hungerbühler, Konrad; Baiker, Alfons

    2014-08-01

    Design and performance of a reactor set-up for attenuated total reflection infrared (ATR-IR) spectroscopy suitable for simultaneous reaction monitoring of bulk liquid and catalytic solid-liquid-gas interfaces under working conditions are presented. As advancement of in situ spectroscopy an operando methodology for gas-liquid-solid reaction monitoring was developed that simultaneously combines catalytic activity and molecular level detection at the catalytically active site of the same sample. Semi-batch reactor conditions are achieved with the analytical set-up by implementing the ATR-IR flow-through cell in a recycle reactor system and integrating a specifically designed gas feeding system coupled with a bubble trap. By the use of only one spectrometer the design of the new ATR-IR reactor cell allows for simultaneous detection of the bulk liquid and the catalytic interface during the working reaction. Holding two internal reflection elements (IRE) the sample compartments of the horizontally movable cell are consecutively flushed with reaction solution and pneumatically actuated, rapid switching of the cell (<1 s) enables to quasi simultaneously follow the heterogeneously catalysed reaction at the catalytic interface on a catalyst-coated IRE and in the bulk liquid on a blank IRE. For a complex heterogeneous reaction, the asymmetric hydrogenation of 2,2,2-trifluoroacetophenone on chirally modified Pt catalyst the elucidation of catalytic activity/enantioselectivity coupled with simultaneous monitoring of the catalytic solid-liquid-gas interface is shown. Both catalytic activity and enantioselectivity are strongly dependent on the experimental conditions. The opportunity to gain improved understanding by coupling measurements of catalytic performance and spectroscopic detection is presented. In addition, the applicability of modulation excitation spectroscopy and phase-sensitive detection are demonstrated. PMID:25173281

  9. Simultaneous probing of bulk liquid phase and catalytic gas-liquid-solid interface under working conditions using attenuated total reflection infrared spectroscopy

    NASA Astrophysics Data System (ADS)

    Meemken, Fabian; Müller, Philipp; Hungerbühler, Konrad; Baiker, Alfons

    2014-08-01

    Design and performance of a reactor set-up for attenuated total reflection infrared (ATR-IR) spectroscopy suitable for simultaneous reaction monitoring of bulk liquid and catalytic solid-liquid-gas interfaces under working conditions are presented. As advancement of in situ spectroscopy an operando methodology for gas-liquid-solid reaction monitoring was developed that simultaneously combines catalytic activity and molecular level detection at the catalytically active site of the same sample. Semi-batch reactor conditions are achieved with the analytical set-up by implementing the ATR-IR flow-through cell in a recycle reactor system and integrating a specifically designed gas feeding system coupled with a bubble trap. By the use of only one spectrometer the design of the new ATR-IR reactor cell allows for simultaneous detection of the bulk liquid and the catalytic interface during the working reaction. Holding two internal reflection elements (IRE) the sample compartments of the horizontally movable cell are consecutively flushed with reaction solution and pneumatically actuated, rapid switching of the cell (<1 s) enables to quasi simultaneously follow the heterogeneously catalysed reaction at the catalytic interface on a catalyst-coated IRE and in the bulk liquid on a blank IRE. For a complex heterogeneous reaction, the asymmetric hydrogenation of 2,2,2-trifluoroacetophenone on chirally modified Pt catalyst the elucidation of catalytic activity/enantioselectivity coupled with simultaneous monitoring of the catalytic solid-liquid-gas interface is shown. Both catalytic activity and enantioselectivity are strongly dependent on the experimental conditions. The opportunity to gain improved understanding by coupling measurements of catalytic performance and spectroscopic detection is presented. In addition, the applicability of modulation excitation spectroscopy and phase-sensitive detection are demonstrated.

  10. Evaluating degradation of silk's fibroin by attenuated total reflectance infrared spectroscopy: Case study of ancient banners from Polish collections

    NASA Astrophysics Data System (ADS)

    Koperska, M. A.; Łojewski, T.; Łojewska, J.

    2015-01-01

    In this study a part of research where artificially aged model samples were used as a guideline to the mechanism of degradation is presented. In previous work Bombyx Mori silk samples were exposed to various environments such as different oxygen, water vapour and volatile organic products content, all at the temperature of 150 °C [11]. Based on those results gathered with by Attenuated Total Reflectance/Fourier Transform Infrared Spectroscopy (ATR-FTIR) the degradation estimators were proposed and classified as follows: Primary functional groups estimators EAmideI/II - intensity ratios of Amide I Cdbnd O stretching vibration to Amide II Nsbnd H in-plane bending and Csbnd N stretching vibrations A1620/A1514. ECOOH - band 1318 cm-1 integral to band integral of CH3 bending vibration band located at 1442 cm-1P1318/P1442. Secondary conformational estimators EcCdbndO2 - intensity ratios within Amide I Cdbnd O stretching vibration of parallel β-sheet to antiparallel β-sheet A1620/A1699. In this work estimators were verified against estimators calculated from spectra of silk samples from 8 museum objects: 3 from 19th, 2 from 18th, 1 from 17th and 2 from 16th century including 3 banners from the storage resources of the Wawel Royal Castle in Cracow, Poland.

  11. Identification of fungal phytopathogens using Fourier transform infrared-attenuated total reflection spectroscopy and advanced statistical methods

    NASA Astrophysics Data System (ADS)

    Salman, Ahmad; Lapidot, Itshak; Pomerantz, Ami; Tsror, Leah; Shufan, Elad; Moreh, Raymond; Mordechai, Shaul; Huleihel, Mahmoud

    2012-01-01

    The early diagnosis of phytopathogens is of a great importance; it could save large economical losses due to crops damaged by fungal diseases, and prevent unnecessary soil fumigation or the use of fungicides and bactericides and thus prevent considerable environmental pollution. In this study, 18 isolates of three different fungi genera were investigated; six isolates of Colletotrichum coccodes, six isolates of Verticillium dahliae and six isolates of Fusarium oxysporum. Our main goal was to differentiate these fungi samples on the level of isolates, based on their infrared absorption spectra obtained using the Fourier transform infrared-attenuated total reflection (FTIR-ATR) sampling technique. Advanced statistical and mathematical methods: principal component analysis (PCA), linear discriminant analysis (LDA), and k-means were applied to the spectra after manipulation. Our results showed significant spectral differences between the various fungi genera examined. The use of k-means enabled classification between the genera with a 94.5% accuracy, whereas the use of PCA [3 principal components (PCs)] and LDA has achieved a 99.7% success rate. However, on the level of isolates, the best differentiation results were obtained using PCA (9 PCs) and LDA for the lower wavenumber region (800-1775 cm-1), with identification success rates of 87%, 85.5%, and 94.5% for Colletotrichum, Fusarium, and Verticillium strains, respectively.

  12. Identification of fungal phytopathogens using Fourier transform infrared-attenuated total reflection spectroscopy and advanced statistical methods.

    PubMed

    Salman, Ahmad; Lapidot, Itshak; Pomerantz, Ami; Tsror, Leah; Shufan, Elad; Moreh, Raymond; Mordechai, Shaul; Huleihel, Mahmoud

    2012-01-01

    The early diagnosis of phytopathogens is of a great importance; it could save large economical losses due to crops damaged by fungal diseases, and prevent unnecessary soil fumigation or the use of fungicides and bactericides and thus prevent considerable environmental pollution. In this study, 18 isolates of three different fungi genera were investigated; six isolates of Colletotrichum coccodes, six isolates of Verticillium dahliae and six isolates of Fusarium oxysporum. Our main goal was to differentiate these fungi samples on the level of isolates, based on their infrared absorption spectra obtained using the Fourier transform infrared-attenuated total reflection (FTIR-ATR) sampling technique. Advanced statistical and mathematical methods: principal component analysis (PCA), linear discriminant analysis (LDA), and k-means were applied to the spectra after manipulation. Our results showed significant spectral differences between the various fungi genera examined. The use of k-means enabled classification between the genera with a 94.5% accuracy, whereas the use of PCA [3 principal components (PCs)] and LDA has achieved a 99.7% success rate. However, on the level of isolates, the best differentiation results were obtained using PCA (9 PCs) and LDA for the lower wavenumber region (800-1775  cm(-1)), with identification success rates of 87%, 85.5%, and 94.5% for Colletotrichum, Fusarium, and Verticillium strains, respectively. PMID:22352668

  13. Infrared spectroscopy with heated attenuated total internal reflectance enabling precise measurement of thermally induced transitions in complex biological polymers.

    PubMed

    Warren, Frederick J; Perston, Benjamin B; Royall, Paul G; Butterworth, Peter J; Ellis, Peter R

    2013-04-16

    We report an improved tool for acquiring temperature-resolved fourier transform infrared (FT-IR) spectra of complex polymer systems undergoing thermal transitions, illustrated by application to several phenomena related to starch gelatinization that have proved difficult to study by other means. Starch suspensions from several botanical origins were gelatinized using a temperature-controlled attenuated total reflectance (ATR) crystal, with IR spectra collected every 0.25 °C. By following the 995/1022 cm(-1) peak ratio, clear transitions occurring between 59 and 70 °C were observed, for which the midpoints could be determined accurately by sigmoidal fits. The magnitude of the change in peak ratio was found to be strongly correlated to the enthalpy of gelatinization as measured by differential scanning calorimetry (DSC, R(2) = 0.988). An important advantage of the technique, compared to DSC, is that the signal-to-noise ratio is not reduced when measuring very broad transitions. This has the potential to allow more precise determination of the gelatinization parameters of high-amylose starches, for which gelatinization may take place over several tens of °C. PMID:23461675

  14. High-Throughput Thermal Stability Analysis of a Monoclonal Antibody by Attenuated Total Reflection FT-IR Spectroscopic Imaging

    PubMed Central

    2014-01-01

    The use of biotherapeutics, such as monoclonal antibodies, has markedly increased in recent years. It is thus essential that biotherapeutic production pipelines are as efficient as possible. For the production process, one of the major concerns is the propensity of a biotherapeutic antibody to aggregate. In addition to reducing bioactive material recovery, protein aggregation can have major effects on drug potency and cause highly undesirable immunological effects. It is thus essential to identify processing conditions which maximize recovery while avoiding aggregation. Heat resistance is a proxy for long-term aggregation propensity. Thermal stability assays are routinely performed using various spectroscopic and scattering detection methods. Here, we evaluated the potential of macro attenuated total reflection Fourier transform infrared (ATR-FT-IR) spectroscopic imaging as a novel method for the high-throughput thermal stability assay of a monoclonal antibody. This chemically specific visualization method has the distinct advantage of being able to discriminate between monomeric and aggregated protein. Attenuated total reflection is particularly suitable for selectively probing the bottom of vessels, where precipitated aggregates accumulate. With focal plane array detection, we tested 12 different buffer conditions simultaneously to assess the effect of pH and ionic strength on protein thermal stability. Applying the Finke model to our imaging kinetics allowed us to determine the rate constants of nucleation and autocatalytic growth. This analysis demonstrated the greater stability of our immunoglobulin at higher pH and moderate ionic strength, revealing the key role of electrostatic interactions. The high-throughput approach presented here has significant potential for analyzing the stability of biotherapeutics as well as any other biological molecules prone to aggregation. PMID:25221926

  15. Chemical Functionalization of Germanium with Dextran Brushes for Immobilization of Proteins Revealed by Attenuated Total Reflection Fourier Transform Infrared Difference Spectroscopy.

    PubMed

    Schartner, Jonas; Hoeck, Nina; Gldenhaupt, Jrn; Mavarani, Laven; Nabers, Andreas; Gerwert, Klaus; Ktting, Carsten

    2015-07-21

    Protein immobilization studied by attenuated total reflection Fourier transform infrared (ATR-FT-IR) difference spectroscopy is an emerging field enabling the study of proteins at atomic detail. Gold or glass surfaces are frequently used for protein immobilization. Here, we present an alternative method for protein immobilization on germanium. Because of its high refractive index and broad spectral window germanium is the best material for ATR-FT-IR spectroscopy of thin layers. So far, this technique was mainly used for protein monolayers, which lead to a limited signal-to-noise ratio. Further, undesired protein-protein interactions can occur in a dense layer. Here, the germanium surface was functionalized with thiols and stepwise a dextran brush was generated. Each step was monitored by ATR-FT-IR spectroscopy. We compared a 70 kDa dextran with a 500 kDa dextran regarding the binding properties. All surfaces were characterized by atomic force microscopy, revealing thicknesses between 40 and 110 nm. To analyze the capability of our system we utilized N-Ras on mono-NTA (nitrilotriacetic acid) functionalized dextran, and the amount of immobilized Ras corresponded to several monolayers. The protein stability and loading capacity was further improved by means of tris-NTA for immobilization. Small-molecule-induced changes were revealed with an over 3 times higher signal-to-noise ratio compared to monolayers. This improvement may allow the observation of very small and so far hidden changes in proteins upon stimulus. Furthermore, we immobilized green fluorescent protein (GFP) and mCherry simultaneously enabling an analysis of the surface by fluorescence microscopy. The absence of a Frster resonance energy transfer (FRET) signal demonstrated a large protein-protein distance, indicating an even distribution of the protein within the dextran. PMID:26102158

  16. The influence of wetting and drying cycles on mid-infrared attenuated total-reflection spectra of quartz: understanding spectroscopy of disturbed soil

    NASA Astrophysics Data System (ADS)

    Karlowatz, Manfred; Aleksandrov, Alexandr; Orlando, Thomas; Cathcart, J. Michael; Mizaikoff, Boris

    2004-09-01

    Attenuated total reflection (ATR) spectroscopy is a well established optical technique investigating fundamental molecular vibrations in the mid-infrared (MIR) spectral regime for a wide variety of samples including liquids, thin films and powders. In the present study, first results simulating the influence of weathering processes on the spectral characteristics of soils are discussed. In particular, the effect of wetting and drying cycles on IR spectra of fine quartz (SiO2) powders has been investigated with ATR techniques. Resulting from a wetting and drying cycle, the sample spectra of quartz powders revealed significantly increased absorption intensities throughout the spectral region of interest (1400-600 cm-1). We hypothesize that this effect results from a higher packing density of the particles following the wetting procedure with the fines packed into interstitial spaces closer to the ATR waveguide surface. Moreover, a strong red shift of approx. 40 cm-1 of the absorption band assigned to asymmetric SiO4 stretching vibrations (1050 cm-1 to 1250 cm-1) could be observed. Both effects, increase in intensity and spectral shift, are reversed by mechanically disturbing the cemented powder after the wetting/drying cycle. Experiments with s- and p-polarized infrared radiation show similar (reversible) spectral shifts for this particular frequency range. It is expected that these findings will lead to better understanding of the spectral characteristics of soil in the mid-infrared spectral domain providing improved interpretation of data retrieved from disturbed soils e.g. potential landmine sites during hyperspectral imaging.

  17. ATR neutron spectral characterization

    SciTech Connect

    Rogers, J.W.; Anderl, R.A.

    1995-11-01

    The Advanced Test Reactor (ATR) at INEL provides intense neutron fields for irradiation-effects testing of reactor material samples, for production of radionuclides used in industrial and medical applications, and for scientific research. Characterization of the neutron environments in the irradiation locations of the ATR has been done by means of neutronics calculations and by means of neutron dosimetry based on the use of neutron activation monitors that are placed in the various irradiation locations. The primary purpose of this report is to present the results of an extensive characterization of several ATR irradiation locations based on neutron dosimetry measurements and on least-squares-adjustment analyses that utilize both neutron dosimetry measurements and neutronics calculations. This report builds upon the previous publications, especially the reference 4 paper. Section 2 provides a brief description of the ATR and it tabulates neutron spectral information for typical irradiation locations, as derived from the more historical neutron dosimetry measurements. Relevant details that pertain to the multigroup neutron spectral characterization are covered in section 3. This discussion includes a presentation on the dosimeter irradiation and analyses and a development of the least-squares adjustment methodology, along with a summary of the results of these analyses. Spectrum-averaged cross sections for neutron monitoring and for displacement-damage prediction in Fe, Cr, and Ni are given in section 4. In addition, section4 includes estimates of damage generation rates for these materials in selected ATR irradiation locations. In section 5, the authors present a brief discussion of the most significant conclusions of this work and comment on its relevance to the present ATR core configuration. Finally, detailed numerical and graphical results for the spectrum-characterization analyses in each irradiation location are provided in the Appendix.

  18. Total reflection X-ray photoelectron spectroscopy as a semiconductor lubricant elemental analysis method

    NASA Astrophysics Data System (ADS)

    Alshehabi, Abbas; Sasaki, Nobuharu; Kawai, Jun

    2015-12-01

    Photoelectron spectra from a typical hard disk storage media device (HDD) were measured at total reflection and non-total reflection at unburnished, acetone-cleaned, and argon-sputtered conditions. F, O, N, and C usually making the upper layer of a typical hard disk medium were detected. Enhancement of the photoelectron emission of the fluorocarbon lubricant was observed at total reflection. Pt and Co were only found by non-total X-ray photoelectron spectroscopy (XPS) because they are constituents of a deeper region than the top and interface regions. Argon-sputtered, ultrasonic acetone-cleaned, and unburnished top layers were compared at total and non-total reflection conditions. Total reflection X-ray photoelectron spectroscopy (TRXPS) is demonstrated to be a powerful tool for storage media lubrication layer chemical state analysis, reliable for industrial quality control application , and reproducible.

  19. Attenuated Total Reflectance-Fourier Transform Infrared Spectroscopy on Intact Dried Leaves of Sage (Salvia officinalis L.): Accelerated Chemotaxonomic Discrimination and Analysis of Essential Oil Composition.

    PubMed

    Gudi, Gennadi; Krähmer, Andrea; Krüger, Hans; Schulz, Hartwig

    2015-10-01

    Sage (Salvia officinalis L.) is cultivated worldwide for its aromatic leaves, which are used as herbal spice, and for phytopharmaceutical applications. Fast analytical strategies for essential oil analysis, performed directly on plant material, would reduce the delay between sampling and analytical results. This would enhance product quality by improving technical control of cultivation. The attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR) method described here provides a reliable calibration model for quantification of essential oil components [EOCs; R(2) = 0.96; root-mean-square error of cross-validation (RMSECV) = 0.249 mL 100 g(-1) of dry matter (DM); and range = 1.115-5.280 mL 100 g(-1) of DM] and main constituents [e.g., α-thujone/β-thujone; R(2) = 0.97/0.86; RMSECV = 0.0581/0.0856 mL 100 g(-1) of DM; and range = 0.010-1.252/0.005-0.893 mL 100 g(-1) of DM] directly on dried intact leaves of sage. Except for drying, no further sample preparation is required for ATR-FTIR, and the measurement time of less than 5 min per sample contrasts with the most common alternative of hydrodistillation followed by gas chromatography analysis, which can take several hours per sample. PMID:26360136

  20. Attenuated total reflection infrared studies of oleate and trioctylphosphine oxide ligand adsorption and exchange reactions on CdS quantum dot films.

    PubMed

    Young, Aidan G; Al-Salim, Najeh; Green, David P; McQuillan, A James

    2008-04-15

    Ligand exchange reactions at the surface of oleate- and trioctylphosphine oxide (TOPO)-capped CdS quantum dots have been studied with attenuated total reflection infrared (ATR-IR) spectroscopy, using thin films deposited from organic solvent suspensions. The oleate and trioctylphosphine capping ligands were found to form highly ordered and densely packed monolayers on the CdS surface. Adsorbed oleate is coordinated to CdS in a chelating bidentate manner through the carboxylate functional group, while adsorbed trioctylphosphine oxide is coordinated though the P=O functional group and appears to have numerous adsorption environments on the CdS surface. Exposure of such films to aqueous solution was found to cause partial delamination of the films from the ATR prism interface which was reversible upon redrying. Ligand exchange reactions on the oleate- and trioctylphosphine-capped CdS films were studied in situ at room temperature by allowing the films to be exposed to dilute aqueous solutions of thiol-containing ligands. Oleate and trioctylphosphine oxide are both strongly adsorbed to the CdS surface, and ligand exchange with monothiol-containing ligands has been found to be highly dependent upon experimental conditions, in particular pH, where exchange is only observed at solution pH where the exchanging ligand is uncharged. This is attributed to the inability of a charged ligand to penetrate the hydrophobic polymethylene layer on the CdS surface. PMID:18312011

  1. Fourier transform infrared attenuated total reflection analysis of human hair: comparison of hair from breast cancer patients with hair from healthy subjects.

    PubMed

    Lyman, Donald J; Murray-Wijelath, Jacqueline

    2005-01-01

    A comparative study of Fourier transform infrared attenuated total reflection (FTIR-ATR) spectra of 32 scalp and pubic hair samples from individuals diagnosed with breast cancer and those who were negative for breast cancer showed increases in the beta-sheet/disorder structures (relative to alpha-helix structures) and C-H lipid content of hair from breast cancer patients. Thus, the presence of breast cancer appears to alter the hair growth process, resulting in changes in the composition and conformation of cell membrane and matrix materials of hair fiber. These appear to be consistent with the changes observed in X-ray diffraction patterns for hair from breast cancer patients. A blind study of 12 additional hair samples using these FTIR-ATR spectral differences as markers correctly identified all four hair samples from cancer patients (100%). Two of these samples were from breast cancer patients. Of the remaining two samples analyzing positive for cancer, one was from a prostate cancer patient and one from a lung cancer patient. Thus, it appears that the mechanism that alters hair fiber synthesis in the three types of cancer may be similar. The blind study incorrectly identified as positive for cancer three hair samples from two apparently healthy individuals and one patient considered cured from prostate cancer. PMID:15720735

  2. Application of multivariate chemometric techniques for simultaneous determination of five parameters of cottonseed oil by single bounce attenuated total reflectance Fourier transform infrared spectroscopy.

    PubMed

    Talpur, M Younis; Kara, Huseyin; Sherazi, S T H; Ayyildiz, H Filiz; Topkafa, Mustafa; Arslan, Fatma Nur; Naz, Saba; Durmaz, Fatih; Sirajuddin

    2014-11-01

    Single bounce attenuated total reflectance (SB-ATR) Fourier transform infrared (FTIR) spectroscopy in conjunction with chemometrics was used for accurate determination of free fatty acid (FFA), peroxide value (PV), iodine value (IV), conjugated diene (CD) and conjugated triene (CT) of cottonseed oil (CSO) during potato chips frying. Partial least square (PLS), stepwise multiple linear regression (SMLR), principal component regression (PCR) and simple Beer׳s law (SBL) were applied to develop the calibrations for simultaneous evaluation of five stated parameters of cottonseed oil (CSO) during frying of French frozen potato chips at 170°C. Good regression coefficients (R(2)) were achieved for FFA, PV, IV, CD and CT with value of >0.992 by PLS, SMLR, PCR, and SBL. Root mean square error of prediction (RMSEP) was found to be less than 1.95% for all determinations. Result of the study indicated that SB-ATR FTIR in combination with multivariate chemometrics could be used for accurate and simultaneous determination of different parameters during the frying process without using any toxic organic solvent. PMID:25127621

  3. Origin identification of dried distillers grains with solubles using attenuated total reflection Fourier transform mid-infrared spectroscopy after in situ oil extraction.

    PubMed

    Vermeulen, Ph; Fernández Pierna, J A; Abbas, O; Dardenne, P; Baeten, V

    2015-12-15

    The ban on using processed animal proteins in feedstuffs led the feed sector to look for other sources of protein. Dried distillers grains with solubles (DDGS) could be considered as an important source in this regard. They are imported into Europe mainly for livestock feed. Identifying their origin is essential when labelling is missing and for feed safety, particularly in a crisis situation resulting from contamination. This study investigated applying attenuated total reflection Fourier transform mid-infrared spectroscopy (ATR-FT-MIR) to the oil fraction extracted from samples in situ in order to identify the origin of DDGS. The use of spectroscopic and chemometric tools enabled the botanical and geographical origins of DDGS, as well as the industrial process used to produce them, to be identified. The models developed during the study provided a classification higher than 95% using an external validation set. PMID:26190596

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

    USGS Publications Warehouse

    Washburn, Kathryn E.; Birdwell, Justin E.

    2013-01-01

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

  5. Visco-thermal effects in acoustic metamaterials: from total transmission to total reflection and high absorption

    NASA Astrophysics Data System (ADS)

    Molerón, Miguel; Serra-Garcia, Marc; Daraio, Chiara

    2016-03-01

    We theoretically and experimentally investigate visco-thermal effects on the acoustic propagation through metamaterials consisting of rigid slabs with subwavelength slits embedded in air. We demonstrate that this unavoidable loss mechanism is not merely a refinement, but that it plays a dominant role in the actual acoustic response of the structure. Specifically, in the case of very narrow slits, the visco-thermal losses avoid completely the excitation of Fabry-Perot resonances, leading to 100% reflection. This is exactly opposite to the perfect transmission predicted in the idealised lossless case. Moreover, for a wide range of geometrical parameters, there exists an optimum slit width at which the energy dissipated in the structure can be as high as 50%. This work provides a clear evidence that visco-thermal effects are necessary to describe realistically the acoustic response of locally resonant metamaterials.

  6. PUREX new substation ATR

    SciTech Connect

    Nelson, D.E.

    1997-05-12

    This document is the acceptance test report (ATR) for the New PUREX Main and Minisubstations. It covers the factory and vendor acceptance and commissioning test reports. Reports are presented for the Main 5 kV substation building, the building fire system, switchgear, and vacuum breaker; the minisubstation control building and switch gear; commissioning test; electrical system and loads inspection; electrical utilities transformer and cable; and relay setting changes based on operational experience.

  7. Simultaneous quantification of verbenalin and verbascoside in Verbena officinalis by ATR-IR and NIR spectroscopy.

    PubMed

    Schönbichler, S A; Bittner, L K H; Pallua, J D; Popp, M; Abel, G; Bonn, G K; Huck, C W

    2013-10-01

    Attenuated-total-reflectance infrared spectroscopy (ATR-IR) and near-infrared diffuse reflectance spectroscopy (NIR) in hyphenation with multivariate analysis was utilized to quantify verbenalin and verbascoside in Verbena officinalis. A new high performance liquid chromatography (HPLC) method as a reference was established and validated. For both vibrational spectroscopic methods test-set and cross validation were performed. Different data-pre-treatments like SNV, 1st and 2nd derivative were applied to remove systematic errors and were evaluated. Quality parameters obtained for the test-set validation revealed that ATR-IR (verbenalin: R(2)=0.94, RPD=4.23; verbascoside: R(2)=0.93, RPD=3.63) has advantages over NIR (verbenalin: R(2)=0.91, RPD=3.75; verbascoside: R(2)=0.80, RPD=2.35) in the given application. PMID:23810849

  8. Investigation on the adsorption characteristics of sodium benzoate and taurine on gold nanoparticle film by ATR-FTIR spectroscopy.

    PubMed

    Kumar, Naveen; Thomas, S; Tokas, R B; Kshirsagar, R J

    2014-01-24

    Fourier transform infrared (FTIR) spectroscopic studies of sodium benzoate and taurine adsorbed on gold nanoparticle (AuNp) film on silanised glass slides have been studied by attenuated total reflection technique (ATR). The surface morphology of the AuNp films has been measured by Atomic Force Microscopy. The ATR spectra of sodium benzoate and taurine deposited on AuNp film are compared with ATR spectra of their powdered bulk samples. A new red-shifted band appeared along with the symmetric and asymmetric stretches of carboxylate group of sodium benzoate leading to a broadening of the above peaks. Similar behavior is also seen in the case of symmetric and asymmetric stretches of sulphonate group of taurine. The results indicate presence of both chemisorbed and physisorbed layers of both sodium benzoate and taurine on the AuNp film with bottom layer chemically bound to AuNp through carboxylate and sulphonate groups respectively. PMID:24091347

  9. Investigation on the adsorption characteristics of sodium benzoate and taurine on gold nanoparticle film by ATR-FTIR spectroscopy

    NASA Astrophysics Data System (ADS)

    Kumar, Naveen; Thomas, S.; Tokas, R. B.; Kshirsagar, R. J.

    2014-01-01

    Fourier transform infrared (FTIR) spectroscopic studies of sodium benzoate and taurine adsorbed on gold nanoparticle (AuNp) film on silanised glass slides have been studied by attenuated total reflection technique (ATR). The surface morphology of the AuNp films has been measured by Atomic Force Microscopy. The ATR spectra of sodium benzoate and taurine deposited on AuNp film are compared with ATR spectra of their powdered bulk samples. A new red-shifted band appeared along with the symmetric and asymmetric stretches of carboxylate group of sodium benzoate leading to a broadening of the above peaks. Similar behavior is also seen in the case of symmetric and asymmetric stretches of sulphonate group of taurine. The results indicate presence of both chemisorbed and physisorbed layers of both sodium benzoate and taurine on the AuNp film with bottom layer chemically bound to AuNp through carboxylate and sulphonate groups respectively.

  10. Single-particle mineralogy of Chinese soil particles by the combined use of low-Z particle electron probe X-ray microanalysis and attenuated total reflectance-FT-IR imaging techniques.

    PubMed

    Malek, Md Abdul; Kim, Bowha; Jung, Hae-Jin; Song, Young-Chul; Ro, Chul-Un

    2011-10-15

    Our previous work on the speciation of individual mineral particles of micrometer size by the combined use of attenuated total reflectance FT-IR (ATR-FT-IR) imaging and a quantitative energy-dispersive electron probe X-ray microanalysis technique (EPMA), low-Z particle EPMA, demonstrated that the combined use of these two techniques is a powerful approach for looking at the single-particle mineralogy of externally heterogeneous minerals. In this work, this analytical methodology was applied to characterize six soil samples collected at arid areas in China, in order to identify mineral types present in the samples. The six soil samples were collected from two types of soil, i.e., loess and desert soils, for which overall 665 particles were analyzed on a single particle basis. The six soil samples have different mineralogical characteristics, which were clearly differentiated in this work. As this analytical methodology provides complementary information, the ATR-FT-IR imaging on mineral types, and low-Z particle EPMA on the morphology and elemental concentrations, on the same individual particles, more detailed information can be obtained using this approach than when either low-Z particle EPMA or ATR-FT-IR imaging techniques are used alone, which has a great potential for the characterization of Asian dust and mineral dust particles. PMID:21894905

  11. Molecular events in deliquescence and efflorescence phase transitions of sodium nitrate particles studied by Fourier transform infrared attenuated total reflection spectroscopy.

    PubMed

    Lu, Pei-Dong; Wang, Feng; Zhao, Li-Jun; Li, Wen-Xue; Li, Xiao-Hong; Dong, Jin-Ling; Zhang, Yun-Hong; Lu, Gao-Qing

    2008-09-14

    The NaNO(3) droplets with sizes of 1-5 microm generated from a nebulizer were deposited on a ZnSe substrate in a Fourier transform infrared attenuated total reflection (FTIR-ATR) chamber. After solidification of the droplets with dry N(2) gas passing through the chamber, the solid NaNO(3) particles were monitored by in situ FTIR-ATR spectra in cycles of deliquescence and efflorescence processes with varying relative humidities (RHs). With an increase in the RH, a dominant peak at approximately 3539 cm(-1), together with three relatively weak peaks at approximately 3400, approximately 3272, and approximately 3167 cm(-1), in the O-H stretching band of water was resolved by the high signal-to-noise ratio FTIR-ATR spectra. The dominant peak and the three relatively weak peaks were contributed by the water monomers and the aggregated water molecules adsorbed on the surfaces of solid NaNO(3) particles, respectively. When the RH approached approximately 72%, slightly lower than the deliquescence RH (74.5%), the band component at approximately 3400 cm(-1) became the main peak, indicating that the water monomers and the aggregated water molecules aggregated to form a thin water layer on the surfaces of solid NaNO(3) particles. A splitting of the nu(3)-NO(3)(-) band at 1363 and 1390 cm(-1) at the RH of approximately 72%, instead of the single nu(3)-NO(3)(-) band at 1357 cm(-1) for the initial solid NaNO(3), was observed. We suggested that this reflected a phase transition from the initial solid to a metastable solid phase of NaNO(3). The metastable solid phase deliquesced completely in the region from approximately 87% to approximately 96% RH according to the fact that the nu(3)-NO(3)(-) band showed two overlapping peaks at 1348 and 1405 cm(-1) similar to those of bulk NaNO(3) solutions. In the efflorescence process of the NaNO(3) droplets, the nu(1)-NO(3)(-) band presented a continuous blueshift from 1049 cm(-1) at approximately 77% RH to 1055 cm(-1) at approximately 36% RH, indicating the formation of contact ion pairs between Na(+) and NO(3)(-). Moreover, in the RH range from approximately 53% down to approximately 26%, two peaks at 836 and 829 cm(-1) were observed in the nu(2)-NO(3)(-) band region, demonstrating the coexistence of NaNO(3) solid particles and droplets. PMID:19044926

  12. Measuring Heterogeneous Reaction Rates with ATR-FTIR Spectroscopy to Evaluate Chemical Fates in an Atmospheric Environment: A Physical Chemistry and Environmental Chemistry Laboratory Experiment

    ERIC Educational Resources Information Center

    Roberts, Jason E.; Zeng, Guang; Maron, Marta K.; Mach, Mindy; Dwebi, Iman; Liu, Yong

    2016-01-01

    This paper reports an undergraduate laboratory experiment to measure heterogeneous liquid/gas reaction kinetics (ozone-oleic acid and ozone-phenothrin) using a flow reactor coupled to an attenuated total reflectance-Fourier transform infrared (ATR-FTIR) spectrometer. The experiment is specially designed for an upper-level undergraduate Physical…

  13. Electro-optical field sensor using single total internal reflection in electro-optical crystals

    NASA Astrophysics Data System (ADS)

    Kijima, K.; Abe, O.; Shimizu, A.; Nakamura, T.; Kono, H.; Hagihara, S.; Torikai, E.; Hori, H.

    2015-08-01

    A novel electro-optical radio frequency field sensor with simple structure and high sensitivity is realized using single total internal reflection in electro-optical crystals. Without employing any waveguide structures, the minimum detectable electric field strength of the total internal reflection electro-optical-sensor is estimated to 86.52 dB μV/m (21.18 mV/m) at a resolution band width of 100 Hz for a short interaction length.

  14. Nanocrystalline diamond sensor targeted for selective CRP detection: an ATR-FTIR spectroscopy study.

    PubMed

    Andersson, Per Ola; Viberg, Pernilla; Forsberg, Pontus; Nikolajeff, Fredrik; Österlund, Lars; Karlsson, Mikael

    2016-05-01

    Protein immobilization on functionalized fluorine-terminated nanocrystalline (NCD) films was studied by attenuated total reflection Fourier transform infrared (ATR-FTIR) spectroscopy using an immobilization protocol developed to specifically bind C-reactive protein (CRP). Using an ATR-FTIR spectroscopy method employing a force-controlled anvil-type configuration, three critical steps of the ex situ CRP immobilization were analyzed. First, the NCD surface was passivated by deposition of a copolymer layer consisting of polyethylene oxide and polypropylene oxide. Second, a synthetic modified polypeptide binder with high affinity to CRP was covalently attached to the polymeric film. Third, CRP dissolved in aqueous buffer in concentrations of 10-20 μg/mL was added on the functionalized NCD surface. Both the amide I and II bands, due to the polypeptide binder and CRP, were clearly observed in ATR-FTIR spectra. CRP amide I bands were extracted from difference spectra and yielded bands that agreed well with the reported amide I band of free (non-bonded) CRP in solution. Thus, our results show that CRP retains its secondary structure when it is attached to the polypeptide binders. Compared to previous IR studies of CRP in solution, about 200 times lower concentration was applied in the present study. Graphical Abstract Direct non-destructive ATR-FTIR analysis of C-reactive protein (CRP) selectively bound to functionalized nanocrystalline diamond (NCD) sensor surface. PMID:27007740

  15. Infrared ATR: a probe for cellular activation

    NASA Astrophysics Data System (ADS)

    Timlin, Jerilyn A.; Martin, Laura E.; Alam, M. Kathleen; Haaland, David M.; Garrison, Kristen; Lyons, C. Richard; Hjelle, Brian

    2002-02-01

    We employ infrared spectroscopy (IR) with attenuated total reflectance (ATR) as a sampling technique to monitor live and dried RAW cells (a murine macrophage cell line) during activation with g-interferon and lipopolysaccharide. By comparing the spectra of activated cells at various time points to the spectra of healthy control cells, we identify spectral bands associated with nucleic acids that are markers for the cell activation process. These spectral changes are slight and can be complicated with the normal metabolic changes that occur within cells. We will discuss the use of data pretreatment strategies to accurately correct for the contribution of the buffer to the live cell spectra. We find the standard background correction method inadequate for concentrated solutions of cells. Data presented shows the severe effect incorrect background subtraction has on the cell spectra. We report a more accurate correction for phosphate buffer spectral contribution using an interactive subtraction of the buffer spectrum. We will show classification of dried control and activated macrophage cell spectra using partial-least squares analysis with multiplicative scatter correction.

  16. Quantitative Total and Diffuse Reflectance Laboratory Measurements for Remote, Standoff, and Point Sensing

    SciTech Connect

    Blake, Thomas A.; Johnson, Timothy J.; Tonkyn, Russell G.; Forland, Brenda M.; Myers, Tanya L.; Brauer, Carolyn S.; Su, Yin-Fong

    2014-06-10

    Methods for making total and diffuse directional/hemispherical reflectance measurements in the shortwave to longwave infrared using an integrating sphere are described. The sphere is a commercial, off-the-shelf optical device with its sample port at the bottom, which is essential for examining powdered samples without using a cover glass. The reflectance spectra of recently-developed National Institute of Standards and Technology (NIST, USA) infrared reflectance standards have been measured using the sphere. Reflectance spectra of other materials such as Spectralon and Infragold were also measured. The relative systematic error for the total reflectance measurements is estimated to be on the order of 3%, and random measurement error for multiple samples of each material is on the order of 0.5%.

  17. High performance total internal reflection type optical switches in silicon-on-insulator

    NASA Astrophysics Data System (ADS)

    Thomson, D.; Knights, A. P.; Walters, D.; Mashanovich, G. Z.; Timotijevic, B.; Gardes, F. Y.; Reed, G. T.

    2007-02-01

    The requirement of a precise and controllable reflection interface in total internal reflection type optical switches is widely acknowledged. When these switches are based upon carrier injection such as those fabricated in silicon-oninsulator the ability to set up a precise reflection interface becomes difficult due to the diffusion of carriers. This diffusion of carriers across the reflection interface creates a refractive index gradient which is likely to cause the input light to be imperfectly reflected into the output port, which is obviously less efficient than reflection from a precise interface in terms of loss due to the absorption by the free carriers and the directivity of the reflected wave. In our work we propose the use of a barrier positioned along the reflection interface, and around a completely enclosed injection region to prevent diffusion of carriers, and therefore set up a precise reflection interface. The barrier will also improve the injection efficiency since the carriers are being injected into a much smaller volume. This will, in turn, lead to a reduced switching current and faster switching speeds. This paper reports the modeling of the device and predicts the bandwidth performance for one specific switch design.

  18. Monte Carlo simulation applied in total reflection x-ray fluorescence: Preliminary results

    SciTech Connect

    Meira, Luiza L. C.; Inocente, Guilherme F.; Vieira, Leticia D.; Mesa, Joel

    2013-05-06

    The X-ray Fluorescence (XRF) analysis is a technique for the qualitative and quantitative determination of chemical constituents in a sample. This method is based on detection of the characteristic radiation intensities emitted by the elements of the sample, when properly excited. A variant of this technique is the Total Reflection X-ray Fluorescence (TXRF) that utilizes electromagnetic radiation as excitation source. In total reflection of X-ray, the angle of refraction of the incident beam tends to zero and the refracted beam is tangent to the sample support interface. Thus, there is a minimum angle of incidence at which no refracted beam exists and all incident radiation undergoes total reflection. In this study, we evaluated the influence of the energy variation of the beam of incident x-rays, using the MCNPX code (Monte Carlo NParticle) based on Monte Carlo method.

  19. High-efficiency, high-dispersion diffraction gratings based on total internal reflection

    NASA Astrophysics Data System (ADS)

    Marciante, John R.; Raguin, Daniel H.

    2004-03-01

    We report a new class of high-dispersion immersed diffraction gratings for which the reflective nature of the diffraction is provided by the phenomenon of total internal reflection (TIR) regardless of grating tooth shape. Thus, the component can be fabricated from a single dielectric material and requires no metallic or dielectric film layers for high reflection diffraction efficiency. With the absence of metallic absorption, diffraction efficiencies of these TIR gratings can reach more than 99% for 15-20-nm spectral bandwidths, making them suitable for many laser-based technologies.

  20. Phylogeny of cultivated and wild wheat species using ATR-FTIR spectroscopy

    NASA Astrophysics Data System (ADS)

    Demir, Pinar; Onde, Sertac; Severcan, Feride

    2015-01-01

    Within the last decade, an increasing amount of genetic data has been used to clarify the problems inherent in wheat taxonomy. The techniques for obtaining and analyzing these data are not only cumbersome, but also expensive and technically demanding. In the present study, we introduce infrared spectroscopy as a method for a sensitive, rapid and low cost phylogenetic analysis tool for wheat seed samples. For this purpose, 12 Triticum and Aegilops species were studied by Attenuated Total Reflection-Fourier Transform Infrared (ATR-FTIR) spectroscopy. Hierarchical cluster analysis and principal component analysis clearly revealed that the lignin band (1525-1505 cm-1) discriminated the species at the genus level. However, the species were clustered according to their genome commonalities when the whole spectra were used (4000-650 cm-1). The successful differentiation of Triticum and its closely related genus Aegilops clearly demonstrated the power of ATR-FTIR spectroscopy as a suitable tool for phylogenetic research.

  1. Structure-Activity Relations In Enzymes: An Application Of IR-ATR Modulation Spectroscopy

    NASA Astrophysics Data System (ADS)

    Fringeli, Urs P.; Ahlstrom, Peter; Vincenz, Claudius; Fringeli, Marianna

    1985-12-01

    Relations between structure and specific activity in immobilized acetylcholinesterase (ACNE) have been studied by means of pH- and Ca++-modulation technique combined with attenuated total reflection (ATR) infrared (IR) spectroscopy and enzyme activity measurement. Periodic modulation of pH and Ca++-concentration enabled a periodic on-off switching of about 40% of the total enzyme activity. It was found that about 0.5 to 1% of the amino acids were involved in this process. These 15 to 30 amino acids assumed antiparallel pleated sheet structure in the inhibited state and random and/or helical structure in the activated state.

  2. Glancing incident MeV ion beams for total reflection PIXE (TPIXE) and RBS surface analysis

    NASA Astrophysics Data System (ADS)

    van Kan, J. A.; Vis, R. D.

    1996-06-01

    In a total reflection geometry at small incident angles ϕ (0-35 mrad), MeV proton and α beams were used to analyse Au and Cu layers on flat quartz substrates by detection of X-rays and backscattered protons. The reflected proton beams were detected as a function of incident angle ϕ. An improved model for theoretical X-ray yield calculations is developed. These calculations showed that a proton beam of 2.5 MeV will be totally reflected from a Au atomic surface layer at an incident angle smaller than 8 mrad. At these small angles the backscattered protons and α particles show a pattern which indicates atomic layer depth resolution.

  3. Measurement of the Longitudinal Shift of Radiation at Total Internal Reflection by Microwave Techniques

    ERIC Educational Resources Information Center

    Akylas, Victor; And Others

    1976-01-01

    Describes a method to experimentally determine the longitudinal shift of a microwave beam at total internal reflection. Suggests that the activity be incorporated into an undergraduate laboratory program due to its ease in set-up and clarity of results. (CP)

  4. Determination of trace elements in uranium oxide by Total Reflection X-ray Fluorescence spectrometry

    NASA Astrophysics Data System (ADS)

    Misra, N. L.; Singh Mudher, K. D.; Adya, V. C.; Rajeswari, B.; Venugopal, V.

    2005-07-01

    A study on the applicability of Total Reflection X-ray Fluorescence for the determination of multielements in trace amounts in U 3O 8 matrix has been made. The calibration of the Total Reflection X-ray Fluorescence spectrometer and the validation of the method were done using multielement standards. The trace elements present in U 3O 8 standards and samples were determined after separating the U matrix by solvent extraction using tri- n-butyl phosphate and trioctyl phosphine oxide as extractants. From the aqueous phase the elements K, Ca, Cr, Mn, Fe, Co, Ni, Cu, Zn, Br, Rb, Sr, Y, Zr, Pb and Ba, etc., were determined by Total Reflection X-ray Fluorescence using Ga as an internal standard. An intercomparison of the Total Reflection X-ray Fluorescence determined concentrations of the trace elements specific to nuclear fuel, e.g. Ca, Cr, Mn, Fe, Co, Ni, Cu, Zn in U 3O 8 standards/samples with certified concentrations for these elements in U 3O 8 standards and Inductively Coupled Plasma Atomic Emission Spectroscopy determined concentrations in real U 3O 8 samples was also made. The method shows a precision and accuracy better than 5% (1 σ) for most elements in concentration range of ng/mL with a sample size of 10 μL.

  5. Reconstruction of the net emission distribution from the total radiance distribution on a reflecting surface.

    PubMed

    Ruyten, W

    2001-01-01

    The problem is considered of reconstructing, from a measurement of the total radiance distribution on an emitting surface, the radiance distribution that would be observed in the absence of reflected radiation. An explicit solution of the implied inverse problem is derived for the case in which the reflective properties of the surface are given in terms of a bidirectional reflection distribution function. Also considered are the limiting cases of diffuse and specular reflection. Practical considerations are discussed for application of the theory to the nonintrusive and remote measurement of temperatures and pressures on concave surfaces, either by traditional radiometry or by the use of thermographic phosphors and temperature- and pressure-sensitive paints. PMID:11152000

  6. ATR-FTIR as a thickness measurement technique for hydrated polymer-on-polymer coatings.

    PubMed

    Kane, Sheryl R; Ashby, Paul D; Pruitt, Lisa A

    2009-11-01

    Hydrated polymer coatings on polymer substrates are common for many biomedical applications, such as tissue engineering constructs, contact lenses, and catheters. The thickness of the coatings can affect the mechanical behavior of the systems and the cellular response, but measuring the coating thickness can be quite challenging using conventional methods. We propose a new method, that is, attenuated total reflection Fourier transform infrared spectroscopy (ATR-FTIR) to determine the relative thickness, combined with atomic force microscopy to calibrate the ATR-FTIR measurements. This technique was successfully employed to determine the hydrated thickness of a series of crosslinked tetraglyme coatings on ultrahigh molecular weight polyethylene substrates intended to reduce wear of acetabular cups in total hip replacements. The hydrated coatings ranged from 30 to 200 nm thick and were accurately measured despite the relatively high root-mean-square (RMS) roughness of the substrates, 20-35 nm (peak-to-peak roughness 55-100 nm). The calibrated ATR-FTIR technique is a promising new method for measuring the thickness of many other polymer-on-polymer and hydrated coatings. PMID:19582857

  7. A versatile total internal reflection photometric detection cell for flow analysis.

    PubMed

    Ellis, Peter S; Gentle, Brady S; Grace, Michael R; McKelvie, Ian D

    2009-08-15

    A total internal reflection (TIR) flow-through cell that is highly tolerant of schlieren effects, has limited hydrodynamic dispersion and does not trap gas bubbles, and which is suitable for sensitive photometric measurements in flow analysis, is described. Light from an optical fibre is introduced into a short length of quartz capillary through the sidewall at an incident angle of ca. 53 degrees. Under this condition, incident light undergoes total internal reflection from the external air-quartz interface and is propagated by successive reflections from the external walls through the aqueous liquid core of the cell. Detection of the transmitted beam is enabled by intentionally introducing an optical coupling medium at a predetermined distance along the capillary wall, which allows the internally reflected light to be captured by a second optical fibre connected to a charge-couple device detector. This configuration embodies a number of the desirable features of a liquid core waveguide cell (i.e. total internal reflection), a multi-reflection (MR) flow cell (i.e. minimum susceptibility to schlieren effects, low hydrodynamic dispersion and little tendency to trap bubbles), and a conventional Z-cell (wide dynamic range). When employed with a flow injection system, a limit of detection of 2.0 microg PL(-1) was achieved for the determination of reactive phosphate using the TIR cell, compared with LOD values of 3.8 microg PL(-1) and 4.9 microg PL(-1) obtained using the MR and Z-cells with same manifold. The combined advantages of schlieren-tolerance and lack of bubble entrapment of the MR cell with the higher S/N ratio and wider dynamic range of a conventional Z-cell, make the TIR cell eminently useful for photometric measurements of samples with widely differing refractive indices. PMID:19576452

  8. Probabilistic fusion of ATR results

    SciTech Connect

    Simonson, K.M.

    1998-08-01

    The problem of combining multi-source information in applications related to automatic target recognition (ATR) is addressed. A mathematical approach is proposed for fusing the (possibly dependent) outputs of multiple ATR systems or algorithms. The method is derived from statistical principles, and the fused decision takes the form of an hypothesis test. The distribution of the test statistic is approximated as gamma, with parameters estimated from available training data. In a brief simulation study, the proposed method outperforms several alternative fusion techniques.

  9. HEATR project: ATR algorithm parallelization

    NASA Astrophysics Data System (ADS)

    Deardorf, Catherine E.

    1998-09-01

    High Performance Computing (HPC) Embedded Application for Target Recognition (HEATR) is a project funded by the High Performance Computing Modernization Office through the Common HPC Software Support Initiative (CHSSI). The goal of CHSSI is to produce portable, parallel, multi-purpose, freely distributable, support software to exploit emerging parallel computing technologies and enable application of scalable HPC's for various critical DoD applications. Specifically, the CHSSI goal for HEATR is to provide portable, parallel versions of several existing ATR detection and classification algorithms to the ATR-user community to achieve near real-time capability. The HEATR project will create parallel versions of existing automatic target recognition (ATR) detection and classification algorithms and generate reusable code that will support porting and software development process for ATR HPC software. The HEATR Team has selected detection/classification algorithms from both the model- based and training-based (template-based) arena in order to consider the parallelization requirements for detection/classification algorithms across ATR technology. This would allow the Team to assess the impact that parallelization would have on detection/classification performance across ATR technology. A field demo is included in this project. Finally, any parallel tools produced to support the project will be refined and returned to the ATR user community along with the parallel ATR algorithms. This paper will review: (1) HPCMP structure as it relates to HEATR, (2) Overall structure of the HEATR project, (3) Preliminary results for the first algorithm Alpha Test, (4) CHSSI requirements for HEATR, and (5) Project management issues and lessons learned.

  10. Hard x-ray nanofocusing using total-reflection zone plates

    NASA Astrophysics Data System (ADS)

    Takano, Hidekazu; Tsuji, Takuya; Matsumura, Atsuyuki; Sakka, Kenji; Tsusaka, Yoshiyuki; Kagoshima, Yasushi

    2016-01-01

    A total-reflection zone plate (TRZP), which is a reflective grating that generates a line focus of hard X-rays, was developed. Newly designed TRZPs, introducing a laminar grating concept, were fabricated with various zone parameters. The focusing performances with regard to the beam size and the diffraction efficiency were evaluated using synchrotron radiation X-rays of 10 keV energy. Although the beam sizes measured are insufficient in comparison with the ideal value, the maximum diffraction efficiency, measured at 20%, exceeds the limitations of conventional TRZPs based on a binary grating.

  11. Multivariate Analysis of Attenuated Total Reflection Fourier Transform Infrared (ATR FT-IR) Spectroscopic Data to Confirm Phase Partitioning in Methacrylate-Based Dentin Adhesive

    PubMed Central

    Ye, Qiang; Parthasarathy, Ranganathan; Abedin, Farhana; Laurence, Jennifer S.; Misra, Anil; Spencer, Paulette

    2014-01-01

    Water is ubiquitous in the mouths of healthy individuals and is a major interfering factor in the development of a durable seal between the tooth and composite restoration. Water leads to the formation of a variety of defects in dentin adhesives; these defects undermine the tooth-composite bond. Our group recently analyzed phase partitioning of dentin adhesives using high-performance liquid chromatography (HPLC). The concentration measurements provided by HPLC offered a more thorough representation of current adhesive performance and elucidated directions to be taken for further improvement. The sample preparation and instrument analysis using HPLC are, however, time-consuming and labor-intensive. The objective of this work was to develop a methodology for rapid, reliable, and accurate quantitative analysis of near-equilibrium phase partitioning in adhesives exposed to conditions simulating the wet oral environment. Analysis by Fourier transform infrared (FT-IR) spectroscopy in combination with multivariate statistical methods, including partial least squares (PLS) regression and principal component regression (PCR), were used for multivariate calibration to quantify the compositions in separated phases. Excellent predictions were achieved when either the hydrophobic-rich phase or the hydrophilic-rich phase mixtures were analyzed. These results indicate that FT-IR spectroscopy has excellent potential as a rapid method of detection and quantification of dentin adhesives that experience phase separation under conditions that simulate the wet oral environment. PMID:24359662

  12. An effective medium study of surface plasmon polaritons in nanostructured gratings using attenuated total reflection

    SciTech Connect

    Tyboroski, M. H.; Anderson, N. R.; Camley, R. E.

    2014-01-07

    Recent work studied surface plasmon resonances in structured materials by the method of attenuated total reflection using a prism on top of a metallic grating. That calculation considered Transverse Magnetic polarized radiation, involved an expansion in 121 Fourier modes, and found a number of interesting features. Many of these features were attributed to localized plasmons or other factors, which arise from a discrete structure. We use a simple effective medium theory to address the same problem, and find many of the same reflection features observed in the more complex calculation, indicating that localization is not an important factor. We also evaluate the possibility of using some of the new features in the reflection spectrum for bio-sensing and find that the sensitivity of the system to small changes in relative permittivity is increased compared to some standard methods.

  13. Super hydrophobic surface of polytetrafluoroethylene fabricated by picosecond laser and phenomenon of total internal reflection underwater

    NASA Astrophysics Data System (ADS)

    Jiang, Yijian; Cao, Wenshen; Zhao, Yan; Wu, Yan; Ji, Lingfei

    2015-03-01

    A groove-shaped array with average 25 μm interval, 25 μm wall thickness, 75 μm depth and a columnar array with average 30 μm side length, 25 μm interval, 43 μm depth are processed by 1064 nm picosecond laser on polytetrafluoroethylene (PTFE) surface at room temperature. The water contact angle of modified PTFE surface can reach 167°, which show super hydrophobic surface of PTFE is prepared. It is observed super hydrophobic surface reflects metal luster underwater through the glassware when super hydrophobic PTFE entirely immerses in pure water. The experiment conducts super hydrophobic surface will enhance intensity of reflection of visible light underwater, which is due to total internal reflection of super hydrophobic surface und erwater.

  14. Intra-Cavity Total Reflection For High Sensitivity Measurement Of Optical Properties

    DOEpatents

    Pipino, Andrew C. R.; Hudgens, Jeffrey W.

    1999-08-24

    An optical cavity resonator device is provided for conducting sensitive murement of optical absorption by matter in any state with diffraction-limited spatial resolution through utilization of total internal reflection within a high-Q (high quality, low loss) optical cavity. Intracavity total reflection generates an evanescent wave that decays exponentially in space at a point external to the cavity, thereby providing a localized region where absorbing materials can be sensitively probed through alteration of the Q-factor of the otherwise isolated cavity. When a laser pulse is injected into the cavity and passes through the evanescent state, an amplitude loss resulting from absorption is incurred that reduces the lifetime of the pulse in the cavity. By monitoring the decay of the injected pulse, the absorption coefficient of manner within the evanescent wave region is accurately obtained from the decay time measurement.

  15. Intra-Cavity Total Reflection For High Sensitivity Measurement Of Optical Properties

    DOEpatents

    Pipino, Andrew Charles Rule

    1999-11-16

    An optical cavity resonator device is provided for conducting sensitive murement of optical absorption by matter in any state with diffraction-limited spatial resolution through utilization of total internal reflection within a high-Q (high quality, low loss) optical cavity. Intracavity total reflection generates an evanescent wave that decays exponentially in space at a point external to the cavity, thereby providing a localized region where absorbing materials can be sensitively probed through alteration of the Q-factor of the otherwise isolated cavity. When a laser pulse is injected into the cavity and passes through the evanescent state, an amplitude loss resulting from absorption is incurred that reduces the lifetime of the pulse in the cavity. By monitoring the decay of the injected pulse, the absorption coefficient of manner within the evanescent wave region is accurately obtained from the decay time measurement.

  16. Polar magneto-optical effects in magnetoplasmonic thin films illuminated by attenuated total reflection

    NASA Astrophysics Data System (ADS)

    Yan, Cunji; Han, Li; Yang, Jinbo; Gu, Wenqi

    2014-09-01

    We investigate the polar magneto-optical Kerr effect as a function of the angle of incidence in Co/Au thin films under attenuated total reflection conditions. An experimental method is proposed to measure the intrinsic polar magneto-optical Kerr rotation of the magnetoplasmonic films while considering the influence of the glass Faraday magneto-optical effect. The experimental results demonstrate that the Kerr rotations of these films are greatly affected by a number of factors including the angle of incidence, the linear polarization of the incident light, and the film thickness. The results suggest that the polar magneto-optical activity is affected by the evanescent fields decaying inside the films; these fields arise not only from attenuated total reflection at the glass/metal interface but also from the surface plasmon polaritons at the metal/air interface. A close relationship between the magneto-optical activity and the electromagnetic field distribution within the magnetoplasmonic films is clearly revealed.

  17. Application of the Total Reflection X-ray Fluorescence technique to trace elements determination in tobacco

    NASA Astrophysics Data System (ADS)

    Martinez, T.; Lartigue, J.; Zarazua, G.; Avila-Perez, P.; Navarrete, M.; Tejeda, S.

    2008-12-01

    Many studies have identified an important number of toxic elements along with organic carcinogen molecules and radioactive isotopes in tobacco. In this work we have analyzed by Total Reflection X-Ray Fluorescence 9 brands of cigarettes being manufactured and distributed in the Mexican market. Two National Institute of Standards and Technology standards and a blank were equally treated at the same time. Results show the presence of some toxic elements such as Pb and Ni. These results are compared with available data for some foreign brands, while their implications for health are discussed. It can be confirmed that the Total Reflection X-Ray Fluorescence method provides precise (reproducible) and accuracy (trueness) data for 15 elements concentration in tobacco samples.

  18. Experimental observation of the Imbert-Fedorov transverse displacement after a single total reflection.

    PubMed

    Pillon, Frank; Gilles, Hervé; Girard, Sylvain

    2004-03-20

    We describe a simple experimental setup with which to observe the transverse shift--also known as the Imbert-Fedorov effect-that circularly or elliptically polarized optical beams undergo after a single total internal reflection on a dielectric plane. A comparison between a theoretical model based on the conservation of energy and experimental measurements shows good agreement simultaneously for longitudinal (Goos-Hänchen) and transverse (Imbert-Fedorov) displacements. PMID:15072036

  19. Determination of styrene-butadiene rubber composition by attenuated total internal reflection infrared spectroscopy

    NASA Astrophysics Data System (ADS)

    Orlov, A. S.; Kiselev, S. A.; Kiseleva, E. A.; Budeeva, A. V.; Mashukov, V. I.

    2013-03-01

    A rapid method for determining the composition of styrene-butadiene rubber using attenuated total internal reflection infrared spectroscopy was proposed. PMR and 13C NMR spectroscopy and infrared transmission spectroscopy were used as absolute techniques for determining the compositions of calibration samples. It was shown that the method was applicable to a wide range of styrene-butadiene rubbers, did not require additional sample preparation, and was easily reproducible.

  20. Quantitative measurement of permeabilization of living cells by terahertz attenuated total reflection

    NASA Astrophysics Data System (ADS)

    Grognot, Marianne; Gallot, Guilhem

    2015-09-01

    Using Attenuated Total Reflection imaging technique in the terahertz domain, we demonstrate non-invasive, non-staining real time measurements of cytoplasm leakage during permeabilization of epithelial cells by saponin. The terahertz signal is mostly sensitive to the intracellular protein concentration in the cells, in a very good agreement with standard bicinchoninic acid protein measurements. It opens the way to in situ real time dynamics of protein content and permeabilization in live cells.

  1. Application of total internal reflection microscopy for laser damage studies on fused silica

    SciTech Connect

    Sheehan, L. M., LLNL

    1997-12-01

    Damage studies show that the majority of damage on ultraviolet grade fused silica initiates at the front or rear surface. The grinding and polishing processes used to produce the optical surfaces of transparent optics play a key role in the development of defects which can ultimately initiate damage. These defects can be on or breaking through the surface or can be sub-surface damage. Total Internal Reflection Microscopy has been documented as a tool for revealing both sub-surface and surface defects in transparent materials. Images taken which compare both Total Internal Reflection Microscopy and Atomic Force Microscopy show that the observed defects can be less than one micron in size. Total Internal Reflection Microscopy has the added benefit of being able to observe large areas (1 square millimeter) with sub-micron detection. Both off-line and in-situ systems have been applied in the Lawrence Livermore National Laboratory`s damage laboratory in order to understand defects in the surface and subsurface of polished fused silica. There is a preliminary indication that TIRM quality can be related to the damage resistance. The in-situ microscope is coupled into a 355 run, 7.5 ns, 10 Hz Nd:YAG laser system in order to study damage occurring at localized scatter sites revealed with the Total Internal Reflection Microscopy method. The tests indicate damage initiating at observed artifacts which have many different morphologies and damage behaviors. Some of the scatter sites and damage morphologies revealed have been related back to the finishing process.

  2. Fourier transform infra-red spectroscopy using an attenuated total reflection probe to distinguish between Japanese larch, pine and citrus plants in healthy and diseased states

    NASA Astrophysics Data System (ADS)

    Gandolfo, D. S.; Mortimer, H.; Woodhall, J. W.; Boonham, N.

    2016-06-01

    FTIR spectroscopy coupled with an Attenuated Total Reflection (ATR) sampling probe has been demonstrated as a technique for detecting disease in plants. Spectral differences were detected in Japanese Larch (Larix kaempferi) infected with Phytophthora ramorum at 3403 cm-1 and 1730 cm-1, from pine (Pinus spp.) infected with Bursaphelenchus xylophilus at 1070 cm-1, 1425 cm-1, 1621 cm-1 and 3403 cm-1 and from citrus (Citrus spp.) infected with 'Candidatus liberibacter' at 960 cm-1, 1087 cm-1, 1109 cm-1, 1154 cm-1, 1225 cm-1, 1385 cm-1, 1462 cm-1, 1707 cm-1, 2882 cm-1, 2982 cm-1 and 3650 cm-1. A spectral marker in healthy citrus has been identified as Pentanone but is absent from the diseased sample spectra. This agrees with recent work by Aksenov, 2014. Additionally, the spectral signature of Cutin was identified in the spectra of Pinus spp. and Citrus spp. and is consistent with work by Dubis, 1999 and Heredia-Guerrero, 2014.

  3. Fourier transform infra-red spectroscopy using an attenuated total reflection probe to distinguish between Japanese larch, pine and citrus plants in healthy and diseased states.

    PubMed

    Gandolfo, D S; Mortimer, H; Woodhall, J W; Boonham, N

    2016-06-15

    FTIR spectroscopy coupled with an Attenuated Total Reflection (ATR) sampling probe has been demonstrated as a technique for detecting disease in plants. Spectral differences were detected in Japanese Larch (Larix kaempferi) infected with Phytophthora ramorum at 3403cm(-1) and 1730cm(-1), from pine (Pinus spp.) infected with Bursaphelenchus xylophilus at 1070cm(-1), 1425cm(-)1, 1621cm(-1) and 3403cm(-1) and from citrus (Citrus spp.) infected with 'Candidatus liberibacter' at 960cm(-1), 1087cm(-1), 1109cm(-1), 1154cm(-1), 1225cm(-1), 1385cm(-1), 1462cm(-1), 1707cm(-1), 2882cm(-1), 2982cm(-1) and 3650cm(-1). A spectral marker in healthy citrus has been identified as Pentanone but is absent from the diseased sample spectra. This agrees with recent work by Aksenov, 2014. Additionally, the spectral signature of Cutin was identified in the spectra of Pinus spp. and Citrus spp. and is consistent with work by Dubis, 1999 and Heredia-Guerrero, 2014. PMID:27054703

  4. Electrochemical oxidation of 2-propanol over platinum and palladium electrodes in alkaline media studied by in situ attenuated total reflection infrared spectroscopy.

    PubMed

    Okanishi, Takeou; Katayama, Yu; Ito, Ryota; Muroyama, Hiroki; Matsui, Toshiaki; Eguchi, Koichi

    2016-04-21

    The electrochemical oxidation of 2-propanol over Pt and Pd electrodes was evaluated in alkaline media. Linear sweep voltammograms (LSVs), chronoamperograms (CAs), and simultaneous time-resolved attenuated total reflection infrared (ATR-IR) spectra of both electrodes were obtained in a 0.25 M KOH solution containing 1 M 2-propanol. The onset potential of 2-propanol oxidation for Pt was lower than that for Pd in LSVs while the degree of performance degradation observed for Pd was significantly smaller than that observed for Pt in CAs. The main product of 2-propanol oxidation was acetone over both electrodes and, over Pt only, acetone produced was catalytically oxidized to the enolate ion, which was accumulated on the Pt surface, leading to significant performance degradation. Carbon dioxide and carbonate species (CO3(2-), HCO3(-)) were not observed during 2-propanol oxidation over both electrodes, indicating that the complete oxidation of 2-propanol to CO2 will be a minor reaction. PMID:27009749

  5. Adsorption of water and butanol in silicalite-1 film studied with in situ attenuated total reflectance-Fourier transform infrared spectroscopy.

    PubMed

    Farzaneh, Amirfarrokh; Zhou, Ming; Potapova, Elisaveta; Bacsik, Zoltán; Ohlin, Lindsay; Holmgren, Allan; Hedlund, Jonas; Grahn, Mattias

    2015-05-01

    Biobutanol produced by, e.g., acetone-butanol-ethanol (ABE) fermentation is a promising alternative to petroleum-based chemicals as, e.g., solvent and fuel. Recovery of butanol from dilute fermentation broths by hydrophobic membranes and adsorbents has been identified as a promising route. In this work, the adsorption of water and butanol vapor in a silicalite-1 film was studied using in situ attenuated total reflectance-Fourier transform infrared (ATR-FTIR) spectroscopy to better understand the adsorption properties of silicalite-1 membranes and adsorbents. Single-component adsorption isotherms were determined in the temperature range of 35-120 °C, and the Langmuir model was successfully fitted to the experimental data. The adsorption of butanol is very favorable compared to that of water. When the silicalite-1 film was exposed to a butanol/water vapor mixture with 15 mol % butanol (which is the vapor composition of an aqueous solution containing 2 wt % butanol, a typical concentration in an ABE fermentation broth, i.e., the composition of the gas obtained from gas stripping of an ABE broth) at 35 °C, the adsorption selectivity toward butanol was as high as 107. These results confirm that silicalite-1 quite selectively adsorbs hydrocarbons from vapor mixtures. To the best of our knowledge, this is the first comprehensive study on the adsorption of water and butanol in silicalite-1 from vapor phase. PMID:25871262

  6. Total internal reflection diffraction grating in conical mounting and its application in planar display

    NASA Astrophysics Data System (ADS)

    Liu, Yujie; Li, Wenqiang; Ding, Quanxin; Zhou, Jiawu

    2015-02-01

    Total internal reflection diffraction gratings in conical mounting, where the plane of incidence does not contain the grating vector, are investigated in this paper and the relevant conditions and parameters for such gratings are presented. These are then used to design total internal reflection diffraction gratings in conical mounting that the diffraction angle into the first order is equal to the incidence angle. The applications of such gratings in conical mounting to planar optics configurations, which have at least three gratings and one of them is total internal reflection diffraction grating in conical mounting, are discussed in detail. Also, the diffraction properties of all three gratings in this configuration, especially the grating period which is the most important parameter of gratings, are analyzed. The main condition, on which all the gratings in planar display configuration have the same grating periods, is presented based on theoretical analysis: the turning grating should be in 60 deg conical mounting. The configuration can be used to virtual display or wearable display.

  7. Application of total internal reflection microscopy for laser damage studies on fused silica

    NASA Astrophysics Data System (ADS)

    Sheehan, Lynn M.; Kozlowski, Mark R.; Camp, David W.

    1998-04-01

    Damage studies show that the majority of damage on UV grade fused silica initiates at the front or rear surface. The grinding and polishing processes used to produce the optical surfaces of transparent optics play a key role in the development of defects which can ultimately initiate damage. These defects can be on or breaking through the surface or can be sub-surface and surface defects in transparent materials. Images taken which compare both total internal reflection microscopy and atomic force microscopy show that the observed defects can be less than one micron in size. Total internal reflection microscopy has the added benefit of being able to observe large areas with sub-micron detection. Both off-line and in- situ systems have been applied in the Lawrence Livermore National Laboratory's damage laboratory in order to understand defects in the surface and subsurface of polished fused silica. There is a preliminary indication that TIRM quality can be related to the damage resistance. The in-situ microscope is coupled into a 355 nm, 7.5 ns, 10 Hz Nd:YAG laser system in order to study damage occurring at localized scatter sites revealed with the total internal reflection microscopy method. The tests indicate damage initiating at observed artifacts which have many different morphologies and damage behaviors. Some of the scatter sites and damage morphologies revealed have been related back to the finishing process.

  8. Using paint to investigate fires: an ATR-IR study of the degradation of paint samples upon heating.

    PubMed

    Roberts, Kelly; Almond, Matthew J; Bond, John W

    2013-03-01

    Fire investigation is a challenging area for the forensic investigator. The aim of this work was to use spectral changes to paint samples to estimate the temperatures to which a paint has been heated. Five paint samples (one clay paint, two car paints, one metallic paint, and one matt emulsion) have been fully characterized by a combination of attenuated total reflectance Fourier transform infrared (ATR-IR), Raman, X-ray fluorescence spectroscopy and powder X-ray diffraction. The thermal decomposition of these paints has been investigated by means of ATR-IR and thermal gravimetric analysis. Clear temperature markers are observed in the ATR-IR spectra namely: loss of ν(C = O) band, >300°C; appearance of water bands on cooling, >500°C; alterations to ν(Si-O) bands due to dehydration of silicate clays, >700°C; diminution of ν(CO3 ) and δ(CO3 ) modes of CaCO3 , >950°C. We suggest the possible use of portable ATR-IR for nondestructive, in situ analysis of paints. PMID:23278849

  9. FTIR-ATR spectroscopy applied to quality control of grape-derived spirits.

    PubMed

    Anjos, Ofélia; Santos, António J A; Estevinho, Letícia M; Caldeira, Ilda

    2016-08-15

    The Fourier transform infrared (FTIR) spectroscopic method with attenuated total reflectance (ATR) was used for predicting the alcoholic strength, the methanol, acetaldehyde and fusel alcohols content of grape-derived spirits. FTIR-ATR spectrum in the mid-IR region (4000-400cm(-1)) was used for the quantitative estimation by applying partial least square (PLS) regression models and the results were correlated with those obtained from reference methods. In the developed method, a cross-validation with 50% of the samples was used for PLS analysis along with a validation test set with 50% of the remaining samples. Good correlation models with a great accuracy were obtained for methanol (r(2)=99.4; RPD=12.8), alcoholic strength (r(2)=97.2; RPD=6.0), acetaldehyde (r(2)=98.2; RPD=7.5) and fusel alcohols (r(2) from 97.4 to 94.1; RPD from 6.2 to 4.1). These results corroborate the hypothesis that FTIR-ATR is a useful technique for the quality control of grape-derived spirits, whose practical application may improve the efficiency and quickness of the current laboratory analysis. PMID:27006210

  10. Fast determination of total ginsenosides content in ginseng powder by near infrared reflectance spectroscopy

    NASA Astrophysics Data System (ADS)

    Chen, Hua-cai; Chen, Xing-dan; Lu, Yong-jun; Cao, Zhi-qiang

    2006-01-01

    Near infrared (NIR) reflectance spectroscopy was used to develop a fast determination method for total ginsenosides in Ginseng (Panax Ginseng) powder. The spectra were analyzed with multiplicative signal correction (MSC) correlation method. The best correlative spectra region with the total ginsenosides content was 1660 nm~1880 nm and 2230nm~2380 nm. The NIR calibration models of ginsenosides were built with multiple linear regression (MLR), principle component regression (PCR) and partial least squares (PLS) regression respectively. The results showed that the calibration model built with PLS combined with MSC and the optimal spectrum region was the best one. The correlation coefficient and the root mean square error of correction validation (RMSEC) of the best calibration model were 0.98 and 0.15% respectively. The optimal spectrum region for calibration was 1204nm~2014nm. The result suggested that using NIR to rapidly determinate the total ginsenosides content in ginseng powder were feasible.

  11. Cation Bridging Studied by Specular Neutron Reflection

    PubMed Central

    2013-01-01

    The binding of an anionic surfactant onto an anionic surface by addition of divalent ions is reported based on experimental data from specular neutron reflection (NR) and attenuated total internal reflection IR spectroscopy (ATR-IR). Similar measurements using monovalent ions (sodium) do not show any evidence of such adsorption, even though the amount of surfactant can be much higher. This data is interpreted in terms of the so-called bridging mechanism of ion binding. PMID:23547891

  12. Design of an fMRI-compatible optical touch stripe based on frustrated total internal reflection.

    PubMed

    Jarrahi, Behnaz; Wanek, Johann

    2014-01-01

    Previously we developed a low-cost, multi-configurable handheld response system, using a reflective-type intensity modulated fiber-optic sensor (FOS) to accurately gather participants' behavioral responses during functional magnetic resonance imaging (fMRI). Inspired by the popularity and omnipresence of the fingertip-based touch sensing user interface devices, in this paper we present the design of a prototype fMRI-compatible optical touch stripe (OTS) as an alternative configuration. The prototype device takes advantage of a proven frustrated total internal reflection (FTIR) technique. By using a custom-built wedge-shaped optically transparent acrylic prism as an optical waveguide, and a plano-concave lens to provide the required light beam profile, the position of a fingertip touching the surface of the wedge prism can be determined from the deflected light beams that become trapped within the prism by total internal reflection. To achieve maximum sensitivity, the optical design of the wedge prism and lens were optimized through a series of light beam simulations using WinLens 3D Basic software suite. Furthermore, OTS performance and MRI-compatibility were assessed on a 3.0 Tesla MRI scanner running echo planar imaging (EPI) sequences. The results show that the OTS can detect a touch signal at high spatial resolution (about 0.5 cm), and is well suited for use within the MRI environment with average time-variant signal-to-noise ratio (tSNR) loss < 3%. PMID:25571103

  13. Development of thin-film total-reflection mirrors for the XUV FEL

    NASA Astrophysics Data System (ADS)

    Jacobi, Sandra; Wiesmann, Joerg; Steeg, Barbara; Feldhaus, Josef; Michaelsen, Carsten

    2001-12-01

    A free electron laser for the XUV spectral range is currently under test at the TESLA Test Facility at DESY. High gain has been demonstrated below 100nm wavelength, and it is expected that the FEL will provide intense, sub-picosecond radiation pulses with photon energies up to 200eV. Thin film optical elements required for this facility are currently being developed by the X-ray optics group of the GKSS research center near Hamburg. Sputter-deposited coatings have been prepared for the use as total reflection X-ray mirrors for FEL beam optics. Coatings of low Z elements with the lowest possible absorption and high reflectivity have been investigated. Silicon substrates have been coated with carbon using different deposition conditions. The films were investigated using the soft X-ray reflectometer at the HASYLAB beamline G1. The measurements show that the reflectivity of the films is typically 90% at energies below 200eV and a grazing incidence angle of 4 degrees. The optical constants of these coatings obtained from the reflectivity measurements and are in agreement with tabulated values. The deposition parameters have been optimized resulting in argon contamination free films with near-theoretical performance. Preliminary investigations concerning the heat resistance of the films were also carried out.

  14. Total-internal-reflection-based photomask for large-area photolithography

    NASA Astrophysics Data System (ADS)

    Hung, Shao-Kang; Lin, Kung-Hsuan; Chen, Cheng-Lung; Chou, Chen-Hsun; Lin, You-Chuan

    2016-05-01

    Photolithography has been widely implemented with a photomask in contact or in close proximity to the photoresist layer. The flatness of the substrates is a crucial factor to guarantee the quality of the entire patterned photoresist (PR) layer especially for large-area photolithography. However, some substrates, such as sapphire wafers, do not possess highly uniform thickness as silicon wafer does. In this work, we demonstrate that a flexible polydimethylsiloxane (PDMS) photomask with optical total-internal-reflection structure can effectively circumvent this problem for mass production. Different from conventional photomask that the light is blocked by the patterned reflective/absorbing materials, the distributions of light intensity on the PR is engineered by the geometric structure of the transparent PDMS photomask. We demonstrate that 4 in. patterned sapphire wafers can be successfully fabricated by using this PDMS photomask, which can be easily integrated into the present techniques in industry for mass production of substrates for GaN-based optoelectronic devices.

  15. Superresolution confocal technology for displacement measurements based on total internal reflection

    SciTech Connect

    Kuang Cuifang; Hao Xiang; Wang Tingting; Liu Xu; Ali, M. Yakut

    2010-10-15

    In order to achieve a higher axial resolution for displacement measurement, a novel method is proposed based on total internal reflection filter and confocal microscope principle. A theoretical analysis of the basic measurement principles is presented. The analysis reveals that the proposed confocal detection scheme is effective in enhancing the resolution of nonlinearity of the reflectance curve greatly. In addition, a simple prototype system has been developed based on the theoretical analysis and a series of experiments have been performed under laboratory conditions to verify the system feasibility, accuracy, and stability. The experimental results demonstrate that the axial resolution in displacement measurements is better than 1 nm in a range of 200 nm which is threefold better than that can be achieved using the plane reflector.

  16. Total internal reflection-based planar waveguide solar concentrator with symmetric air prisms as couplers.

    PubMed

    Xie, Peng; Lin, Huichuan; Liu, Yong; Li, Baojun

    2014-10-20

    We present a waveguide coupling approach for planar waveguide solar concentrator. In this approach, total internal reflection (TIR)-based symmetric air prisms are used as couplers to increase the coupler reflectivity and to maximize the optical efficiency. The proposed concentrator consists of a line focusing cylindrical lens array over a planar waveguide. The TIR-based couplers are located at the focal line of each lens to couple the focused sunlight into the waveguide. The optical system was modeled and simulated with a commercial ray tracing software (Zemax). Results show that the system used with optimized TIR-based couplers can achieve 70% optical efficiency at 50 × geometrical concentration ratio, resulting in a flux concentration ratio of 35 without additional secondary concentrator. An acceptance angle of ± 7.5° is achieved in the x-z plane due to the use of cylindrical lens array as the primary concentrator. PMID:25607295

  17. Total internal reflection fluorescence microscopy of intraflagellar transport in Tetrahymena thermophila.

    PubMed

    Jiang, Yu-Yang; Lechtreck, Karl; Gaertig, Jacek

    2015-01-01

    Live imaging has become a powerful tool in studies of ciliary proteins. Tetrahymena thermophila is an established ciliated model with well-developed genetic and biochemical approaches, but its large size, complex shape, and the large number of short and overlapping cilia, have made live imaging of ciliary proteins challenging. Here we describe a method that combines paralysis of cilia by nickel ions and total internal reflection microscopy for live imaging of fluorescent proteins inside cilia of Tetrahymena. Using this method, we quantitatively documented the intraflagellar transport in Tetrahymena. PMID:25837403

  18. Microplate-compatible total internal reflection fluorescence microscopy for receptor pharmacology

    NASA Astrophysics Data System (ADS)

    Chen, Minghan; Zaytseva, Natalya V.; Wu, Qi; Li, Min; Fang, Ye

    2013-05-01

    We report the use of total internal reflection fluorescence (TIRF) microscopy for analyzing receptor pharmacology and the development of a microplate-compatible TIRF imaging system. Using stably expressed green fluorescence protein tagged β2-adrenergic receptor as the reporter, we found that the activation of different receptors results in distinct kinetic signatures of the TIRF intensity of cells. These TIRF signatures closely resemble the characteristics of their respective label-free dynamic mass redistribution signals in the same cells. This suggests that TIRF in microplate can be used for profiling and screening drugs.

  19. Study of the interaction between HSA and oligo-DNA using total internal reflection ellipsometry

    NASA Astrophysics Data System (ADS)

    Jung, Y. W.; Byun, J. S.; Kim, Y. D.; Hemzal, D.; Humliček, J.

    2012-04-01

    Techniques of quantitative analysis are very important for studies of the interactions between bio-molecules in the field of biotechnology and drug development. The total internal reflection ellipsometry system (TIRE) is an attractive label-free procedure for the quantitative analysis of biomolecules because it combines the analytic ability of ellipsometry and the high surface sensitivity of surface plasmon resonance. In this work, we have used TIRE to study the optical properties of an aquatic monolayer of human serum albumin (HSA) and oligo-DNA. Also, we have monitored the adsorption and the interaction processes of protein layers.

  20. High-resolution total-internal-reflection fluorescence microscopy using periodically nanostructured glass slides.

    PubMed

    Sentenac, Anne; Belkebir, Kamal; Giovannini, Hugues; Chaumet, Patrick C

    2009-12-01

    We compare the performance of a total-internal-reflection fluorescence microscope under varying illumination and substrate conditions. The samples are deposited on a standard homogeneous glass slide or on a grating and illuminated by one or two interfering beams at various incident angles. A conjugate gradient with positivity a priori information is used to reconstruct the fluorophore density from the images. Numerical studies demonstrate that when the sample lies on an optimized grating, the lateral resolution of the microscope is greatly improved, up to fourfold, the best result being obtained when the grating is illuminated by two interfering beams. PMID:19956323

  1. Infrared total internal reflection spectroscopy of dimethylcadmium on chemically passivated silicon surfaces

    NASA Astrophysics Data System (ADS)

    Sanchez, Esaul; Shaw, Ping S.; O'Neill, James A.; Osgood, Richard M., Jr.

    1988-06-01

    The chemistry of dimethylcadmium (DMCd) on chemically passivated silicon surfaces is monitored through changes in the infrared spectra of the CH vibrational modes in both chemically and physically adsorbed molecules. Total internal reflection of the IR probe beam was employed to isolate the surface-molecule signal from that due to ambient gas-phase molecules. Excimer laser irradiation of the adsorbed DMCd at 248 nm under conditions appropriate for Cd film deposition resulted in changes in the observed spectra which indicate a high hydrocarbon content in the deposited metal layer.

  2. Three-dimensional characterization of tethered microspheres by total internal reflection fluorescence microscopy

    NASA Technical Reports Server (NTRS)

    Blumberg, Seth; Gajraj, Arivalagan; Pennington, Matthew W.; Meiners, Jens-Christian

    2005-01-01

    Tethered particle microscopy is a powerful tool to study the dynamics of DNA molecules and DNA-protein complexes in single-molecule experiments. We demonstrate that stroboscopic total internal reflection microscopy can be used to characterize the three-dimensional spatiotemporal motion of DNA-tethered particles. By calculating characteristic measures such as symmetry and time constants of the motion, well-formed tethers can be distinguished from defective ones for which the motion is dominated by aberrant surface effects. This improves the reliability of measurements on tether dynamics. For instance, in observations of protein-mediated DNA looping, loop formation is distinguished from adsorption and other nonspecific events.

  3. Frustrated total internal reflection and critical coupling in a thick plasmonic grating with narrow slits

    SciTech Connect

    Mattiucci, N.; D'Aguanno, G. E-mail: giuseppe.daguanno@us.army.mil; Bloemer, M. J.; Alù, A.

    2014-06-02

    We demonstrate the possibility of critical coupling through frustrated total internal reflection in a thick plasmonic grating below the first diffraction order. Differently from conventional approaches relying on the excitation of surface plasmon-polaritons, here we exploit the light coupling with the leaky modes supported by the grating. This mechanism entails a wide-angle coupling and effectively access spectral bands that would otherwise be difficult to probe using conventional plasmonic critical coupling techniques, such as the Otto configuration. Our finding may pave the way to efficient plasmonic bio-sensor devices.

  4. Synchrotron total reflection X-ray fluorescence at BL-16 microfocus beamline of Indus-2

    SciTech Connect

    Tiwari, M. K. Singh, A. K. Das, Gangadhar Chowdhury, Anupam Lodha, G. S.

    2014-04-24

    Determination of ultra trace elements is important in many disciplines both in basic and applied sciences. Numerous applications show their importance in medical science, environmental science, materials science, food processing and semiconductor industries and in maintaining the quality control of ultra pure chemicals and reagents. We report commissioning of a synchrotron based total reflection x-ray fluorescence (TXRF) facility on the BL-16 microfocus beamline of Indus-2. This paper describes the performance of the BL-16 TXRF spectrometer and the detailed description of its capabilities through examples of measured results.

  5. Synchrotron total reflection X-ray fluorescence at BL-16 microfocus beamline of Indus-2

    NASA Astrophysics Data System (ADS)

    Tiwari, M. K.; Singh, A. K.; Das, Gangadhar; Chowdhury, Anupam; Lodha, G. S.

    2014-04-01

    Determination of ultra trace elements is important in many disciplines both in basic and applied sciences. Numerous applications show their importance in medical science, environmental science, materials science, food processing and semiconductor industries and in maintaining the quality control of ultra pure chemicals and reagents. We report commissioning of a synchrotron based total reflection x-ray fluorescence (TXRF) facility on the BL-16 microfocus beamline of Indus-2. This paper describes the performance of the BL-16 TXRF spectrometer and the detailed description of its capabilities through examples of measured results.

  6. Quantitative imaging of cellular adhesion by total internal reflection holographic microscopy.

    PubMed

    Ash, William M; Krzewina, Leo; Kim, Myung K

    2009-12-01

    Total internal reflection (TIR) holographic microscopy uses a prism in TIR as a near-field imager to perform quantitative phase microscopy of cell-substrate interfaces. The presence of microscopic organisms, cell-substrate interfaces, adhesions, and tissue structures on the prism's TIR face causes relative index of refraction and frustrated TIR to modulate the object beam's evanescent wave phase front. We present quantitative phase images of test specimens such as Amoeba proteus and cells such as SKOV-3 and 3T3 fibroblasts. PMID:19956284

  7. Innovative light collimator with afocal lens and total internal reflection lens for daylighting system.

    PubMed

    Chen, Bo-Jian; Chen, Yin-Ti; Ullah, Irfan; Chou, Chun-Han; Chan, Kai-Cyuan; Lai, Yi-Lung; Lin, Chia-Ming; Chang, Cheng-Ming; Whang, Allen Jong-Woei

    2015-10-01

    This research presents a novel design of the collimator, which uses total internal reflection (TIR), convex, and concave lenses for the natural light illumination system (NLIS). The concept of the NLIS is to illuminate building interiors with natural light, which saves energy consumption. The TIR lens is used to collimate the light, and convex and concave lenses are used to converge the light to the required area. The results have shown that the efficiency in terms of achieving collimated light using the proposed collimator at the output of the light collector is better than that of a previous system without a collimator. PMID:26479648

  8. Total internal reflection Raman spectroscopy of barley leaf epicuticular waxes in vivo.

    PubMed

    Greene, Phillip R; Bain, Colin D

    2005-11-10

    The use of total internal reflection (TIR)-Raman spectroscopy to examine cuticular wax layers in vivo at the surface of barley leaves (Hordeum vulgare L. cultivar Pastoral) is demonstrated. The limited penetration depth (40 nm) of the evanescent wave compared to the thickness of the wax layer eliminates problems arising from fluorescence from underlying pigments. Epicuticular wax crystals are observed to be more crystalline than the amorphous wax layer, which is analysed after removal of the wax crystals by cellulose acetate stripping. Carotenoids are detected as trace species in the cuticular waxes. PMID:16198093

  9. Energy Flux and Density of Nonuniform Electromagnetic Waves with Total Reflection

    NASA Astrophysics Data System (ADS)

    Petrov, N. S.

    2014-07-01

    Analytic expressions are obtained for the energy flux and density of refracted nonuniform waves produced during total reflection at the boundary between two isotropic media for the general case of elliptically polarized incident light. The average values are determined as functions of the parameters of the adjoining media and the angle of incidence. The cases of linearly and circularly polarized incident waves are examined in detail. An explicit general expression relating the energy fl ux and density of these waves for arbitrarily polarized incident light is obtained.

  10. Total Internal Reflection Tomography (TIRT) for Three-Dimensional Sub-Wavelength Imaging

    NASA Technical Reports Server (NTRS)

    Fischer, David G.; Carney, P. Scott

    2002-01-01

    We will present a novel new form of near-field microscopy known as total internal reflection tomography (TIRT), which allows for true three-dimensional sub-wavelength imaging. It is based on recent theoretical advances regarding the fundamental interaction of light with sub-wavelength structures, as well as stable algorithms for the near-field inverse problem. We will discuss its theoretical underpinnings, as well describe current efforts at the NASA Glenn Research Center to implement a TIRT system for biofluid research.

  11. Attenuated total reflection design for in situ FT-IR spectroelectrochemical studies.

    PubMed

    Visser, H; Curtright, A E; McCusker, J K; Sauer, K

    2001-09-01

    A versatile spectroelectrochemical apparatus is introduced to study the changes in IR spectra of organic and inorganic compounds upon oxidation or reduction. The design is based on an attenuated total reflection device, which permits the study of a wide spectral range of 16,700 (600 nm)-250 cm(-1), with a small opaque region of 2250-1900 cm(-1). In addition, an IR data collection protocol is introduced to deal with electrochemically nonreversible background signals. This method is tested with ferrocene in acetonitrile; concentrations as low as 1 mM produce results that agree with those in the literature. PMID:11569833

  12. Reflection effects during the radiation sterilization of ultra high molecular weight polyethylene for total knee replacements.

    PubMed

    Barron, Declan; Birkinshaw, Colin; Collins, Maurice N

    2015-08-01

    Ultra high molecular weight polyethylene has been subject to γ irradiation whilst in contact with a stainless steel backing. This leads to reflection of the incident radiation and to backscattered electrons, both of which contribute to an effective increase in dose received. Radiation induced damage through scission of inter-lamellae tie chains results in an increase in crystallinity. At a nominal received dose of 100 kGy the effect of the metal backing is to increase crystallinity by approximately a third relative to the increase observed in materials irradiated in the absence of the backing. The metal backing induced reflections cause a bimodal recrystallization distribution giving rise to a more refined crystal population. As implant materials are subject to intermittent, but high, stress levels it is clearly of importance to examine how these reflection induced structural changes influence mechanical properties. Stress/strain results have indicated that subsequent yielding behavior is governed by the counteracting mechanisms of crystal growth and lamella reorganization mechanisms and in metal backed components the resulting morphological inhomogeneity may have important property consequences for wear induced failures in total knee replacement materials. PMID:25913607

  13. Application of transparent nanostructured electrodes for modulation of total internal reflection

    NASA Astrophysics Data System (ADS)

    Hrudey, P. C. P.; Martinuk, M. A.; Mossman, M. A.; van Popta, A. C.; Brett, M. J.; Dunbar, T. D.; Huizinga, J. S.; Whitehead, L. A.

    2007-09-01

    We present a novel method of modulating total internal reflection (TIR) from an optical surface using a solution of dye ions in combination with a nanostructured electrode. Previous work using the electrophoretic movement of pigment particles to modulate TIR was limited by agglomeration of the pigment over time. Dye ions do not suffer from this limitation, but because of their small size they have significantly smaller absorption cross-section per unit charge than pigment particles which are generally two orders of magnitude larger. This significantly limits the maximum absorption caused by electrostatic attraction of the ions to a transparent conductive electrode. This can be overcome by using a transparent conductive nanoporous thin film as the electrode in which the porosity increases the effective surface area, allowing more dye ions to move into the evanescent wave region near the nanoporous transparent electrode and thus substantially increases the amount of absorption. In this paper, we demonstrate the modulation of TIR by observing the time-dependent variation of the reflectance as the dye ions are moved into and out of the evanescent wave region. This approach may have applications in reflective displays and active diffractive devices.

  14. Modeling total and polarized reflectances of ice clouds: evaluation by means of POLDER and ATSR-2 measurements.

    PubMed

    Knap, Wouter H; Labonnote, Laurent C; Brogniez, Grard; Stammes, Piet

    2005-07-01

    Four ice-crystal models are tested by use of ice-cloud reflectances derived from Along Track Scanning Radiometer-2 (ATSR-2) and Polarization and Directionality of Earth's Reflectances (POLDER) radiance measurements. The analysis is based on dual-view ATSR-2 total reflectances of tropical cirrus and POLDER global-scale total and polarized reflectances of ice clouds at as many as 14 viewing directions. Adequate simulations of ATSR-2 total reflectances at 0.865 microm are obtained with model clouds consisting of moderately distorted imperfect hexagonal monocrystals (IMPs). The optically thickest clouds (tau > approximately 16) in the selected case tend to be better simulated by use of pure hexagonal monocrystals (PHMs). POLDER total reflectances at 0.670 microm are best simulated with columnar or platelike IMPs or columnar inhomogeneous hexagonal monocrystals (IHMs). Less-favorable simulations are obtained for platelike IHMs and polycrystals (POLYs). Inadequate simulations of POLDER total and polarized reflectances are obtained for model clouds consisting of PHMs. Better simulations of the POLDER polarized reflectances at 0.865 microm are obtained with IMPs, IHMs, or POLYs, although POLYs produce polarized reflectances that are systematically lower than most of the measurements. The best simulations of the polarized reflectance for the ice-crystal models assumed in this study are obtained for model clouds consisting of columnar IMPs or IHMs. PMID:16004054

  15. Total Reflection X-ray Fluorescence attachment module modified for analysis in vacuum

    NASA Astrophysics Data System (ADS)

    Wobrauschek, P.; Streli, C.; Kregsamer, P.; Meirer, F.; Jokubonis, C.; Markowicz, A.; Wegrzynek, D.; Chinea-Cano, E.

    2008-12-01

    Based on the design of the low cost Total Reflection X-Ray Fluorescence attachment module available since 1986 from Atominstitut (WOBRAUSCHEK-module) which can be attached to existing X-ray equipment, a new version was developed which allows the analysis of samples in vacuum. This design was in particular possible as the Peltier cooled light weight Silicon Drift Detector is following all adjustment procedures for total reflection as angle rotation and linear motion. The detector is mounted through a vacuum feed and O-ring tightening to the small vacuum chamber. The standard 30 mm round quartz, Si-wafer or Plexiglas reflectors are used to carry the samples. The reflectors are placed on the reference plane with the dried sample down looking facing in about 0.5 mm distance the up looking detector window. The reflectors are resting on 3 steel balls defining precisely the reference plane for the adjustment procedure. As the rotation axis of the module is in the plane of the reflector surface, angle dependent experiments can be made to distinguish between film and particulate type contamination of samples. Operating with a Mo anode at 50 kV and 40 mA with a closely attached multilayer monochromator and using a 10 mm 2 KETEK silicon drift detector with 8 ?m Be window, a sensitivity of 70 cps/ng for Rb was measured and detection limits of 2 pg were obtained.

  16. Minimally invasive identification of degraded polyester-urethane magnetic tape using attenuated total reflection Fourier transform infrared spectroscopy and multivariate statistics.

    PubMed

    Cassidy, Brianna M; Lu, Zhenyu; Fuenffinger, Nathan C; Skelton, Samantha M; Bringley, Eric J; Nguyen, Linhchi; Myrick, Michael L; Breitung, Eric M; Morgan, Stephen L

    2015-09-15

    Audio recordings are a significant component of the world's modern cultural history and are retained for future generations in libraries, archives, and museums. The vast majority of tapes contain polyester-urethane as the magnetic particle binder, the degradation of which threatens the playability and integrity of these often unique recordings. Magnetic tapes with stored historical data are degrading and need to be identified prior to digitization and/or preservation. We demonstrate the successful differentiation of playable and nonplayable quarter-inch audio tapes, allowing the minimally invasive triage of tape collections. Without such a method, recordings are put at risk during playback, which is the current method for identifying degraded tapes. A total of 133 quarter-inch audio tapes were analyzed by attenuated total reflectance Fourier transform-infrared spectroscopy (ATR FT-IR). Classification of IR spectra in regards to tape playability was accomplished using principal component analysis (PCA) followed by quadratic discriminant analysis (QDA) and K-means cluster analysis. The first principal component suggests intensities at the following wavenumbers to be representative of nonplayable tapes: 1730 cm(-1), 1700 cm(-1), 1255 cm(-1), and 1140 cm(-1). QDA and cluster analysis both successfully identified 93.78% of nonplayable tapes in the calibration set and 92.31% of nonplayable tapes in the test set. This application of IR spectra assessed with multivariate statistical analysis offers a path to greatly improve efficiency of audio tape preservation. This rapid, minimally invasive technique shows potential to replace the manual playback test, a potentially destructive technique, ultimately allowing the safe preservation of culturally valuable content. PMID:26275025

  17. Rapid determination of free fatty acids in poultry feed lipid extracts by SB-ATR FTIR spectroscopy.

    PubMed

    Sherazi, S T H; Mahesar, S A; Bhanger, M I; van de Voort, F R; Sedman, J

    2007-06-27

    A simple, rapid, and reproducible method has been developed for the quantitative determination of free fatty acid (FFA) content in lipids extracted from poultry feeds by Fourier transform infrared (FTIR) spectroscopy with the use of a single-bounce attenuated total reflectance (SB-ATR) accessory. An FTIR calibration curve was prepared by gravimetrically adding oleic acid (15-37%) to pure refined, bleached, and deodorized (RBD) canola oil and measuring the area of the COOH absorption band at 1710 cm-1. The oil from each of 12 poultry feed formulations was extracted using conventional Soxhlet extraction, and after evaporation of the solvent, the FFA content was determined by the conventional AOCS titrimetric procedure and by the SB-ATR/FTIR method. The SB-ATR/FTIR FFA predictions were related to those determined by the AOCS titrimetric method by linear regression, producing an R value of 0.999 and a SD of +/-0.28% FFA. Time-course spectra collected as lipids extracted into hexane indicated that a 15 min extraction was adequate to obtain a representative sample for FFA determination, with further extraction resulting in little, if any, change in the proportion of FFA in the lipid extract. Only a small volume of the hexane extract ( approximately 20 mL) yielded sufficient material for the SB-ATR/FTIR analysis. Thus, by shortening the extraction time and taking a small sample so as to reduce solvent removal time, the SB-ATR/FTIR procedure provides a very simple and rapid means of determining the FFA content of poultry feed lipids. PMID:17530766

  18. Bromine and bromide content in soils: Analytical approach from total reflection X-ray fluorescence spectrometry.

    PubMed

    Gallardo, Helena; Queralt, Ignasi; Tapias, Josefina; Candela, Lucila; Margui, Eva

    2016-08-01

    Monitoring total bromine and bromide concentrations in soils is significant in many environmental studies. Thus fast analytical methodologies that entail simple sample preparation and low-cost analyses are desired. In the present work, the possibilities and drawbacks of low-power total reflection X-ray fluorescence spectrometry (TXRF) for the determination of total bromine and bromide contents in soils were evaluated. The direct analysis of a solid suspension using 20 mg of fine ground soil (<63 μm) gave a 3.7 mg kg(-1) limit of detection for bromine which, in most cases, was suitable for monitoring total bromine content in soils (Br content range in soils = 5-40 mg kg(-1)). Information about bromide determination in soils is also possible by analyzing the Br content in water soil extracts. In this case, the TXRF analysis can be directly performed by depositing 10 μL of the internal standardized soil extract sample on a quartz glass reflector in a measuring time of 1500 s. The bromide limit of detection by this approach was 10 μg L(-1). Good agreement was obtained between the TXRF results for the total bromine and bromide determinations in soils and those obtained by other popular analytical techniques, e.g. energy dispersive X-ray fluorescence spectrometry (total bromine) and ionic chromatography (bromide). As a study case, the TXRF method was applied to study bromine accumulation in two agricultural soils fumigated with a methyl bromide pesticide and irrigated with regenerated waste water. PMID:27179429

  19. Transmission and total reflection of subhertz electromagnetic waves at the earth-atmosphere interface

    SciTech Connect

    Shiozawa, Toshiyuki

    2010-12-15

    For the purpose of providing for a theoretical background for the study of electromagnetic fields generated by precursory effects of earthquakes, the problem of transmission and total reflection at the earth-atmosphere interface is investigated in detail for a subhertz plane electromagnetic wave incident from the earth's crust. The term ''subhertz'' means 'below 1 Hz'. First, for the special case of normal incidence, the overall power transmission coefficient at the earth-atmosphere interface is found to take a maximum value at a definite frequency f{sub 0} which is inversely proportional to the square of the depth of a virtual hypocenter. A typical value of f{sub 0} falls around 0.01 Hz. For oblique incidence as well, this feature of the overall power transmission coefficient is retained except in the vicinity of the critical angle of incidence for the H-wave. At the critical angle of incidence, the power flow carried by a surface wave along the interface becomes anomalously large for the H-wave. However, over a wide range of angles of incidence greater than the critical angle, the power flow carried by the E-wave exceeds that carried by the H-wave by orders of magnitude. Finally, the energy conservation relations for the incident, reflected, and transmitted waves at the earth-atmosphere interface are discussed. For an incident wave coming from the earth's crust, the interactive power between the incident and reflected waves plays a crucial role for the conservation of energy at the interface.

  20. Characterization of amorphous carbon films as total-reflection mirrors for XUV free-electron lasers

    NASA Astrophysics Data System (ADS)

    Jacobi, Sandra; Steeg, Barbara; Wiesmann, Jorg; Stormer, Michael; Feldhaus, Josef; Bormann, R.'diger; Michaelsen, Carsten

    2002-12-01

    As part of the TESLA (TeV-Energy Superconducting Linear Accelerator) project a free electron laser (FEL) in the XUV (Extreme Ultra-Violet, (6-200 eV)) and X-ray (0.5-15 keV) range is being developed at DESY (Deutsches Elektronen Synchrotron, Hamburg). At the TESLA Test Facility (TTF) a prototype FEL has recently demonstrated maximum light amplification in the range of 80 nm to 120 nm. It is expected that the FEL will provide intense, sub-picosecond radiation pulses with photon energies up to 200 eV in the next development stage. In a joint project between DESY and GKSS, thin film optical elements with very high radiation stability, as required for FEL applications, are currently being developed. Sputter-deposited amorphous carbon coatings have been prepared for use as total reflection X-ray mirrors. The optical characterization of the mirrors has been carried out using the soft X-ray reflectometer at HASYLAB (Hamburger Synchrotronstrahlungslabor) beamline G1. The reflectivity of the carbon films at 2 deg incidence angle is close to the theoretical reflectivity of 95.6 %, demonstrating the high quality of the coatings. For comparison, layers produced by different methods (e.g. Chemical vapor deposition, Pulsed laser deposition) have been characterized as well. Annealing experiments have been performed to evaluate the thermal stability of the amorphous carbon films. Further investigations concerning the radiation stability of the X-ray mirrors have also been conducted. The mirrors were irradiated in the FELIS (Free Electron Laser-Interaction with Solids) experiment at the TTF-FEL. Microscopic investigations demonstrate that the carbon mirrors are fairly stable.

  1. Watch your step! A frustrated total internal reflection approach to forensic footwear imaging

    NASA Astrophysics Data System (ADS)

    Needham, J. A.; Sharp, J. S.

    2016-02-01

    Forensic image retrieval and processing are vital tools in the fight against crime e.g. during fingerprint capture. However, despite recent advances in machine vision technology and image processing techniques (and contrary to the claims of popular fiction) forensic image retrieval is still widely being performed using outdated practices involving inkpads and paper. Ongoing changes in government policy, increasing crime rates and the reduction of forensic service budgets increasingly require that evidence be gathered and processed more rapidly and efficiently. A consequence of this is that new, low-cost imaging technologies are required to simultaneously increase the quality and throughput of the processing of evidence. This is particularly true in the burgeoning field of forensic footwear analysis, where images of shoe prints are being used to link individuals to crime scenes. Here we describe one such approach based upon frustrated total internal reflection imaging that can be used to acquire images of regions where shoes contact rigid surfaces.

  2. Photothermal deflectometry enhanced by total internal reflection enables non-invasive glucose monitoring in human epidermis.

    PubMed

    Pleitez, M A; Hertzberg, O; Bauer, A; Seeger, M; Lieblein, T; Lilienfeld-Toal, H V; Mäntele, W

    2015-01-21

    We present TIR-PTD spectroscopy, an IR-pump/VIS-probe method for the measurement of IR absorption spectra by means of photothermal deflectometry (PTD) enhanced by total internal reflection (TIR). It overcomes the limitations of IR spectroscopy for the study of opaque samples and allows molecular fingerprinting of IR-active liquids or solids. Another important advantage of the presented approach over traditional IR spectroscopy methods is the ability to obtain IR information by means of VIS detection, which is generally much cheaper and easier to handle than IR detection. By application of mid-IR TIR-PTD spectroscopy on human skin in vivo, we are demonstrating the correlation between epidermal- and blood-glucose levels on a type 1 diabetic patient. PMID:25408951

  3. Nanoscale characterization of vesicle adhesion by normalized total internal reflection fluorescence microscopy.

    PubMed

    Cardoso Dos Santos, Marcelina; Vézy, Cyrille; Jaffiol, Rodolphe

    2016-06-01

    We recently proposed a straightforward fluorescence microscopy technique to study adhesion of Giant Unilamellar Vesicles. This technique is based on dual observations which combine epi-fluorescence microscopy and total internal reflection fluorescence (TIRF) microscopy: TIRF images are normalized by epi-fluorescence ones. By this way, it is possible to map the membrane/substrate separation distance with a nanometric resolution, typically ~20nm, with a maximal working range of 300-400nm. The purpose of this paper is to demonstrate that this technique is useful to quantify vesicle adhesion from ultra-weak to strong membrane-surface interactions. Thus, we have examined unspecific and specific adhesion conditions. Concerning unspecific adhesion, we have controlled the strength of electrostatic forces between negatively charged vesicles and various functionalized surfaces which exhibit a positive or a negative effective charge. Specific adhesion was highlighted with lock-and-key forces mediated by the well defined biotin/streptavidin recognition. PMID:26972045

  4. Determination of uranium in human urine by total reflection X-ray fluorescence

    NASA Astrophysics Data System (ADS)

    Zarkadas, Ch; Karydas, A. G.; Paradellis, T.

    2001-12-01

    Uranium has been classified as a toxic chemical. It affects the kidneys, with nephritis being the primarily chemically-induced effect in animals and humans. Intermediate-term studies on animals indicate that increased uranium doses are positively correlated with various biochemical effects and histopathological changes. Since the kidneys efficiently excrete in urine the major portion of solubilized uranium circulating in blood, an increased urinary uranium excretion can provide a sensitive quantitative measure of exposure, especially in the case of acute exposure. In the present work a method was developed for the quantitative determination of uranium in human urine. It combines the chemical treatment of urine, which results in a significant pre-concentration of uranium, with its subsequent detection by means of total reflection X-ray fluorescence (TXRF). The method has been proven to be relatively fast, offering detection limits that allow for monitoring uranium intake above normal levels.

  5. Analysis on the magnetic sensitivity in a total reflection prisms (TRP) ring resonator

    NASA Astrophysics Data System (ADS)

    Li, Dong; Zhao, Jianlin; Bi, Chao

    2015-07-01

    Based on the theory of transfer matrix and the condition of eigenmode self-reproduction, the model of the magnetic sensitivity in a total reflection prisms (TRP) ring laser resonator is established. Then the influences of the slight nonplanar effect on the output frequency difference and the magnetic sensitivity are analyzed theoretically and numerically. The results show that the slightly nonplanar effect will bring an additional ellipticity of the eigenmode and the environment magnetic field can produce an additional output frequency difference in a TRP ring laser resonator. It can also be found that the output frequency difference increases versus the augment of nonplanar angle and the intensity of magnetic field. These interesting results may be useful for designing and optimizing the structure of super high precision TRP ring laser gyroscopes.

  6. Imaging with total internal reflection fluorescence microscopy for the cell biologist

    PubMed Central

    Mattheyses, Alexa L.; Simon, Sanford M.; Rappoport, Joshua Z.

    2010-01-01

    Total internal reflection fluorescence (TIRF) microscopy can be used in a wide range of cell biological applications, and is particularly well suited to analysis of the localization and dynamics of molecules and events near the plasma membrane. The TIRF excitation field decreases exponentially with distance from the cover slip on which cells are grown. This means that fluorophores close to the cover slip (e.g. within ~100 nm) are selectively illuminated, highlighting events that occur within this region. The advantages of using TIRF include the ability to obtain high-contrast images of fluorophores near the plasma membrane, very low background from the bulk of the cell, reduced cellular photodamage and rapid exposure times. In this Commentary, we discuss the applications of TIRF to the study of cell biology, the physical basis of TIRF, experimental setup and troubleshooting. PMID:20971701

  7. Large tunable optical absorption of CVD graphene under total internal reflection by strain engineering.

    PubMed

    Dong, Bin; Wang, Peng; Liu, Zhi-Bo; Chen, Xu-Dong; Jiang, Wen-Shuai; Xin, Wei; Xing, Fei; Tian, Jian-Guo

    2014-11-14

    We have developed a method to tune polarization-dependent optical absorption of large-scale chemical vapor deposition (CVD) graphene under total internal reflection (TIR) by strain engineering. Through control of the strain direction, the optical absorption of graphene for transverse magnetic or transverse electric waves can be separately tuned. Strain-induced modulation of the optical absorption has been theoretically expected when light is normally incident through graphene. Under TIR, however, we experimentally observed a significant increase in the strain-induced tunability of optical absorption for CVD graphene, with the modulation efficiency of optical absorption in monolayer graphene increasing by a factor of three times that for normal incidence. We conclude that the strain sensitivity of optical absorption of graphene under TIR offers significant potential for application in many areas such as ultra-thin optical devices and strain sensors. PMID:25338947

  8. Redistribution of fluorescent molecules at the solid/liquid interface with total internal reflection illumination.

    PubMed

    Wei, Lin; Ye, Zhongju; Luo, Wenjuan; Chen, Bo; Xiao, Lehui

    2016-08-01

    Many intriguing physical and chemical processes commonly take place at the solid/liquid interface. Total internal reflection illumination, together with single molecule spectroscopy, provides a robust platform for the selective exploration of kinetic processes close the interface. With these techniques, it was observed that the distribution of Rhodamine B molecules close to a solid/liquid interface could be regulated in a photo-induced route. The laser-induced repulsion force at this interface is enough to compromise the Brownian diffusion of single molecules in a range of several hundred nanometers normal to the solid/liquid interface. This observation is fundamentally and practically interesting because moderate laser intensity is enough to initiate this repulsion effect. Therefore, it might display extensive applications in the development of photo-modulation technique with high throughput capability. PMID:27216678

  9. Study of Spectral Modifications in Acidified Ignitable Liquids by Attenuated Total Reflection Fourier Transform Infrared Spectroscopy.

    PubMed

    Martín-Alberca, Carlos; Ojeda, Fernando Ernesto Ortega; García-Ruiz, Carmen

    2016-03-01

    In this work, the spectral characteristics of two types of acidified gasoline and acidified diesel fuel are discussed. Neat and acidified ignitable liquids (ILs) infrared absorption spectra obtained by attenuated total reflection Fourier transform infrared spectroscopy were compared in order to identify the modifications produced by the reaction of the ILs with sulfuric acid. Several bands crucial for gasoline identification were modified, and new bands appeared over the reaction time. In the case of acidified diesel fuel, no significant modifications were observed. Additionally, the neat and acidified ILs spectra were used to perform a principal components analysis in order to confirm objectively the results. The complete discrimination among samples was successfully achieved, including the complete differentiation among gasoline types. Taking into account the results obtained in this work, it is possible to propose spectral fingerprints for the identification of non-burned acidified ILs in forensic investigations related with arson or the use of improvised incendiary devices (IIDs). PMID:26810182

  10. The mid-infrared (attenuated total reflection) spectroscopy of ethylene carbonate in water

    NASA Astrophysics Data System (ADS)

    Brooksby, Paula A.; Fawcett, W. Ronald

    2001-05-01

    Ethylene carbonate (EC) and water solution compositions ranging from pure water to 60 mass% EC have been examined using infrared (attenuated total reflection) spectroscopy. The fundamental vibrational modes of EC in the mid-infrared between 2050 and 1000 cm -1 were fitted to mixed Lorentzian-Gaussian bandshapes. The spectral data for EC bands between 1000 and 650 cm -1 are also shown but were not curve-fitted due to baseline distortions from water librational modes. The results of the band analysis have provided information regarding the molecular structure of these solutions, and the fact that the structure is also concentration dependent. The Fermi resonance coupling between the ν 2 and 2ν 7 vibrations of EC have been analysed using a standard perturbation model.

  11. Watch your step! A frustrated total internal reflection approach to forensic footwear imaging.

    PubMed

    Needham, J A; Sharp, J S

    2016-01-01

    Forensic image retrieval and processing are vital tools in the fight against crime e.g. during fingerprint capture. However, despite recent advances in machine vision technology and image processing techniques (and contrary to the claims of popular fiction) forensic image retrieval is still widely being performed using outdated practices involving inkpads and paper. Ongoing changes in government policy, increasing crime rates and the reduction of forensic service budgets increasingly require that evidence be gathered and processed more rapidly and efficiently. A consequence of this is that new, low-cost imaging technologies are required to simultaneously increase the quality and throughput of the processing of evidence. This is particularly true in the burgeoning field of forensic footwear analysis, where images of shoe prints are being used to link individuals to crime scenes. Here we describe one such approach based upon frustrated total internal reflection imaging that can be used to acquire images of regions where shoes contact rigid surfaces. PMID:26880687

  12. Total-Internal-Reflection Platforms for Chemical and Biological Sensing Applications

    NASA Astrophysics Data System (ADS)

    Sapsford, Kim E.

    Sensing platforms based on the principle of total internal reflection (TIR) represent a fairly mature yet still expanding and exciting field of research. Sensor development has mainly been driven by the need for rapid, stand-alone, automated devices for application in the fields of clinical diagnosis and screening, food and water safety, environmental monitoring, and chemical and biological warfare agent detection. The technologies highlighted in this chapter are continually evolving, taking advantage of emerging advances in microfabrication, lab-on-a-chip, excitation, and detection techniques. This chapter describes many of the underlying principles of TIR-based sensing platforms and additionally focusses on planar TIR fluorescence (TIRF)-based chemical and biological sensors.

  13. Total reflection X-ray spectrometry (TXRF) for trace elements assessment in edible clams.

    PubMed

    Marguí, Eva; de Fátima Marques, Alexandra; de Lurdes Prisal, Maria; Hidalgo, Manuela; Queralt, Ignasi; Carvalho, Maria Luisa

    2014-01-01

    The present contribution presents a preliminary investigation of the chemical composition with respect to major, minor, trace, and ultratrace elements in several clam species that are frequently used for human consumption in Portuguese markets and worldwide. In order to use a simple and rapid analytical methodology for clam analysis, energy dispersive X-ray fluorescence (EDXRF) spectrometry and total reflection X-ray fluorescence (TXRF) spectrometry were selected as analytical techniques. The analytical capabilities of TXRF spectrometry were evaluated for the determination of minor and trace elements in commercial edible clams. We compared the direct analysis of powdered suspensions (using different sample amounts and dispersant agents) with the analysis of the digested samples for trace element determination. Inductively coupled plasma mass spectrometry analysis of clam digests was also performed to evaluate the analytical possibilities of TXRF spectrometry for trace and ultratrace analysis. PMID:25286343

  14. Watch your step! A frustrated total internal reflection approach to forensic footwear imaging

    PubMed Central

    Needham, J. A.; Sharp, J. S.

    2016-01-01

    Forensic image retrieval and processing are vital tools in the fight against crime e.g. during fingerprint capture. However, despite recent advances in machine vision technology and image processing techniques (and contrary to the claims of popular fiction) forensic image retrieval is still widely being performed using outdated practices involving inkpads and paper. Ongoing changes in government policy, increasing crime rates and the reduction of forensic service budgets increasingly require that evidence be gathered and processed more rapidly and efficiently. A consequence of this is that new, low-cost imaging technologies are required to simultaneously increase the quality and throughput of the processing of evidence. This is particularly true in the burgeoning field of forensic footwear analysis, where images of shoe prints are being used to link individuals to crime scenes. Here we describe one such approach based upon frustrated total internal reflection imaging that can be used to acquire images of regions where shoes contact rigid surfaces. PMID:26880687

  15. Quantitative Analysis of Protein Translocations by Microfluidic Total Internal Reflection Fluorescence Flow Cytometry

    PubMed Central

    Wang, Jun; Fei, Bei; Geahlen, Robert L.

    2010-01-01

    Protein translocation, or the change in a proteins location between different subcellular compartments, is a critical process by which intracellular proteins carry out their cellular functions. Aberrant translocation events contribute to various diseases ranging from metabolic disorders to cancer. In this study, we demonstrate the use of a newly developed single-cell tool, microfluidic total internal reflection fluorescence flow cytometry (TIRF-FC), for detecting both cytosol to plasma membrane and cytosol to nucleus translocations using the tyrosine kinase Syk and the transcription factor NF-?B as models. This technique detects fluorescent molecules at the plasma membrane and in the membrane-proximal cytosol in single cells. We were able to record quantitatively changes in the fluorescence density in the evanescent field associated with these translocation processes for large cell populations with single cell resolution. We envision that TIRF-FC will provide a new approach to explore the molecular biology and clinical relevance of protein translocations. PMID:20820633

  16. Near IR Scanning Angle Total Internal Reflection Raman Spectroscopy at Smooth Gold Films

    SciTech Connect

    McKee, Kristopher; Meyer, Matthew; Smith, Emily

    2012-04-13

    Total internal reflection (TIR) Raman and reflectivity spectra were collected for nonresonant analytes as a function of incident angle at sapphire or sapphire/smooth 50 nm gold interfaces using 785 nm excitation. For both interfaces, the Raman signal as a function of incident angle is well-modeled by the calculated interfacial mean square electric field (MSEF) relative to the incident field times the thickness of the layer being probed in the Raman measurement (D{sub RS}). The Raman scatter was reproducibly enhanced at the interface containing a gold film relative to the sapphire interface by a factor of 4.3–4.6 for aqueous pyridine or 2.2–3.7 for neat nitrobenzene, depending on the analyzed vibrational mode. The mechanism for the increased Raman signal is the enhanced MSEF at incident angles where propagating surface plasmons are excited in the metal film. The background from the TIR prism was reduced by 89–95% with the addition of the gold film, and the percent relative uncertainty in peak area was reduced from 15 to 1.7% for the 1347 cm–1 mode of nitrobenzene. Single monolayers of benzenethiol (S/N = 6.8) and 4-mercaptopyridine (S/N = 16.5) on gold films were measured by TIR Raman spectroscopy with 785 nm excitation (210 mW) without resonant enhancement in 1 min.

  17. Analysis of total oil and fatty acids composition by near infrared reflectance spectroscopy in edible nuts

    NASA Astrophysics Data System (ADS)

    Kandala, Chari V.; Sundaram, Jaya

    2014-10-01

    Near Infrared (NIR) Reflectance spectroscopy has established itself as an important tool in quantifying water and oil present in various food materials. It is rapid and nondestructive, easier to use, and does not require processing the samples with corrosive chemicals that would render them non-edible. Earlier, the samples had to be ground into powder form before making any measurements. With the development of new soft ware packages, NIR techniques could now be used in the analysis of intact grain and nuts. While most of the commercial instruments presently available work well with small grain size materials such as wheat and corn, the method present here is suitable for large kernel size products such as shelled or in-shell peanuts. Absorbance spectra were collected from 400 nm to 2500 nm using a NIR instrument. Average values of total oil contents (TOC) of peanut samples were determined by standard extraction methods, and fatty acids were determined using gas chromatography. Partial least square (PLS) analysis was performed on the calibration set of absorption spectra, and models were developed for prediction of total oil and fatty acids. The best model was selected based on the coefficient of determination (R2), Standard error of prediction (SEP) and residual percent deviation (RPD) values. Peanut samples analyzed showed RPD values greater than 5.0 for both absorbance and reflectance models and thus could be used for quality control and analysis. Ability to rapidly and nondestructively measure the TOC, and analyze the fatty acid composition, will be immensely useful in peanut varietal improvement as well as in the grading process of grain and nuts.

  18. The role of total-reflection X-ray fluorescence in atomic spectroscopy

    NASA Astrophysics Data System (ADS)

    Tölg, G.; Klockenkämper, R.

    1993-02-01

    Total-reflection X-ray fluorescence (TXRF) is a universal and economic method for the simultaneous determination of elements with atomic numbers > 11 down to the lower pg-level. It is a microanalytical tool for the analysis of small sample amounts placed on flat carriers and for contaminations on flat sample surfaces. Analyses of stratified near-surface layers are made possible by varying the incident angle of the primary beam in the region of total-reflection. This non-destructive method is especially suitable for thin layers of a few nanometres, deposited on wafer material although not usable as a microprobe method with a high lateral resolution. Furthermore, depth profiles of biological samples can be recorded by means of microtome sectioning of only a few micrometres, as, for example in the gradient analysis of human organs. In addition to micro- and surface-layer analysis, TXRF is effectively applied to element trace analysis. Homogeneous solutions, for example aqueous solutions, high-purity adds or body fluids, are pipetted onto carriers and, after evaporation, the dry residues are analysed directly down to the pg/ml region. Particularly advantageous is the absence of matrix effects, so that an easy calibration can be carried out by adding a single internal standard element. A digestion or separation step preceding the actual determination becomes necessary if a more complex matrix is to be analysed or especially low detection limits have to be reached. A critical evaluation of the recent developments in atomic spectroscopy places TXRF in a leading position. Its outstanding features compete with those of e.g. electrothermal atomic absorption spectrometry (ETAAS), microwave induced plasma optical emission spectroscopy (MIP-OES) and inductively coupled plasma mass spectrometry (ICP-MS) in the field of micro- and trace analysis and with Rutherford backscattering (RBS) and secondary ion mass spectrometry (SIMS) in the surface-layer analysis.

  19. Low-temperature, low-cost growth of robust ATR GeO2 hollow fibers based on copper capillary tubes for transmission of CO2 laser light

    NASA Astrophysics Data System (ADS)

    Jing, Chengbin; Bai, Wei; Hu, Zhigao; Yang, Pingxiong; Liu, Aiyun; Lin, Fangtin; Shi, Yiwei; Chu, Junhao

    2014-02-01

    Attenuated total reflectance (ATR) infrared hollow waveguide attracts particular interest since it has both advantages of a hollow fiber and a light guiding mechanism similar to that of solid-core fibers. Presently, ATR hollow waveguides are mainly structured with single-crystal sapphire or glassy materials. These waveguides are somewhat brittle. More robust ATR hollow fibers are required in many military and domestic applications. In this work, ATR GeO2 hollow waveguides were prepared based on a copper capillary tube for transmitting CO2 laser light. The inner wall of the copper structural tube was polished using a high-pressure pulsed nanofluid technique. A hexagonal crystalline GeO2 reflective layer with sufficient thickness (>4 μm) was grown on the inner tube wall via a simple liquid phase deposition process at room temperature. The GeO2 coated copper hollow fiber exhibits a low-loss band within 10-11.5 μm. It can still be bent since the hollow-core size (1.4 mm) and the wall thickness (50 μm) are not too large. The transmissions of CO2 laser light are 91% and 43% under a straight condition and a 90° bend with a 30-cm radius condition, respectively. The waveguide displays high heat-resisting properties due to high thermal conductivity of the copper substrate tube and a high melting point (1115°C) of the GeO2 reflective layer. This work opens a door for low-temperature, low-cost growth of long ATR GeO2 infrared hollow fibers based on various substrate tubes, even including plastic capillary tubes.

  20. Sensitivity Studies for Space-based Measurements of Atmospheric Total Column Carbon Dioxide Using Reflected Sunlight

    NASA Technical Reports Server (NTRS)

    Mao, Jianping; Kawa, S. Randolph

    2003-01-01

    A series of sensitivity studies is carried out to explore the feasibility of space-based global carbon dioxide (CO2) measurements for global and regional carbon cycle studies. The detection method uses absorption of reflected sunlight in the CO2 vibration-rotation band at 1.58 micron. The sensitivities of the detected radiances are calculated using the line-by-line model (LBLRTM), implemented with the DISORT (Discrete Ordinates Radiative Transfer) model to include atmospheric scattering in this band. The results indicate that (a) the small (approx.1%) changes in CO2 near the Earth's surface are detectable in this CO2 band provided adequate sensor signal-to-noise ratio and spectral resolution are achievable; (b) the effects of other interfering constituents, such as water vapor, aerosols and cirrus clouds, on the radiance are significant but the overall effects of the modification of light path length on total back-to-space radiance sensitivity to CO2 change are minor for general cases, which means that generally the total column CO2 can be derived in high precision from the ratio of the on-line center to off-line radiances; (c) together with CO2 gas absorption aerosol/cirrus cloud layer has differential scattering which may result in the modification of on-line to off-line radiance ratio which could lead a large bias in the total column CO2 retrieval. Approaches to correct such bias need further investigation. (d) CO2 retrieval requires good knowledge of the atmospheric temperature profile, e.g. approximately 1K RMS error in layer temperature, which is achievable from new atmospheric sounders in the near future; (e) the atmospheric path length, over which the CO2 absorption occurs, should be known in order to correctly interpret horizontal gradients of CO2 from the total column CO2 measurement; thus an additional sensor for surface pressure measurement needs to be attached for a complete measurement package.

  1. An informative confidence metric for ATR.

    SciTech Connect

    Bow, Wallace Johnston Jr.; Richards, John Alfred; Bray, Brian Kenworthy

    2003-03-01

    Automatic or assisted target recognition (ATR) is an important application of synthetic aperture radar (SAR). Most ATR researchers have focused on the core problem of declaration-that is, detection and identification of targets of interest within a SAR image. For ATR declarations to be of maximum value to an image analyst, however, it is essential that each declaration be accompanied by a reliability estimate or confidence metric. Unfortunately, the need for a clear and informative confidence metric for ATR has generally been overlooked or ignored. We propose a framework and methodology for evaluating the confidence in an ATR system's declarations and competing target hypotheses. Our proposed confidence metric is intuitive, informative, and applicable to a broad class of ATRs. We demonstrate that seemingly similar ATRs may differ fundamentally in the ability-or inability-to identify targets with high confidence.

  2. A label-free continuous total-internal-reflection-fluorescence-based immunosensor.

    PubMed

    Engstrm, Henrik A; Andersson, Per Ola; Ohlson, Sten

    2006-10-15

    In this study, we continuously monitored, second-by-second, concentration changes of two different carbohydrates (maltose and panose) by using monoclonal antibodies in an optical immunosensor based on total internal reflection fluorescence. Earlier studies have demonstrated that these antibodies increase their intrinsic tryptophan fluorescence upon binding of carbohydrate antigens. Using the four immobilized monoclonal antibodies with low affinities (K(d)>10(-6)M), fast kinetics (k(off)>1s(-1)), and high reversibility gave opportunities for developing a continuous immunosensor without any need for regeneration. Since intrinsic fluorescence was used, no extrinsic labeling was necessary. Sensitivity was in the range of 1-5 microM for panose, and 10-15 microM for maltose and the loss of intensity was as low as 3.5% per hour during measurements. Calculations of DeltaH degrees and DeltaS degrees from the temperature dependence of K(d) indicated an enthalpic driven antigen-antibody binding event that is diminished upon antibody immobilization. We feel certain that weakly interacting antibodies can be used in future applications for continuous monitoring where there is a need to achieve instantaneous information on the concentration of an analyte. PMID:16934212

  3. Novel Bio, Chemical, Environmental Sensing Based on New Model of Total Internal Reflection in Turbid Media

    NASA Astrophysics Data System (ADS)

    Bali, Samir; Judge, Patrick; Phillip, Nathan; Boivin, Jordan; Scaffidi, Jonathan; Berberich, Jason; Bali, Lalit

    2014-05-01

    We have initiated a collaborative experimental research program that combines new advances in optical physics, field portable chemical analysis, and biosensing. Our goal is to discover and characterize new optical sensing methodologies in opaque, highly scattering (i.e., ``turbid'') media, and demonstrate new paradigms for optical sensing in research and industry. We have three specific objectives. First, we propose to fully characterize and validate a new model of total internal reflection (TIR) from highly turbid media thus enabling a first demonstration of non-invasive, in-situ, real-time particle sizing for the case of arbitrary scattering particle size-a holy grail in colloidal science. Second, we propose to implement a first demonstration of real-time non-invasive measurement of nanoparticle aggregation in highly turbid media. Third, we propose to use our new sensing methodology to demonstrate real-time in-situ label-free monitoring of molecular interactions and adsorption at surfaces. We gratefully acknowledge support from the American Chemical Society Petroleum Research Fund and Miami University's Interdisciplinary Roundtable Fund. We also gratefully acknowledge experimental help from the Miami University Instrumentation Laboratory.

  4. Total internal reflection fluorescence microscopy for determination of size of individual immobilized vesicles: Theory and experiment

    NASA Astrophysics Data System (ADS)

    Olsson, Thomas; Zhdanov, Vladimir P.; Höök, Fredrik

    2015-08-01

    Lipid vesicles immobilized via molecular linkers at a solid support represent a convenient platform for basic and applied studies of biological processes occurring at lipid membranes. Using total internal reflection fluorescence microscopy (TIRFM), one can track such processes at the level of individual vesicles provided that they contain dyes. In such experiments, it is desirable to determine the size of each vesicle, which may be in the range from 50 to 1000 nm. Fortunately, TIRFM in combination with nanoparticle tracking analysis makes it possible to solve this problem as well. Herein, we present the formalism allowing one to interpret the TIRFM measurements of the latter category. The analysis is focused primarily on the case of unpolarized light. The specifics of the use of polarized light are also discussed. In addition, we show the expected difference in size distribution of suspended and immobilized vesicles under the assumption that the latter ones are deposited under diffusion-controlled conditions. In the experimental part of our work, we provide representative results, showing explicit advantages and some shortcomings of the use of TIRFM in the context under consideration, as well as how our refined formalism improves previously suggested approaches.

  5. Preparation of Reactions for Imaging with Total Internal Reflection Fluorescence Microscopy.

    PubMed

    Kudalkar, Emily M; Davis, Trisha N; Asbury, Charles L

    2016-01-01

    Here we present our standard protocol for studying the binding of kinetochore proteins to microtubules as a paradigm for designing single-molecule total internal reflection fluorescence (TIRF) microscopy experiments. Several aspects of this protocol require empirical optimization, including the method for anchoring the polymer or substrate to the coverslip, the type and amount of blocking protein to prevent nonspecific protein adsorption to the glass, the appropriate protein concentration, the laser power, and the duration of imaging. Our method uses bovine serum albumin and κ-casein as blocking agents to coat any imperfections in the coverslip silanization and thereby prevent protein adsorption to the coverslip. Protein concentration and duration of imaging must be optimized for each experiment and protein of interest. Ideally, a range is determined that allows for resolution of single complexes binding to microtubules to ensure proper measurement of kinetic off rates and diffusion along microtubules. Excessively high concentrations may lead to overlapping binding of proteins on microtubules, making it impossible to resolve single binding events. The duration of imaging must be long enough to capture very low off rates (long residence time on microtubules) and we typically image at 10 frames/sec for 200 sec. The laser power can be adjusted to prevent photobleaching, but must be high enough to achieve a sufficient signal/noise ratio. PMID:27140912

  6. Small-angle measurement with highly sensitive total-internal-reflection heterodyne interferometer.

    PubMed

    Lin, Jiun-You; Liao, Yu-Cheng

    2014-03-20

    In this paper, a high-sensitivity total-internal-reflection (TIR) heterodyne interferometer is proposed for measuring small angles. In the proposed interferometer, a half-wave plate and two quarter-wave plates that exhibit specific optic-axis azimuths are combined to form a phase shifter. When a rhomboid prism is placed between the phase shifter and an analyzer that exhibits suitable transmission-axis azimuth, it shifts and enhances the phase difference of the s- and p-polarization states at double TIR. The enhanced phase difference is dependent on the incident angle; thus small angles can be easily and accurately measured by estimating the phase difference. The experimental results demonstrate the feasibility of this method. Angular resolution and sensitivity levels superior to 1.2×10⁻⁴ deg (2.1×10⁻⁶ rad) and 100 (deg/deg), respectively, were attainable in a dynamic range of 0.5 deg. PMID:24663469

  7. Use of liposomal amplifiers in total internal reflection fluorescence fiber-optic biosensors for protein detection.

    PubMed

    Chang, Ying-Feng; Fu, Chen; Chen, Yi-Ting; Fang-Ju Jou, Amily; Chen, Chii-Chang; Chou, Chien; Annie Ho, Ja-An

    2016-03-15

    Evanescent-wave excited fluorescence technology has been demonstrated to enhance sensitivity and reduce matrix effects, making it suitable for biosensor development. In this study, we developed a liposome-based, total internal reflection fluorescence, fiber-optic biosensor (TIRF-FOB) for protein detection, which integrates a liposomal amplifier and sandwich immunoassay format with TIRF-FOB. In addition, the antibody-tagged and fluorophore-entrapped liposomes for heterogeneous detection of target molecules were designed and synthesized. This biosensor successfully detected the target protein (model analyzed here is IgG) with a limit of detection (LOD) of 2.0 attomoles for the target protein (equivalent to 2.0 pg/mL of protein presented in 150 μL of sample solution). The features of this ultra-sensitive liposomal TIRF-FOB are (i) fluorescence is excited via evanescent waves and amplified via liposomes; (ii) the use of two polyclonal antibodies in the sandwich assay format increases the specificity and lowers the cost of our assay. Based on the exceptional detection sensitivity and cost-effectiveness, we believe that the proposed biosensor has great potential as a practical, clinical diagnostic tool in the near future. PMID:26595485

  8. Tunable Wide-Angle Tunneling in Graphene-Assisted Frustrated Total Internal Reflection

    PubMed Central

    Tran, Thang Q.; Lee, Sangjun; Heo, Hyungjun; Kim, Sangin

    2016-01-01

    Electrically tunable permittivity of graphene provides an excellent tool in photonic device design. Many previous works on graphene-based photonic devices relied on variable absorption in graphene, which is naturally small in the optical region, and resonant structures to enhance it. Here we proposed a novel scheme to control evanescent coupling strength by inserting two graphene layers to a frustrated total internal reflection (FTIR) configuration. The resulting structure behaves in a drastically different way from the original FTIR: optical transmission though the structure can be electrically controlled from ~10−5 to ~1 with little dependency on angle of incidence. This unique feature stems from the fact that the permittivity of doped graphene can be close to zero at a certain photon energy. The electrical controllability of evanescent coupling strength can enable novel design of optical devices. As a proof-of-concept, we designed a waveguide-type optical modulator of a novel operation principle: transmission modulation depends on the electrically controlled existence of a guided-mode of the waveguide, not the variation of the ohmic loss of graphene, resulting in a low insertion loss and a small device footprint. PMID:26815116

  9. Identification of novel insulin mimetic drugs by quantitative total internal reflection fluorescence (TIRF) microscopy

    PubMed Central

    Lanzerstorfer, Peter; Stadlbauer, Verena; Chtcheglova, Lilia A; Haselgrübler, Renate; Borgmann, Daniela; Wruss, Jürgen; Hinterdorfer, Peter; Schröder, Klaus; Winkler, Stephan M; Höglinger, Otmar; Weghuber, Julian

    2014-01-01

    Background and Purpose Insulin stimulates the transport of glucose in target tissues by triggering the translocation of glucose transporter 4 (GLUT4) to the plasma membrane. Resistance to insulin, the major abnormality in type 2 diabetes, results in a decreased GLUT4 translocation efficiency. Thus, special attention is being paid to search for compounds that are able to enhance this translocation process in the absence of insulin. Experimental Approach Total internal reflection fluorescence (TIRF) microscopy was applied to quantify GLUT4 translocation in highly insulin-sensitive CHO-K1 cells expressing a GLUT4-myc-GFP fusion protein. Key Results Using our approach, we demonstrated GLUT4 translocation modulatory properties of selected substances and identified novel potential insulin mimetics. An increase in the TIRF signal was found to correlate with an elevated glucose uptake. Variations in the expression level of the human insulin receptor (hInsR) showed that the insulin mimetics identified stimulate GLUT4 translocation by a mechanism that is independent of the presence of the hInsR. Conclusions and Implications Taken together, the results indicate that TIRF microscopy is an excellent tool for the quantification of GLUT4 translocation and for identifying insulin mimetic drugs. PMID:25039620

  10. Uniform total internal reflection fluorescence illumination enables live cell fluorescence resonance energy transfer microscopy.

    PubMed

    Lin, Jia; Hoppe, Adam D

    2013-04-01

    Fluorescence resonance energy transfer (FRET) microscopy is a powerful technique to quantify dynamic protein-protein interactions in live cells. Total internal reflection fluorescence (TIRF) microscopy can selectively excite molecules within about 150 nm of the glass-cell interface. Recently, these two approaches were combined to enable high-resolution FRET imaging on the adherent surface of living cells. Here, we show that interference fringing of the coherent laser excitation used in TIRF creates lateral heterogeneities that impair quantitative TIRF-FRET measurements. We overcome this limitation by using a two-dimensional scan head to rotate laser beams for donor and acceptor excitation around the back focal plane of a high numerical aperture objective. By setting different radii for the circles traced out by each laser in the back focal plane, the penetration depth was corrected for different wavelengths. These modifications quell spatial variations in illumination and permit calibration for quantitative TIRF-FRET microscopy. The capability of TIRF-FRET was demonstrated by imaging assembled cyan and yellow fluorescent protein-tagged HIV-Gag molecules in single virions on the surfaces of living cells. These interactions are shown to be distinct from crowding of HIV-Gag in lipid rafts. PMID:23472941

  11. Total internal reflection holographic microscopy (TIRHM) for quantitative phase characterization of cell-substrate adhesion

    NASA Astrophysics Data System (ADS)

    Ash, William Mason, III

    Total Internal Reflection Holographic Microscopy (TIRHM) combines near-field microscopy with digital holography to produce a new form of near-field phase microscopy. Using a prism in TIR as a near-field imager, the presence of microscopic organisms, cell-substrate interfaces, and adhesions, causes relative refractive index (RRI) and frustrated TIR (f-TIR) to modulate the object beam's evanescent wave phase front. Quantitative phase images of test specimens such as Amoeba proteus, Dictyostelium Discoideum and cells such as SKOV-3 ovarian cancer and 3T3 fibroblasts are produced without the need to introduce stains or fluorophores. The angular spectrum method of digital holography to compensate for tilt anamorphism due to the inclined TIR plane is also discussed. The results of this work conclusively demonstrate, for the first time, the integration of near-field microscopy with digital holography. The cellular images presented show a correlation between the physical extent of the Amoeba proteus plasma membrane and the adhesions that are quantitatively profiled by phase cross-sectioning of the holographic images obtained by digital holography. With its ability to quantitatively characterise cellular adhesion and motility, it is anticipated that TIRHM can be a tool for characterizing and combating cancer metastasis, as well as improving our understanding of morphogenesis and embryogenesis itself.

  12. Design and Construction of a Multi-wavelength, Micromirror Total Internal Reflectance Fluorescence Microscope

    PubMed Central

    Larson, Joshua; Kirk, Matt; Drier, Eric A.; OBrien, William; MacKay, James F.; Friedman, Larry; Hoskins, Aaron

    2015-01-01

    Colocalization Single Molecule Spectroscopy (CoSMoS) has proven to be a useful method for studying the composition, kinetics, and mechanisms of complex cellular machines. Key to the technique is the ability to simultaneously monitor multiple proteins and/or nucleic acids as they interact with one another. Here we describe a protocol for constructing a CoSMoS micromirror Total Internal Reflection Fluorescence Microscope (mmTIRFM). Design and construction of a scientific microscope often requires a number of custom components and a significant time commitment. In our protocol, we have streamlined this process by implementation of a commercially available microscopy platform designed to accommodate the optical components necessary for a mmTIRFM. The mmTIRF system eliminates the need for machining custom parts by the end-user and facilitates optical alignment. Depending on the experience-level of the microscope builder, these time-savings and the following protocol can enable mmTIRF construction to be completed within two months. PMID:25188633

  13. Total reflection X-ray fluorescence analysis of pollen as an indicator for atmospheric pollution*1

    NASA Astrophysics Data System (ADS)

    Pepponi, G.; Lazzeri, P.; Coghe, N.; Bersani, M.; Gottardini, E.; Cristofolini, F.; Clauser, G.; Torboli, A.

    2004-08-01

    The viability of pollen is affected by environmental pollution and its use as a bio-indicator is proposed. Such effects can be observed and quantified by biological tests. However, a more accurate identification of the agents affecting the viability is required in order to validate the biological assay for environmental monitoring. The chemical analysis of pollen is meant to ascertain the existence of a correlation between its reduced biological functions and the presence of pollutants. Moreover, such biological systems act as accumulators and allow the detection and quantification of species present in the environment at low concentrations. Total reflection X-ray fluorescence analysis (TXRF) has been chosen for the investigation due to its high sensitivity, multielement capability and wide dynamic range. Corylus avellana L. (hazel) pollen has been collected in areas with different anthropic impact in the province of Trento, Italy. For the TXRF measurements, a liquid sample is needed, especially if a quantitative analysis is required. In the present work, the analysis after a microwave digestion has been compared with the analysis of a suspension of the pollen samples. In both cases, an internal standard has been used for the quantification. The concentrations of 17 elements ranging from Al to Pb have been determined in 13 samples. Analysis of the suspensions showed to be comparable to that of digested samples in terms of spectral quality, but the latter preparation method gave better reproducibility. Sub-ppm lowest limits of detection were obtained for iron and heavier elements detected.

  14. High pressure sample cell for total internal reflection fluorescence spectroscopy at pressures up to 2500 bar

    NASA Astrophysics Data System (ADS)

    Koo, Juny; Czeslik, Claus

    2012-08-01

    Total internal reflection fluorescence (TIRF) spectroscopy is a surface sensitive technique that is widely used to characterize the structure and dynamics of molecules at planar liquid-solid interfaces. In particular, biomolecular systems, such as protein adsorbates and lipid membranes can easily be studied by TIRF spectroscopy. Applying pressure to molecular systems offers access to all kinds of volume changes occurring during assembly of molecules, phase transitions, and chemical reactions. So far, most of these volume changes have been characterized in bulk solution, only. Here, we describe the design and performance of a high pressure sample cell that allows for TIRF spectroscopy under high pressures up to 2500 bar (2.5 108 Pa), in order to expand the understanding of volume effects from the bulk phase to liquid-solid interfaces. The new sample cell is based on a cylindrical body made of Nimonic 90 alloy and incorporates a pressure transmitting sample cuvette. This cuvette is composed of a fused silica prism and a flexible rubber gasket. It contains the sample solution and ensures a complete separation of the sample from the liquid pressure medium. The sample solution is in contact with the inner wall of the prism forming the interface under study, where fluorescent molecules are immobilized. In this way, the new high pressure TIRF sample cell is very useful for studying any biomolecular layer that can be deposited at a planar water-silica interface. As examples, high pressure TIRF data of adsorbed lysozyme and two phospholipid membranes are presented.

  15. Direct measurements of particle-surface interactions in aqueous solutions with total internal reflection microscopy.

    PubMed

    Gong, Xiangjun; Wang, Zhaohui; Ngai, To

    2014-06-25

    Non-covalent intermolecular forces, such as van der Waals, electrostatic, steric, and hydrophobic interactions, have played essential roles in determining the association, aggregation, adhesion and sedimentation processes of colloidal particles, surfactant micelles, and macromolecules, in solutions and biological systems. These interaction forces, however, are normally weak (Total Internal Reflection Microscopy (TIRM) for studying the interactions between a single colloidal particle and a flat surface. We begin with a brief overview of quantitative measurements of particle-surface interactions in aqueous solutions, and then show recent developments associated with TIRM for measuring kT-scale interactions between a single particle and surface in the presence of polymer chains, micelles, and colloidal particles with different softness based on our recent work. We also highlight how TIRM can be used to measure particle-surface interactions after the particle and the flat surface are physically adsorbed or grafted with polyelectrolytes, as well as to investigate the non-specific and specific interactions between proteins and protein-carbohydrate in biological systems. Lastly, we conclude with some perspectives on future research efforts in this field. PMID:24718492

  16. Tunable Wide-Angle Tunneling in Graphene-Assisted Frustrated Total Internal Reflection

    NASA Astrophysics Data System (ADS)

    Tran, Thang Q.; Lee, Sangjun; Heo, Hyungjun; Kim, Sangin

    2016-01-01

    Electrically tunable permittivity of graphene provides an excellent tool in photonic device design. Many previous works on graphene-based photonic devices relied on variable absorption in graphene, which is naturally small in the optical region, and resonant structures to enhance it. Here we proposed a novel scheme to control evanescent coupling strength by inserting two graphene layers to a frustrated total internal reflection (FTIR) configuration. The resulting structure behaves in a drastically different way from the original FTIR: optical transmission though the structure can be electrically controlled from ~10-5 to ~1 with little dependency on angle of incidence. This unique feature stems from the fact that the permittivity of doped graphene can be close to zero at a certain photon energy. The electrical controllability of evanescent coupling strength can enable novel design of optical devices. As a proof-of-concept, we designed a waveguide-type optical modulator of a novel operation principle: transmission modulation depends on the electrically controlled existence of a guided-mode of the waveguide, not the variation of the ohmic loss of graphene, resulting in a low insertion loss and a small device footprint.

  17. Tunable Wide-Angle Tunneling in Graphene-Assisted Frustrated Total Internal Reflection.

    PubMed

    Tran, Thang Q; Lee, Sangjun; Heo, Hyungjun; Kim, Sangin

    2016-01-01

    Electrically tunable permittivity of graphene provides an excellent tool in photonic device design. Many previous works on graphene-based photonic devices relied on variable absorption in graphene, which is naturally small in the optical region, and resonant structures to enhance it. Here we proposed a novel scheme to control evanescent coupling strength by inserting two graphene layers to a frustrated total internal reflection (FTIR) configuration. The resulting structure behaves in a drastically different way from the original FTIR: optical transmission though the structure can be electrically controlled from ~10(-5) to ~1 with little dependency on angle of incidence. This unique feature stems from the fact that the permittivity of doped graphene can be close to zero at a certain photon energy. The electrical controllability of evanescent coupling strength can enable novel design of optical devices. As a proof-of-concept, we designed a waveguide-type optical modulator of a novel operation principle: transmission modulation depends on the electrically controlled existence of a guided-mode of the waveguide, not the variation of the ohmic loss of graphene, resulting in a low insertion loss and a small device footprint. PMID:26815116

  18. Elucidation of perovskite film micro-orientations using two-photon total internal reflectance fluorescence microscopy

    SciTech Connect

    Watson, Brianna R.; Yang, Bin; Xiao, Kai; Ma, Ying -Zhong; Doughty, Benjamin L.; Calhoun, Tessa R.

    2015-07-29

    The emergence of efficient hybrid organic-inorganic perovskite photovoltaic materials has caused the rapid development of a variety of preparation and processing techniques designed to maximize their performance. As processing methods continue to emerge, it is important to understand how the optical properties of these materials are affected on a microscopic scale. Here polarization resolved two-photon total internal reflectance microscopy (TIRFM) was used to probe changes in transition dipole moment orientation as a function of thermal annealing time in hybrid organic-inorganic lead iodide based perovskite (CH3NH3PbI3) thin films on glass. These results show that as thermal annealing time is increased the distribution of transition moments pointing out-of-plane decreases in favor of forming areas with increased in-plane orientations. As a result, it was also shown through the axial sensitivity of TIRFM that the surface topography is manifested in the signal intensity and can be used to survey aspects of morphology in coincidence with the optical properties of these films.

  19. Real-time imaging of Mu opioid receptors by total internal reflection fluorescence microscopy

    PubMed Central

    Roman-Vendrell, Cristina; Yudowski, Guillermo Ariel

    2016-01-01

    Receptor trafficking and signaling are intimately linked, especially in the Mu opioid receptor (MOR) where ligand dependent endocytosis and recycling have been associated to opioid tolerance and dependence. Ligands of the Mu opioid receptor (MOR) can induce receptor endocytosis and recycling within minutes of exposure in heterologous systems and cultured neurons. Endocytosis removes desensitized receptors after their activation from the plasma membrane, while recycling promotes resensitization by delivering functional receptors to the cell surface. These rapid mechanisms can escape traditional analytical methods where only snapshots are obtained from highly dynamic events. Total internal reflection fluorescence (TIRF) microscopy is a powerful tool that can be used to investigate, in real-time, surface trafficking events at the single molecule level. The restricted excitation of fluorophores located at or near the plasma membrane in combination with high sensitivity quantitative cameras, makes it possible to record and analyze individual endocytic and recycling event in real time. In this chapter, we describe a TIRF microscopy protocol to investigate in real time, the ligand dependent MOR trafficking in Human Embryonic Kidney 293 cells and dissociated striatal neuronal cultures. This approach can provide unique spatio-temporal resolution to understand the fundamental events controlling MOR trafficking at the plasma membrane. PMID:25293317

  20. Optical design and laser ablation of surface textures: demonstrating total internal reflection

    NASA Astrophysics Data System (ADS)

    Gommans, Hans; Booij, Silvia; Pijlman, Fetze; Krijn, Marcel; de Zwart, Siebe; Sepkhanov, Ruslan; Beaumont, Dave; van der Schaft, Hans; Sanders, Rene

    2015-09-01

    In lighting applications key drivers for optical design of surface textures are integration of optical elements, the disentanglement of optical functionality and appearance and late stage configuration. We investigated excimer laser ablation as a mastering technology for micro textured surfaces, where we targeted an increase in correspondence between surface design and ablated surface for high aspect ratio structures. To achieve this we have improved the photo mask design using a heuristic algorithm that corrects for the angular dependence of the ablation process and the loss of image resolution at ablation depths that exceed the depth of field. Using this approach we have been able to demonstrate close correspondence between designed and ablated facet structures up to 75° inclination at 75 μm depth. These facet design parameters allow for total internal reflection (TIR) as a means of beam deflection which is demonstrated in a range of mono shaped cone arrays in hexagonal tessellation. BSDF analysis was used to characterize the narrow TIR deflection beams that matched the peak positions of the design down to 28° apex. In addition, a single surface TIR-Fresnel lens design with focal distance 5 mm has been manufactured using this photo mask design algorithm and beam collimation up to 12° beam angle and 32° field angle is shown. These outcomes demonstrate that the laser ablation process intrinsically yields sufficient small dispersion in structure and fillet radii for lighting applications.

  1. Portable total reflection x-ray fluorescence analysis in the identification of unknown laboratory hazards

    SciTech Connect

    Liu, Ying Imashuku, Susumu; Sasaki, Nobuharu; Ze, Long; Kawai, Jun; Takano, Shotaro; Sohrin, Yoshiki; Seki, Hiroko; Miyauchi, Hiroya

    2014-05-15

    In this study, a portable total reflection x-ray fluorescence (TXRF) spectrometer was used to analyze unknown laboratory hazards that precipitated on exterior surfaces of cooling pipes and fume hood pipes in chemical laboratories. With the aim to examine the accuracy of TXRF analysis for the determination of elemental composition, analytical results were compared with those of wavelength-dispersive x-ray fluorescence spectrometry, scanning electron microscope and energy-dispersive x-ray spectrometry, energy-dispersive x-ray fluorescence spectrometry, inductively coupled plasma atomic emission spectrometry, x-ray diffraction spectrometry (XRD), and x-ray photoelectron spectroscopy (XPS). Detailed comparison of data confirmed that the TXRF method itself was not sufficient to determine all the elements (Z > 11) contained in the samples. In addition, results suggest that XRD should be combined with XPS in order to accurately determine compound composition. This study demonstrates that at least two analytical methods should be used in order to analyze the composition of unknown real samples.

  2. Rainwater analysis by synchrotron radiation-total reflection X-ray fluorescence

    NASA Astrophysics Data System (ADS)

    López, María L.; Ceppi, Sergio A.; Asar, María L.; Bürgesser, Rodrigo E.; Ávila, Eldo E.

    2015-11-01

    Total reflection X-ray fluorescence analysis excited with synchrotron radiation was used to quantify the elemental concentration of rainwater in Córdoba, Argentina. Standard solutions with gallium as internal standard were prepared for the calibration curves. Rainwater samples of 5 μl were added to an acrylic reflector, allowed to dry, and analyzed for 200 s measuring time. The elemental concentrations of As, Ca, Co, Cr, Cu, Fe, K, Mn, Ni, Pb, S, Sr, V, and Zn were determined. The electrical conductivity, pH, and elemental concentrations were compared to data previously reported for the soluble fraction of rainwater at different sites. A factor analysis was performed in order to determine the sources that contributed to the elemental concentration in rainwater. Anthropogenic sources were identified as traffic pollution, vehicular emissions, and metallurgical factories. The quality of rainwater was analyzed by comparing the concentrations of all the elements in rainwater samples with the WHO guideline values for drinking water. The results show the need to control the atmospheric emissions in order to preserve the quality of rainwater. SR-TXRF analysis of chemical composition of rainwater in Córdoba represents the very first contribution in the region to the knowledge of the concentration of trace metals in the soluble fraction of rainwater. These data are scarce, especially in the Southern Hemisphere.

  3. Frustrated total internal reflection in organic light-emitting diodes employing sphere cavity embedded in polystyrene

    NASA Astrophysics Data System (ADS)

    Zhu, Peifen

    2016-02-01

    The light extraction efficiency of top-emitting organic light-emitting diodes (OLEDs) is numerically investigated employing the finite-difference time-domain method. The periodic nanostructures formed by embedding the sphere arrays in polystyrene (PS) are placed on top of OLED to frustrate the total internal reflection at the interface between OLED and free space. These nanostructures serve as an intermediate medium to extract the light out of OLED devices. Efficiently coupling both evanescent waves and propagation waves into spheres and subsequently extracting these light waves out of the sphere is key to achieving high extraction efficiency. By tuning the thickness of PS layer, both of the in-coupling efficiency and out-coupling efficiency are optimized for achieving high light extraction efficiency. Thicker PS layer results in higher in-coupling efficiency in sphere while the thinner PS layer leads to higher out-coupling efficiency. Thus the maximum light extraction is a trade-off between the in-coupling efficiency and out-coupling efficiency. The study shows that light extraction efficiency of 89% can be achieved by embedding 0.90 μm TiO2 sphere in 0.30 μm PS layer with optimized in-coupling efficiency, out-coupling efficiency and cavity effect.

  4. Extraction of light trapped due to total internal reflection using porous high refractive index nanoparticle films

    NASA Astrophysics Data System (ADS)

    Mao, Peng; Sun, Fangfang; Yao, Hanchao; Chen, Jing; Zhao, Bo; Xie, Bo; Han, Min; Wang, Guanghou

    2014-06-01

    TiO2 nanoparticle layers composed of columnar TiO2 nanoparticle piles separated with nanoscale pores were fabricated on the bottom surface of the hemispherical glass prism by performing gas phase cluster beam deposition at glancing incidence. The porosity as well as the refractive index of the nanoparticle layer was precisely tuned by the incident angle. Effective extraction of the light trapped in the substrate due to total internal reflection with the TiO2 nanoparticle layers was demonstrated and the extraction efficiency was found to increase with the porosity. An enhanced Rayleigh scattering mechanism, which results from the columnar aggregation of the nanoparticles as well as the strong contrast in the refractive index between pores and TiO2 nanoparticles in the nanoporous structures, was proposed. The porous TiO2 nanoparticle coatings were fabricated on the surface of GaN LEDs to enhance their light output. A nearly 92% PL enhancement as well as a 30% EL enhancement was observed. For LED applications, the enhanced light extraction with the TiO2 nanoparticle porous layers can be a supplement to the microscale texturing process for light extraction enhancement.

  5. Silver nanocube aggregation gradient materials in search for total internal reflection with high phase sensitivity.

    PubMed

    König, Tobias A F; Ledin, Petr A; Russell, Michael; Geldmeier, Jeffrey A; Mahmoud, Mahmoud A; El-Sayed, Mostafa A; Tsukruk, Vladimir V

    2015-03-12

    We fabricated monolayer coatings of a silver nanocube aggregation to create a step-wise optical strip by applying different surface pressures during slow Langmuir-Blodgett deposition. The varying amount of randomly distributed nanocube aggregates with different surface coverages in gradient manner due to changes in surface pressure allows for continuous control of the polarization sensitive absorption of the incoming light over a broad optical spectrum. Optical characterization under total internal reflection conditions combined with electromagnetic simulations reveal that the broadband light absorption depends on the relative orientation of the nanoparticles to the polarization of the incoming light. By using computer simulations, we found that the electric field vector of the s-polarized light interacts with the different types of silver nanocube aggregations to excite different plasmonic resonances. The s-polarization shows dramatic changes of the plasmonic resonances at different angles of incidence (shift of 64 nm per 10° angle of incidence). With a low surface nanocube coverage (from 5% to 20%), we observed a polarization-selective high absorption of 80% (with an average 75%) of the incoming light over a broad optical range in the visible region from 400 nm to 700 nm. This large-area gradient material with location-dependent optical properties can be of particular interest for broadband light absorption, phase-sensitive sensors, and imaging. PMID:25707955

  6. Brain tumour differentiation: rapid stratified serum diagnostics via attenuated total reflection Fourier-transform infrared spectroscopy.

    PubMed

    Hands, James R; Clemens, Graeme; Stables, Ryan; Ashton, Katherine; Brodbelt, Andrew; Davis, Charles; Dawson, Timothy P; Jenkinson, Michael D; Lea, Robert W; Walker, Carol; Baker, Matthew J

    2016-05-01

    The ability to diagnose cancer rapidly with high sensitivity and specificity is essential to exploit advances in new treatments to lead significant reductions in mortality and morbidity. Current cancer diagnostic tests observing tissue architecture and specific protein expression for specific cancers suffer from inter-observer variability, poor detection rates and occur when the patient is symptomatic. A new method for the detection of cancer using 1 μl of human serum, attenuated total reflection-Fourier transform infrared spectroscopy and pattern recognition algorithms is reported using a 433 patient dataset (3897 spectra). To the best of our knowledge, we present the largest study on serum mid-infrared spectroscopy for cancer research. We achieve optimum sensitivities and specificities using a Radial Basis Function Support Vector Machine of between 80.0 and 100 % for all strata and identify the major spectral features, hence biochemical components, responsible for the discrimination within each stratum. We assess feature fed-SVM analysis for our cancer versus non-cancer model and achieve 91.5 and 83.0 % sensitivity and specificity respectively. We demonstrate the use of infrared light to provide a spectral signature from human serum to detect, for the first time, cancer versus non-cancer, metastatic cancer versus organ confined, brain cancer severity and the organ of origin of metastatic disease from the same sample enabling stratified diagnostics depending upon the clinical question asked. PMID:26874961

  7. Elemental concentration analysis in prostate tissues using total reflection X-ray fluorescence

    NASA Astrophysics Data System (ADS)

    Leitão, R. G.; Palumbo, A.; Souza, P. A. V. R.; Pereira, G. R.; Canellas, C. G. L.; Anjos, M. J.; Nasciutti, L. E.; Lopes, R. T.

    2014-02-01

    Prostate cancer (PCa) currently represents the second most prevalent malignant neoplasia in men, representing 21% of all cancer cases. Benign Prostate Hyperplasia (BPH) is an illness prevailing in men above the age of 50, close to 90% after the age of 80. The prostate presents a high zinc concentration, about 10-fold higher than any other body tissue. In this work, samples of human prostate tissues with cancer, BPH and normal tissue were analyzed utilizing total reflection X-ray fluorescence spectroscopy using synchrotron radiation technique (SR-TXRF) to investigate the differences in the elemental concentrations in these tissues. SR-TXRF analyses were performed at the X-ray fluorescence beamline at Brazilian National Synchrotron Light Laboratory (LNLS), in Campinas, São Paulo. It was possible to determine the concentrations of the following elements: P, S, K, Ca, Fe, Cu, Zn and Rb. By using Mann-Whitney U test it was observed that almost all elements presented concentrations with significant differences (α=0.05) between the groups studied.

  8. Extraction of light trapped due to total internal reflection using porous high refractive index nanoparticle films.

    PubMed

    Mao, Peng; Sun, Fangfang; Yao, Hanchao; Chen, Jing; Zhao, Bo; Xie, Bo; Han, Min; Wang, Guanghou

    2014-07-21

    TiO₂ nanoparticle layers composed of columnar TiO₂ nanoparticle piles separated with nanoscale pores were fabricated on the bottom surface of the hemispherical glass prism by performing gas phase cluster beam deposition at glancing incidence. The porosity as well as the refractive index of the nanoparticle layer was precisely tuned by the incident angle. Effective extraction of the light trapped in the substrate due to total internal reflection with the TiO₂ nanoparticle layers was demonstrated and the extraction efficiency was found to increase with the porosity. An enhanced Rayleigh scattering mechanism, which results from the columnar aggregation of the nanoparticles as well as the strong contrast in the refractive index between pores and TiO₂ nanoparticles in the nanoporous structures, was proposed. The porous TiO₂ nanoparticle coatings were fabricated on the surface of GaN LEDs to enhance their light output. A nearly 92% PL enhancement as well as a 30% EL enhancement was observed. For LED applications, the enhanced light extraction with the TiO₂ nanoparticle porous layers can be a supplement to the microscale texturing process for light extraction enhancement. PMID:24927071

  9. Total reflection X-ray fluorescence as a tool for food screening

    NASA Astrophysics Data System (ADS)

    Borgese, Laura; Bilo, Fabjola; Dalipi, Rogerta; Bontempi, Elza; Depero, Laura E.

    2015-11-01

    This review provides a comprehensive overview of the applications of total reflection X-ray fluorescence (TXRF) in the field of food analysis. Elemental composition of food is of great importance, since food is the main source of essential, major and trace elements for animals and humans. Some potentially toxic elements, dangerous for human health may contaminate food, entering the food chain from the environment, processing, and storage. For this reason the elemental analysis of food is fundamental for safety assessment. Fast and sensitive analytical techniques, able to detect major and trace elements, are required as a result of the increasing demand on multi-elemental information and product screening. TXRF is suitable for elemental analysis of food, since it provides simultaneous multi-elemental identification in a wide dynamic range of concentrations. Several different matrices may be analyzed obtaining results with a good precision and accuracy. In this review, the most recent literature about the use of TXRF for the analysis of food is reported. The focus is placed on the applications within food quality monitoring of drinks, beverages, vegetables, fruits, cereals, animal derivatives and dietary supplements. Furthermore, this paper provides a critical outlook on the developments required to transfer these methods from research to the industrial and analytical laboratories contexts.

  10. Elucidation of perovskite film micro-orientations using two-photon total internal reflectance fluorescence microscopy

    DOE PAGESBeta

    Watson, Brianna R.; Yang, Bin; Xiao, Kai; Ma, Ying -Zhong; Doughty, Benjamin L.; Calhoun, Tessa R.

    2015-07-29

    The emergence of efficient hybrid organic-inorganic perovskite photovoltaic materials has caused the rapid development of a variety of preparation and processing techniques designed to maximize their performance. As processing methods continue to emerge, it is important to understand how the optical properties of these materials are affected on a microscopic scale. Here polarization resolved two-photon total internal reflectance microscopy (TIRFM) was used to probe changes in transition dipole moment orientation as a function of thermal annealing time in hybrid organic-inorganic lead iodide based perovskite (CH3NH3PbI3) thin films on glass. These results show that as thermal annealing time is increased themore » distribution of transition moments pointing out-of-plane decreases in favor of forming areas with increased in-plane orientations. As a result, it was also shown through the axial sensitivity of TIRFM that the surface topography is manifested in the signal intensity and can be used to survey aspects of morphology in coincidence with the optical properties of these films.« less

  11. Uranium determination in seawater by total reflection X-ray fluorescence spectrometry

    NASA Astrophysics Data System (ADS)

    Misra, N. L.; Dhara, S.; Mudher, K. D. Singh

    2006-11-01

    A study regarding uranium determination in seawater by total reflection X-ray fluorescence (TXRF) spectrometry is reported. Uranium, present in seawater in concentration of about 3.3 ng/mL, was selectively extracted in diethyl ether and determined by TXRF after its preconcentration by evaporation and subsequent dissolution in a small volume of 1.5% suprapure HNO 3. Yttrium was used as an internal standard. Before using diethyl ether for selective extraction of uranium from seawater, its extraction behavior for different elements was studied using a multielement standard solution having elemental concentrations in 5 ng/mL levels. It was observed that the extraction efficiency of diethyl ether for uranium was about 100% whereas for other elements it was negligible. The detection limit of TXRF method for uranium in seawater samples after pre-concentration step approaches to 67 pg/mL. The concentrations of uranium in seawater samples determined by TXRF are in good agreement with the values reported in the literature. The method shows a precision within 5% (1 σ). The study reveals that TXRF can be used as a fast analytical technique for the determination of uranium in seawater.

  12. Analysis of mineral water from Brazil using total reflection X-ray fluorescence by synchrotron radiation

    NASA Astrophysics Data System (ADS)

    Costa, A. C. M.; Anjos, M. J.; Moreira, S.; Lopes, R. T.; de Jesus, E. F. O.

    2003-12-01

    The total reflection X-ray fluorescence using synchrotron radiation (SRTXRF) has become a competitive technique for the determination of trace elements in samples that the concentrations are lower than 100 ng ml -1. In this work, thirty-seven mineral waters commonly available in supermarkets of Rio de Janeiro, Brazil, were analyzed by SRTXRF. The measurements were performed at the X-Ray Fluorescence Beamline at Brazilian National Synchrotron Light Laboratory (LNLS), in Campinas, São Paulo, using a polychromatic beam with maximum energy of 20 keV for the excitation. Standard solutions with gallium as internal standard were prepared for calibration of the system. Mineral water samples of 10 μl were added to Perspex sample carrier, dried under infrared lamp and analyzed for 200 s measuring time. It was possible to determine the concentrations of the following elements: Si, S, K, Ca, Ti, Cr, Mn, Ni, Cu, Zn, Ge, Rb, Sr, Ba and Pb. The elemental concentration values were compared with the limits established by the Brazilian legislation.

  13. Total reflection X-ray fluorescence analysis using polycapillaries. A comparison with conventional setups

    NASA Astrophysics Data System (ADS)

    Sánchez, Héctor Jorge; Perez, Roberto Daniel; Carvalho, Maria Luisa; Rubio, Marcelo

    2010-12-01

    The possibility of producing parallel X-ray beams with low divergence by means of half monolithic polycapillaries gives the impression to be useful in total reflection X-ray fluorescence (TXRF) experiments. On one hand, the use of polycapillaries facilitates the alignment and the setup of the experiment. As expected, the spectra registered in the experiment shown low background and good signal-noise ratio. On the other hand, the intensity of photons on the samples when polycapillaries are employed is lower than in other configurations, which produces a loss of efficiency for the excitation of the sample mainly for light elements. In this work, different TXRF experiments were carried out and the minimum detection limits attained were compared with the ones obtained from TXRF using polycapillaries. The results indicate that the decrease of intensity produced by polycapillaries is imposing when detection limits are analyzed. Nevertheless, detection limits are better than conventional XRF. The possibility of employing non-symmetrical polycapillaries could eventually improve the detection limits so as to be equivalent to the conventional TXRF setups.

  14. Live-Cell Imaging of the Estrogen Receptor by Total Internal Reflection Fluorescence Microscopy.

    PubMed

    Kisler, Kassandra; Dominguez, Reymundo

    2016-01-01

    Trafficking studies of plasma membrane-localized intracellular estrogen receptors have mainly relied on biochemical and histological techniques to locate the receptor before and after estradiol stimulation. More often than not these experiments were performed using postmortem, lysed, or fixed tissue samples, whose tissue or cellular structure is typically severely altered or at times completely lost, making the definitive localization of estrogen receptors difficult to ascertain. To overcome this limitation we began using total internal reflection fluorescence microscopy (TIRFM) to study the trafficking of plasma membrane estrogen receptors. This real-time imaging approach, described in this chapter, permits observation of live, intact cells while allowing visualization of the steps (in time and spatial distribution) involved in receptor activation by estradiol and movements on and near the membrane. TIRFM yields high-contrast real-time images of fluorescently labeled E6BSA molecules on and just below the cell surface and is ideal for studying estrogen receptor trafficking in living cells. PMID:26585135

  15. N × N polymer matrix switches using thermo-optic total-internal-reflection switch.

    PubMed

    Han, Young-Tak; Shin, Jang-Uk; Park, Sang-Ho; Lee, Hyung-Jong; Hwang, Wol-Yon; Park, Hyo-Hoon; Baek, Yongsoon

    2012-06-01

    We have developed fully non-blocking optical matrix switches using a thermo-optic polymer 1 × 2 total-internal-reflection (TIR) switch as a unit switching element. The TIR switch consists of crossed multimode polymer waveguides and an offset heater electrode at the switching node. The fabricated 4 × 4 and 8 × 8 optical matrix switch chips show excellent switching performances. The insertion losses are less than 2.5 and 4.5 dB for the 4 × 4 and 8 × 8 matrix switches, respectively, and their switching isolations during a turned-off state are higher than 38 dB. The switching time is about 3 ms, and the power consumption for each switching element is below 30 mW. Compact integration of the 4 × 4 and 8 × 8 switch chips is achieved at sizes of 25 mm × 4.25 mm, and 42.4 mm × 5 mm, respectively, through an optimization of the waveguide and heater geometries. PMID:22714356

  16. Determination of trace elements in rainwater by total-reflection X-ray fluorescence

    SciTech Connect

    Stoessel, R.P.; Prange, A.

    1985-12-01

    Three quasi-independent analytical procedures for the determination of trace elements in rainwater are presented, which are based on total-reflection X-ray fluorescence (TXRF), a special variant of energy-dispersive X-ray fluorescence. The three sample preparation techniques compared are (1) direct analysis, (2) preenrichment of the trace elements in rainwater by freeze-drying and redissolution in dilute nitric acid, and (3) a matrix removal and preconcentration procedure by metal chelation, chromatographic adsorption of the metal complexes, and subsequent elution of the metal chelates prior to TXRF measurement. The elements determined are S, K, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Pb, Se, Rb, Sr, Mo, Cd, and Ba. For a measuring time of 1000 s, detection limits down to 5-20 ng/L were achieved for the heavy-metal traces. The limits are slightly higher for iron, nickel, copper, zinc, and lead because of fluctuations in the blan values. The procedures were tested on rainwater samples from the Island of Pellworm (German Bight) containing comparatively low trace-metal contents. Systematic investigations for the characterization of the analytical procedures with regard to blanks, detection limits, precision, and accuracy are described and discussed. The accuracy was checked by independent analyses of duplicate samples using differential pulse anodic stripping voltammetry (KFA Juelich). 17 references, 4 figures, 2 tables.

  17. Application of Near Infrared Reflectance Spectroscopy on Determination of Moisture, Total oil and Protein Contents of In-shell Peanuts

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Moisture, total oil and protein content of peanuts are important factors in peanut grading. A method that could rapidly and nondestructively measure these parameters for in-shell peanuts would be extremely useful. NIR reflectance spectroscopy was used to analyze the moisture, total oil and protein ...

  18. Investigation of the effect of atmospheric dust on the determination of total ozone from the earth's ultraviolet reflectivity measurements, 2

    NASA Technical Reports Server (NTRS)

    Dave, J. V.

    1976-01-01

    Results of a detailed analysis of the simulated measurements for the BUV (Nimbus-4) configuration are described by using a total-ozone estimation procedure. A set of recommendations are discussed for increasing the accuracy and confidence level of the total ozone values estimated from the measurements of the earth's ultraviolet reflectivity at five different wavelengths (BUV configuration). A tentative procedure is also considered for the estimation of total ozone from measurements of reflectivity at six different wavelengths specified in the SBUV/TOMS (Nimbus-G) configuration.

  19. Rapid discrimination of maggots utilising ATR-FTIR spectroscopy.

    PubMed

    Pickering, Claire L; Hands, James R; Fullwood, Leanne M; Smith, Judith A; Baker, Matthew J

    2015-04-01

    Entomological evidence is used in forensic investigations to indicate time since death. The species and age of maggots or flies that are present at the scene can be used when estimating how much time has passed since death. Current methods that are used to identify species and developmental stage of larvae and fly samples are highly subjective, costly and often time consuming processes and require the expertise of an entomologist or species identification via DNA analysis. The use of vibrational spectroscopy, as an alternative identification method, would allow for a quicker, cheaper and less subjective technique and would allow entomological evidence to be used more commonly in the forensic process. This proof of principle study shows the potential for using attenuated total reflection-Fourier transform infrared spectroscopy (ATR-FTIR) as a rapid tool for differentiating between various species of larvae, such as those commonly found at crime scenes. The proposed regime would provide a rapid and valuable tool resulting in reduced time for both species identification and life cycle determination, particularly in forensic situations. PMID:25703014

  20. Application of FTIR-ATR Spectroscopy to Determine the Extent of Lipid Peroxidation in Plasma during Haemodialysis

    PubMed Central

    Oleszko, Adam; Olsztyńska-Janus, Sylwia; Grzeszczuk-Kuć, Karolina; Bujok, Jolanta; Gałecka, Katarzyna; Czerski, Albert; Witkiewicz, Wojciech; Komorowska, Małgorzata

    2015-01-01

    During a haemodialysis (HD), because of the contact of blood with the surface of the dialyser, the immune system becomes activated and reactive oxygen species (ROS) are released into plasma. Particularly exposed to the ROS are lipids and proteins contained in plasma, which undergo peroxidation. The main breakdown product of oxidized lipids is the malondialdehyde (MDA). A common method for measuring the concentration of MDA is a thiobarbituric acid reactive substances (TBARS) method. Despite the formation of MDA in plasma during HD, its concentration decreases because it is removed from the blood in the dialyser. Therefore, this research proposes the Fourier Transform Infrared Attenuated Total Reflectance (FTIR-ATR) spectroscopy, which enables determination of primary peroxidation products. We examined the influence of the amount of hydrogen peroxide added to lipid suspension that was earlier extracted from plasma specimen on lipid peroxidation with use of TBARS and FTIR-ATR methods. Linear correlation between these methods was shown. The proposed method was effective during the evaluation of changes in the extent of lipid peroxidation in plasma during a haemodialysis in sheep. A measurement using the FTIR-ATR showed an increase in plasma lipid peroxidation after 15 and 240 minutes of treatment, while the TBARS concentration was respectively lower. PMID:25961007

  1. ATR-FTIR Spectroscopy Highlights the Problem of Distinguishing Between Exophiala dermatitidis and E. phaeomuriformis Using MALDI-TOF MS.

    PubMed

    Ergin, Çağrı; Gök, Yaşar; Bayğu, Yasemin; Gümral, Ramazan; Özhak-Baysan, Betil; Döğen, Aylin; Öğünç, Dilara; Ilkit, Macit; Seyedmousavi, Seyedmojtaba

    2016-02-01

    The present study compared two chemical-based methods, namely, matrix-assisted laser desorption/ionization-time-of-flight mass spectrometry (MALDI-TOF MS) and attenuated total reflectance-Fourier transform infrared (ATR-FTIR) spectroscopy, to understand the misidentification of Exophiala dermatitidis and Exophiala phaeomuriformis. The study utilized 44 E. dermatitidis and 26 E. phaeomuriformis strains, which were partially treated with strong acids and bases for further evaluation. MALDI-TOF MS and ATR-FTIR spectroscopy data of the two Exophiala species were compared. Data groupings were observed for the chromic acid- and nitric acid-treated species when the black yeast sources were categorized as creosoted-oak sleepers, concrete sleepers, or dishwasher isolates. The MALDI-TOF MS data for the metalloenzyme-containing regions were consistent with the ATR-FTIR spectroscopy data. These results indicated that environmental isolates might contain metals not found in human isolates and might interfere with chemical-based identification methods. Therefore, MALDI-TOF MS reference libraries should be created for clinical strains and should exclude petroleum-associated environmental isolates. PMID:26373644

  2. Tethered bilayer lipid membranes studied by simultaneous attenuated total reflectance infrared spectroscopy and electrochemical impedance spectroscopy

    PubMed Central

    Erbe, Andreas; Bushby, Richard J.; Evans, Stephen D.; Jeuken, Lars J. C.

    2013-01-01

    The formation of tethered lipid bilayer membranes (tBLMs) from unilamelar vesicles of egg yolk phosphatidylcholine (EggPC) on mixed self–assembled monolayers (SAMs) from varying ratios of 6-mercaptohexanol and EO3Cholesteryl on gold has been monitored by simultaneous attenuated total reflectance fourier transform infrared (ATR–FTIR) spectroscopy and electrochemical impedance spectroscopy (EIS). The influence of the lipid orientation (and hence the anisotropy) of lipids on a gold film on the dichroic ratio was studied by simulations of spectra with a matrix method for anisotropic layers. It is shown that for certain tilt angles of the dielectric tensor of the adsorbed anisotropic layer dispersive and negative absorption bands are possible. The experimental data indicates that the structure of the assemblies obtained varies with varying SAM composition. On SAMs with a high content of EO3Cholesteryl, tBLMs with reduced fluidity are formed. For SAMs with high content of 6-mercaptohexanol, the results are consistent with the adsorption of flattened vesicles, while spherical vesicles have been found in a small range of surface compositions. The kinetics of the adsorption process is consistent with the assumption of spherical vesicles as long–living intermediates for surfaces of high 6-mercaptohexanol content. No long–living spherical vesicles have been detected for surfaces with large fraction of EO3Cholesteryl tethers. The observed differences between the surfaces suggest that for the formation of tBLMs (unlike supported BLMs) no critical surface coverage of vesicles is needed prior to lipid bilayer formation. PMID:17388505

  3. Total reflection of x-ray fluorescence (TXRF): a mature technique for environmental chemical nanoscale metrology

    NASA Astrophysics Data System (ADS)

    Borgese, L.; Zacco, A.; Bontempi, E.; Colombi, P.; Bertuzzi, R.; Ferretti, E.; Tenini, S.; Depero, L. E.

    2009-08-01

    Total reflection x-ray fluorescence (TXRF) is a technique well established for chemical analysis of samples deposited as a thin layer. Nowadays it is mainly employed for electronic industry quality control. Recently, very compact and economic TXRF instrumentation was proposed. Combining this with the capability to analyze liquid samples, this technique is suitable to be employed in many different applications, comprising the very critical field of environmental analysis. Comparisons with the standard atomic absorption spectroscopy (AAS) technique show that TXRF is a practical, accurate, and reliable technique. Indeed, round-robin activities have already been started. Despite the efficiency and economy of the developed portable TXRF instrumentation, this is not widely employed for chemical laboratory analysis probably because TXRF is not an officially recognized technique, i.e. it is not yet normative-subjected. This fact could also be due to the long background of analytical applications developed for AAS, ICPS or inductively coupled plasma mass spectroscopy (ICP-MS) up to now. In this paper, we present a work of environmental monitoring of an industrial site, performed by means of bioindicators (lichens). The analysis of trace elements concentration in lichen was usually conducted with spectrophotometric techniques, such as AAS and ICP-MS, which were accepted by common regulations and normative-subjected. In this study, we accomplished a comparative lichen analysis by AAS and TXRF. The reproducibility of the obtained results showed the high correspondence between the two techniques. This comparison highlighted the versatility of the TXRF apparatus that allowed more rapid and simultaneous element detection. The obtained results suggested that this portable TXRF system could be suitable for regulation to produce certificated analysis upto ppb concentrations for some elements.

  4. Using Total Internal Reflection Fluorescence Microscopy To Visualize Rhodopsin-Containing Cells

    PubMed Central

    Keffer, J. L.; Sabanayagam, C. R.; Lee, M. E.; DeLong, E. F.; Hahn, M. W.

    2015-01-01

    Sunlight is captured and converted to chemical energy in illuminated environments. Although (bacterio)chlorophyll-based photosystems have been characterized in detail, retinal-based photosystems, rhodopsins, have only recently been identified as important mediators of light energy capture and conversion. Recent estimates suggest that up to 70% of cells in some environments harbor rhodopsins. However, because rhodopsin autofluorescence is low—comparable to that of carotenoids and significantly less than that of (bacterio)chlorophylls—these estimates are based on metagenomic sequence data, not direct observation. We report here the use of ultrasensitive total internal reflection fluorescence (TIRF) microscopy to distinguish between unpigmented, carotenoid-producing, and rhodopsin-expressing bacteria. Escherichia coli cells were engineered to produce lycopene, β-carotene, or retinal. A gene encoding an uncharacterized rhodopsin, actinorhodopsin, was cloned into retinal-producing E. coli. The production of correctly folded and membrane-incorporated actinorhodopsin was confirmed via development of pink color in E. coli and SDS-PAGE. Cells expressing carotenoids or actinorhodopsin were imaged by TIRF microscopy. The 561-nm excitation laser specifically illuminated rhodopsin-containing cells, allowing them to be differentiated from unpigmented and carotenoid-containing cells. Furthermore, water samples collected from the Delaware River were shown by PCR to have rhodopsin-containing organisms and were examined by TIRF microscopy. Individual microorganisms that fluoresced under illumination from the 561-nm laser were identified. These results verify the sensitivity of the TIRF microscopy method for visualizing and distinguishing between different molecules with low autofluorescence, making it useful for analyzing natural samples. PMID:25769822

  5. Study of antibody/antigen binding kinetics by total internal reflection ellipsometry.

    PubMed

    Baleviciute, Ieva; Balevicius, Zigmas; Makaraviciute, Asta; Ramanaviciene, Almira; Ramanavicius, Arunas

    2013-01-15

    Total internal reflection ellipsometry (TIRE) has been applied for the investigation of (i) kinetics of biosensing layer formation, which was based on the immobilization of fragmented and intact antibodies, and (ii) kinetics of antigen interaction with the immobilized antibodies. It has been demonstrated that ellipsometric parameter Δ(t) showed much higher sensitivity at the initial phase of Au-protein and protein-protein interaction, while the parameter Ψ(t) was more sensitive when the steady-state conditions were established. A new method, which taking into consideration this feature and nonlinear change of Δ(t) and Ψ(t) parameters during various stages of biological layer formation process, was used for the calculation of antibody and antigen adsorption/interaction kinetics. The obtained results were analyzed using a model, which took into account partial reversibility during the formation of both antibody and antigen based monolayers. It was shown that the immobilization rate of antibody during the preparation of the sensing layer was similar for the formation of both intact and fragmented antibody based layers; however, the residence time was 25 times longer for intact antibody based layer formation in comparison to that of fragmented antibody based layer formation. On the contrary, residence time of antigen interaction with immobilized antibodies was about 8 times longer for the sensor based on fragmented antibodies. Moreover, it has been determined that the structural differences of immobilized antibodies (fragmented or intact) significantly influence antibody-antigen interaction rate, the major difference being in the residence time of antigen interaction with both types of immobilized antibodies. PMID:22938839

  6. Optical characterization of a radiochromic film by total reflectance and transmittance measurements.

    PubMed

    Fusi, Franco; Mercatelli, Luca; Marconi, Giacomo; Cuttone, Giacomo; Romano, Giovanni

    2004-07-01

    The GafChromic film (GCF) MD-55-2, a radiochromic material, was examined for its optical properties through total reflectance and transmittance measurements in visible spectrum (400-700 nm). By using a multilayer model of the film and Kubelka-Munk's (KM) theory, absorption and scattering coefficients of the film sensitive layer (K and S, respectively) were obtained from measurements of irradiated and nonirradiated slides. This has allowed calculation of the absorbance A(KM) of the sensitive layer of the GCF. The model easily splits scattering from absorption. Unlike absorption, scattering is essentially insensitive to irradiation dose and decreases slowly as the wavelength increases. The scattering effect is predominant over absorption in the 400-500 nm range, while beyond 600 nm absorption prevails. The A(KM) absorbance of the sensitive layer was calculated using the K coefficient and compared with the optical densities (OD) measured considering only ballistic photons (as in a standard spectrophotometer) as well as the optical densities measured collecting all the transmitted photons (as in many densitometers). The values of A(KM) found were always lower than OD measured by the other methods and they had the best linearity on the whole visible range. These data support the hypothesis that the sensitive layer reacts to irradiation more linearly than that shown by measurements using standard commercial devices. However, in the 600-680 nm range, correction is not very important because absorption is predominant over scattering. When GCF is used for imaging, scattering produces a loss of spatial information. Consequently, it is necessary to collect only ballistic photons and to correct absorbance by K and S coefficients. PMID:15305469

  7. In Situ Fluorescent Protein Imaging with Metal Film-Enhanced Total Internal Reflection Microscopy

    PubMed Central

    Burghardt, Thomas P.; Charlesworth, Jon E.; Halstead, Miriam F.; Tarara, James E.; Ajtai, Katalin

    2006-01-01

    Fluorescence detection of single molecules provides a means to investigate protein dynamics minus ambiguities introduced by ensemble averages of unsynchronized protein movement or of protein movement mimicking a local symmetry. For proteins in a biological assembly, taking advantage of the single molecule approach could require single protein isolation from within a high protein concentration milieu. Myosin cross-bridges in a muscle fiber are proteins attaining concentrations of ∼120 μM, implying single myosin detection volume for this biological assembly is ∼1 attoL (10−18 L) provided that just 2% of the cross-bridges are fluorescently labeled. With total internal reflection microscopy (TIRM) an exponentially decaying electromagnetic field established on the surface of a glass-substrate/aqueous-sample interface defines a subdiffraction limit penetration depth into the sample that, when combined with confocal microscopy, permits image formation from ∼3 attoL volumes. Demonstrated here is a variation of TIRM incorporating a nanometer scale metal film into the substrate/glass interface. Comparison of TIRM images from rhodamine-labeled cross-bridges in muscle fibers contacting simultaneously the bare glass and metal-coated interface show the metal film noticeably reduces both background fluorescence and the depth into the sample from which fluorescence is detected. High contrast metal film-enhanced TIRM images allow secondary label visualization in the muscle fibers, facilitating elucidation of Z-disk structure. Reduction of both background fluorescence and detection depth will enhance TIRM's usefulness for single molecule isolation within biological assemblies. PMID:16565065

  8. Real-time monitoring of NKCC2 endocytosis by total internal reflection fluorescence (TIRF) microscopy.

    PubMed

    Jaykumar, Ankita Bachhawat; Caceres, Paulo S; Sablaban, Ibrahim; Tannous, Bakhos A; Ortiz, Pablo A

    2016-01-15

    The apical Na-K-2Cl cotransporter (NKCC2) mediates NaCl reabsorption by the thick ascending limb (TAL). The amount of NKCC2 at the apical membrane of TAL cells is determined by exocytic delivery, recycling, and endocytosis. Surface biotinylation allows measurement of NKCC2 endocytosis, but it has low time resolution and does not allow imaging of the dynamic process of endocytosis. We hypothesized that total internal reflection fluorescence (TIRF) microscopy imaging of labeled NKCC2 would allow monitoring of NKCC2 endocytosis in polarized Madin-Darby canine kidney (MDCK) and TAL cells. Thus we generated a NKCC2 construct containing a biotin acceptor domain (BAD) sequence between the transmembrane domains 5 and 6. Once expressed in polarized MDCK or TAL cells, surface NKCC2 was specifically biotinylated by exogenous biotin ligase (BirA). We also demonstrate that expression of a secretory form of BirA in TAL cells induces metabolic biotinylation of NKCC2. Labeling biotinylated surface NKCC2 with fluorescent streptavidin showed that most apical NKCC2 was located within small discrete domains or clusters referred to as "puncta" on the TIRF field. NKCC2 puncta were observed to disappear from the TIRF field, indicating an endocytic event which led to a decrease in the number of surface puncta at a rate of 1.18 ± 0.16%/min in MDCK cells, and a rate 1.09 ± 0.08%/min in TAL cells (n = 5). Treating cells with a cholesterol-chelating agent (methyl-β-cyclodextrin) completely blocked NKCC2 endocytosis. We conclude that TIRF microscopy of labeled NKCC2 allows the dynamic imaging of individual endocytic events at the apical membrane of TAL cells. PMID:26538436

  9. Total reflection X-ray fluorescence analysis of airborne silver nanoparticles from fabrics.

    PubMed

    Menzel, Magnus; Fittschen, Ursula Elisabeth Adriane

    2014-03-18

    Ag nanoparticles (NPs) are usually applied to consumer products because of their antimicrobial properties, which are desired in fabrics for sportswear as well as cloth used for cleaning. Hazards to human health from airborne Ag NPs may occur when the NPs are inhaled. NPs are comparable in size to macromolecules and viruses and able to penetrate deep into the lungs, e.g., the alveoli, where they may cause damage to cells and tissue due to their large surface area. In this study, aerosols released form fabrics treated with Ag NPs were collected using a low pressure Berner impactor and analyzed with total reflection X-ray fluorescence (TXRF). We found that the Ag NPs are released primarily in the form of larger particles, mainly 0.13-2 μm, probably attached to fiber material. Using an electron micro probe, single particles could be identified. The detection of backscattered electrons suggests small spots on the particle consist of a heavier element, which most likely is Ag, although the signal in energy-dispersive X-ray spectroscopy (EDX) was below the lower limit of detection (LOD). To achieve LODs necessary for Ag determination, Ar peaks were eliminated by a nitrogen atmosphere provided by the "Picofox-box". This enables linear calibration and quantification of Ag. The LOD was calculated at 0.2 ng (2.0 ppb). Following the TXRF and scanning electron microscopy (SEM)/EDX analysis, the aerosol samples were dissolved in nitric acid and analyzed with ICPMS to successfully confirm the results obtained by the TXRF measurements. PMID:24524688

  10. Measurements of long-range interactions between protein-functionalized surfaces by total internal reflection microscopy.

    PubMed

    Wang, Zhaohui; Gong, Xiangjun; Ngai, To

    2015-03-17

    Understanding the interaction between protein-functionalized surfaces is an important subject in a variety of protein-related processes, ranging from coatings for biomedical implants to targeted drug carriers and biosensors. In this work, utilizing a total internal reflection microscope (TIRM), we have directly measured the interactions between micron-sized particles decorated with three types of common proteins concanavalin A (ConA), bovine serum albumin (BSA), lysozyme (LYZ), and glass surface coated with soy proteins (SP). Our results show that the protein adsorption greatly affects the charge property of the surfaces, and the interactions between those protein-functionalized surfaces depend on solution pH values. At pH 7.5-10.0, all these three protein-functionalized particles are highly negatively charged, and they move freely above the negatively charged SP-functionalized surface. The net interaction between protein-functionalized surfaces captured by TIRM was found as a long-range, nonspecific double-layer repulsion. When pH was decreased to 5.0, both protein-functionalized surfaces became neutral and double-layer repulsion was greatly reduced, resulting in adhesion of all three protein-functionalized particles to the SP-functionalized surface due to the hydrophobic attraction. The situation is very different at pH = 4.0: BSA-decorated particles, which are highly charged, can move freely above the SP-functionalized surfaces, while ConA- and LYZ-decorated particles can only move restrictively in a limited range. Our results quantify these nonspecific kT-scale interactions between protein-functionalized surfaces, which will enable the design of surfaces for use in biomedical applications and study of biomolecular interactions. PMID:25719226

  11. Total reflection X-ray fluorescence spectrometers for multielement analysis: status of equipment

    NASA Astrophysics Data System (ADS)

    Ayala Jiménez, Rony E.

    2001-11-01

    Multielement analysis by total reflection X-ray fluorescence spectrometry has evolved during two decades. At present commercial equipment is available for chemical analysis of all types of biological and mineral samples. The electronic industry has also benefited from scientific and technological developments in this field due to new instrumentation to determine contamination on the surface of silicon wafers (the equipment will not be covered in this paper). The basic components of the spectrometers can be summarized as follows: (a) excitation source; (b) geometric arrangement (optics) for collimation and monochromatization of the primary radiation; (c) X-ray detector; and (d) software for operation of the instrument, data acquisition and spectral deconvolution to determine the concentrations of the elements (quantitative analysis). As an optional feature one manufacturer offers a conventional 45° geometry for direct excitation. Personal communications of the author and commercial brochures available have allowed us to list the components used in TXRF for multielement analysis. Excitation source: high-power sealed X-ray tubes, output from 1300 to 3000 W, different mixed alloy anodes Mo/W are used but molybdenum, tungsten and copper are common; single anode metal ceramic low power X-ray tubes, output up to 40 W. Excitation systems can be customized according to the requirements of the laboratory. Detector: silicon-lithium drifted semiconductor detector liquid nitrogen cooled; or silicon solid state thermoelectrically cooled detector (silicon drift detector SDD and silicon-PIN diode detector). Optics: multilayer monochromator of silicon-tungsten, nickel-carbon or double multilayer monochromator. Electronics: spectroscopy amplifier, analog to digital converter adapted to a PC compatible computer with software in a Windows environment for the whole operation of the spectrometer and for qualitative/quantitative analysis of samples are standard features in the production of this instrument. The detection limits reported in the literature are presented; pricing, analytical capability, ease of operation, calibration and optical alignment as well as technical support are also discussed.

  12. Sensitivity Studies for Space-based Measurement of Atmospheric Total Column Carbon Dioxide Using Reflected Sunlight

    NASA Technical Reports Server (NTRS)

    Mao, Jianping; Kawa, S. Randolph

    2003-01-01

    A series of sensitivity studies is carried out to explore the feasibility of space-based global carbon dioxide (CO2) measurements for global and regional carbon cycle studies. The detection method uses absorption of reflected sunlight in the CO2 vibration-rotation band at 1.58 microns. The sensitivities of the detected radiances are calculated using the line-by-line model (LBLRTM), implemented with the DISORT (Discrete Ordinates Radiative Transfer) model to include atmospheric scattering in this band. The results indicate that (a) the small (approx.1%) changes in CO2 near the Earth's surface are detectable in this CO2 band provided adequate sensor signal-to-noise ratio and spectral resolution are achievable; (b) the radiance signal or sensitivity to CO2 change near the surface is not significantly diminished even in the presence of aerosols and/or thin cirrus clouds in the atmosphere; (c) the modification of sunlight path length by scattering of aerosols and cirrus clouds could lead to large systematic errors in the retrieval; therefore, ancillary aerosol/cirrus cloud data are important to reduce retrieval errors; (d) CO2 retrieval requires good knowledge of the atmospheric temperature profile, e.g. approximately 1K RMS error in layer temperature; (e) the atmospheric path length, over which the CO2 absorption occurs, must be known in order to correctly interpret horizontal gradients of CO2 from the total column CO2 measurement; thus an additional sensor for surface pressure measurement needs to be attached for a complete measurement package.

  13. Prospects for the Use of ATR Inhibitors to Treat Cancer

    PubMed Central

    Wagner, Jill M.; Kaufmann, Scott H.

    2010-01-01

    ATR is an apical kinase in one of the DNA-damage induced checkpoint pathways. Despite the development of inhibitors of kinases structurally related to ATR, as well as inhibitors of the ATR substrate Chk1, no ATR inhibitors have yet been developed. Here we review the effects of ATR downregulation in cancer cells and discuss the potential for development of ATR inhibitors for clinical use.

  14. Rapid detection of melamine adulteration in dairy milk by SB-ATR-Fourier transform infrared spectroscopy.

    PubMed

    Jawaid, Sana; Talpur, Farah N; Sherazi, S T H; Nizamani, Shafi M; Khaskheli, Abid A

    2013-12-01

    Melamine is a nitrogenous chemical substance used principally as a starting material for the manufacture of synthetic resins. Due to its very high proportion of nitrogen melamine has been added illegitimately to foods and feeds to increase the measured protein content, which determines the value of the product. These issues prompted private as well as governmental laboratories to develop methods for the analysis of melamine in a wide variety of food products and ingredients. Owing to this fact present study is aimed to use single bounce attenuated total reflectance (SB-ATR) Fourier transform infrared spectroscopy (FTIR) method as an effective rapid tool for the detection and quantification of melamine in milk (liquid and powder). Partial least-squares (PLS) models were established for correlating spectral data to melamine concentration with R(2)>0.99, and RMSEC 0.370. Linear calibration curves were obtained over the calibration range of 25-0.0625%. The LOD and LOQ of the method was 0.00025% (2.5 ppm) and 0.0015% (15 ppm) respectively. Proposed SB-ATR-FTIR method requires little or no sample preparation with an assay time of 1-2 min. PMID:23871060

  15. Evanescent wave absorption measurements of corroded materials using ATR and optical fibers

    NASA Astrophysics Data System (ADS)

    Namkung, Juock; Hoke, Mike; Schwartz, Andy

    2011-06-01

    The purpose of this research effort is to develop an in-situ corrosion sensing capability. The technique will permit detection of corrosion on and within aircraft structures. This includes component junctions that are susceptible to corrosion but which are not accessible for visual inspection. The prototype experimental configuration we are developing includes long wave infrared transmitting optical fiber probes interfaced with a Fourier Transform Infrared (FTIR) interferometer for evanescent wave absorption spectroscopic measurements. The mature and fielded technique will allow periodic remote sensing for detection of corrosion and for general onboard aircraft structural health monitoring. An experimental setup using an Attenuated Total Reflection (ATR) crystal integrated with an FTIR spectrometer has been assembled. Naturally occurring corrosion including Aluminum Hydroxide [Al(OH)3] is one of the main corrosion products of aluminum the principle structural metal of aircraft. Absorption spectra of our model corrosion product, pure Al(OH)3, have been collected with this ATR/FTIR experimental setup. The Al(OH)3spectra serve as reference spectral signatures. The spectra of corrosion samples from a simulated corrosion process have been collected and compared with the reference Al(OH)3 spectra. Also absorption spectra of naturally occurring corrosion collected from a fielded corroded aircraft part have been obtained and compared with the spectra from the simulated corrosion.

  16. The influence of LO-TO splitting on vSO 2 exciton bands in IR and ATR spectra of crystalline dimethyl sulphone

    NASA Astrophysics Data System (ADS)

    Remizov, A. B.

    1997-06-01

    The IR and attenuated total reflection (ATR) spectra of polycrystalline solids and oriented specimens of dimethyl sulphone (CH 3) 2SO 2(DMS) and DMS- d6 have been measured. Several anomalies are seen in the range of the v SO 2 stretching bands. Among these are the appearance of v SO 2 bands in the ATR spectra outside the contours of those bands in the IR spectra. Another anomaly was found to be in the variations of the v SO 2 band contours and maxima in the IR spectra of oriented specimens. The experimental data can be explained within the framework of the LO-TO splitting (a difference in frequency of the longitudinal and transverse vibrations).

  17. In situ ATR-FTIR study of H2O and D2O adsorption on TiO2 under UV irradiation.

    PubMed

    Belhadj, Hamza; Hakki, Amer; Robertson, Peter K J; Bahnemann, Detlef W

    2015-09-21

    The adsorption of water and deuterium oxide on TiO2 surfaces was investigated in the dark as well as under UV(A) irradiation using in situ ATR-FTIR spectroscopy under oxygen and oxygen free conditions. Adsorption of H2O-D2O mixtures revealed an isotopic exchange reaction occurring onto the surface of TiO2 in the dark. Under UV(A) irradiation, the amount of both OH and OD groups was found to be increased by the presence of molecular oxygen. Furthermore, the photocatalytic formation of hydroperoxide under oxygenated condition has been recorded utilizing Attenuated Total Reflection Fourier Transformed Infrared (ATR-FTIR) spectroscopy which appeared as new band at 3483 cm(-1). Different possible mechanisms are discussed in terms of the source of hydroxyl groups formed and/or hydration water on the TiO2 surface for the photocatalytic reaction and photoinduced hydrophilicity. PMID:26266701

  18. Excitation of plasmonic terahertz photovoltaic effects in a periodic two-dimensional electron system by the attenuated total reflection method

    SciTech Connect

    Fateev, D. V. Mashinsky, K. V.; Bagaeva, T. Yu.; Popov, V. V.

    2015-01-15

    The problem of the rectification of terahertz radiation due to plasmonic nonlinearities in a periodic two-dimensional electron system upon the excitation of plasma oscillations by the attenuated total reflection method is solved. This model allows the independent study of different plasmonic rectification mechanisms, i.e., plasmonic electron drag and plasmonic ratchet effects.

  19. Development of off-line layer chromatographic and total reflection X-ray fluorescence spectrometric methods for arsenic speciation

    NASA Astrophysics Data System (ADS)

    Mihucz, Victor G.; Móricz, Ágnes M.; Kröpfl, Krisztina; Szikora, Szilvia; Tatár, Enikő; Parra, Lué Merú Marcó; Záray, Gyula

    2006-11-01

    Rapid and low cost off-line thin layer chromatography-total reflection X-ray fluorescence spectrometry and overpressured thin layer chromatography-total reflection X-ray fluorescence spectrometry methods have been developed for separation of 25 ng of each As(III), As(V), monomethyl arsonic acid and dimethylarsinic acid applying a PEI cellulose stationary phase on plastic sheets and a mixture of acetone/acetic acid/water = 2:1:1 (v/v/v) as eluent system. The type of eluent systems, the amounts (25-1000 ng) of As species applied to PEI cellulose plates, injection volume, development distance, and flow rate (in case of overpressured thin layer chromatography) were taken into consideration for the development of the chromatographic separation. Moreover, a microdigestion method employing nitric acid for the As spots containing PEI cellulose scratched from the developed plates divided into segments was developed for the subsequent total reflection X-ray fluorescence spectrometry analysis. The method was applied for analysis of root extracts of cucumber plants grown in As(III) containing modified Hoagland nutrient solution. Both As(III) and As(V) were detected by applying the proposed thin layer chromatography/overpressured thin layer chromatography-total reflection X-ray fluorescence spectrometry methods.

  20. A plastic total internal reflection-based photoluminescence device for enzymatic biosensors

    NASA Astrophysics Data System (ADS)

    Thakkar, Ishan G.

    Growing concerns for quality of water, food and beverages in developing and developed countries drive sizeable markets for mass-producible, low cost devices that can measure the concentration of contaminant chemicals in water, food, and beverages rapidly and accurately. Several fiber-optic enzymatic biosensors have been reported for these applications, but they exhibit very strong presence of scattered excitation light in the signal for sensing, requiring expensive thin-film filters, and their non-planar structure makes them challenging to mass-produce. Several other planar optical waveguide-based biosensors prove to be relatively costly and more fragile due to constituent materials and the techniques involved in their fabrication. So, a plastic total internal reflection (TIR)-based low cost, low scatter, field-portable device for enzymatic biosensors is fabricated and demonstrated. The design concept of the TIR-based photoluminescent enzymatic biosensor device is explained. An analysis of economical materials with appropriate optical and chemical properties is presented. PMMA and PDMS are found to be appropriate due to their high chemical resistance, low cost, high optical transmittance and low auto-fluorescence. The techniques and procedures used for device fabrication are discussed. The device incorporated a PMMA-based optical waveguide core and PDMS-based fluid cell with simple multi-mode fiber-optics using cost-effective fabrication techniques like molding and surface modification. Several techniques of robustly depositing photoluminescent dyes on PMMA core surface are discussed. A pH-sensitive fluorescent dye, fluoresceinamine, and an O2-sensitive phosphorescent dye, Ru(dpp) both are successfully deposited using Si-adhesive gel-based as well as HydroThane-based deposition methods. Two different types of pH-sensors using two different techniques of depositing fluoresceinamine are demonstrated. Also, the effect of concentration of fluoresceinamine-dye molecules on fluorescence intensity and scattered excitation light intensity is investigated. The fluorescence intensity to the scattered excitation light intensity ratio for dye deposition is found to increase with increase in concentration. However, both the absolute fluorescence intensity and absolute scatter intensity are found to decrease in different amounts with an increase in concentration. An enzymatic hydrogen peroxide (H2O2) sensor is made and demonstrated by depositing Ruthenium-based phosphorescent dye (Ru(dpp) 3) and catalase-enzyme on the surface of the waveguide core. The O 2-sensitive phosphorescence of Ru(dpp)3 is used as a transduction signal and the catalase-enzyme is used as a bio-component for sensing. The H2O2 sensor exhibits a phosphorescence signal to scattered excitation light ratio of 100+/-18 without filtering. The unfiltered device demonstrates a detection limit of (2.20+/-0.6) microM with the linear range from 200microM to 20mM. An enzymatic lactose sensor is designed and characterized using Si-adhesive gel based Ru(dpp)3 deposition and oxidase enzyme. The lactose sensor exhibits the linear range of up to 0.8mM, which is too small for its application in industrial process control. So, a flow cell-based sensor device with a fluid reservoir is proposed and fabricated to increase the linear range of the sensor. Also, a multi-channel pH-sensor device with four channels is designed and fabricated for simultaneous sensing of multiple analytes.

  1. Two-dimensional attenuated total reflection infrared correlation spectroscopy study of desorption process of water-soaked cotton fibers

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Two-dimensional (2D) correlation analysis was applied to characterize the ATR spectral intensity fluctuations of native cotton fibers with various water contents. Prior to 2D analysis, the spectra were leveled to zero at the peak intensity of 1800 cm-1 and then were normalized at the peak intensity ...

  2. Mobility and surfactant migration in EA/MAA latex films; ATR FT-IR spectroscopic study

    SciTech Connect

    Thorstenson, T.A.; Tebelius, L.K.; Urban, M.W.

    1993-12-31

    Although numerous factors such as compatibility, mechanical deformation, and the nature of the substrate have been addressed with respect to surfactant migration and distribution within latex films, latex suspension stability and the effects of particle flocculation are also key issues. In this paper, surfactant behavior in an ethyl acrylate/methacrylic acid/sodium dioctyl sulfosuccinate (EA/MAA/SDOSS) latex system is monitored as a function of stability of the liquid latex suspensions. Particle size data obtained using light scattering reveals an appreciable degree of flocculation over the period of study. It is found that flocculation is paralleled by a significantly increased degree of interfacial surfactant enrichment, a monitored by attenuated total reflectance Fourier transform infrared spectroscopy (ATR FT-IR). It is concluded that the enhanced surfactant exudation observed for flocculated latexes is due to displacement of adsorbed surfactant during the course of flocculation.

  3. FTIR-ATR evaluation of topical skin protectants useful for sulfur mustard and related compounds

    NASA Astrophysics Data System (ADS)

    Braue, Ernest H., Jr.; Litchfield, Marty R.; Bangledorf, Catherine R.; Rieder, Robert G.

    1992-03-01

    The US Army has a need to develop topical protectants that can decrease the effects of cutaneous exposure to chemical warfare (CW) agents. Such materials would enhance a soldier's ability to carry out the mission in a chemically hostile environment, would lessen the burden on medical personnel, and may allow the casualties to return to duty in a shorter period of time than might otherwise be possible. In a preliminary report (E. H. Braue, Jr. and M. G. Pannella, Applied Spectrosc., 44, 1061 (1990)), we described a unique analytical method using FT-IR spectroscopy and the horizontal attenuated total reflectance (ATR) accessory for evaluating the effectiveness of topical skin protectants (TSPs) against penetration by chemical agents. We now describe the application of this method to the chemical warfare agent sulfur mustard (HD).

  4. - and Longwave Infrared Total and Diffuse Reflectance Measurements Using AN Integrating Sphere with a Two-Sample Design

    NASA Astrophysics Data System (ADS)

    Blake, Thomas A.; Johnson, Timothy J.; Juette, Michael; Simon, Arno

    2010-06-01

    We report here improved methodologies for the use of the Bruker A 562-G integrating sphere for quantitative total and diffuse reflectance measurements. The sphere has an internal diameter of 75 mm and the interior surface is coated with matte gold. It has an input port (20 mm diameter), top (32 mm) and bottom (19 mm) sample ports, all on a sphere circumference defined by a vertical plane than includes the sphere center, and a baffled port (10 mm) for an MCT detector (2 mm x 2 mm), that is on a sphere circumference defined by a horizontal plane that includes the sphere center. An interior flip mirror is used to direct light from the input port to either the top or bottom sample ports. The sphere sits in the sample compartment of a benchtop Fourier transform spectrometer. Total reflectance measurements are made by placing the sample in one of the sample ports and blocking the other sample port with a matte gold reference material, recording spectra with the flip mirror pointed towards the sample and then towards the reference material, and then ratio-ing the two spectra. Using this method excellent agreement (< 2% difference) was observed between measurements made using the Bruker sphere and FTIR and reported values for five NIST-calibrated total reflectance standards. Diffuse reflectance measurements are made by placing the sample in one of the sample ports and leaving the other port open to allow the specular reflection component of the sample to exit the sphere, recording spectra with the flip mirror pointing towards the sample and then towards a point on the sphere wall. The two spectra are again ratioed. The diffuse spectrum is thus the total spectrum less the specular component. In the shortwave infrared, where there is sufficient overlap, total and diffuse measurements using the Bruker sphere and FTIR compare favorably with results from a Varian Spectralon-coated integrating sphere and Cary 5000i spectrometer for a number of different materials.

  5. Total reflection X-ray fluorescence trace mercury determination by trapping complexation: Application in advanced oxidation technologies

    NASA Astrophysics Data System (ADS)

    Custo, Graciela; Litter, Marta I.; Rodríguez, Diana; Vázquez, Cristina

    2006-11-01

    It is well known that Hg species cause high noxious effects on the health of living organisms even at very low levels (5 μg/L). Quantification of this element is an analytical challenge due to the peculiar physicochemical properties of all Hg species. The regulation of the maximal allowable Hg concentration led to search for sensitive methods for its determination. Total reflection X-ray fluorescence is a proved instrumental analytical tool for the determination of trace elements. In this work, the use of total reflection X-ray fluorescence for Hg quantification is investigated. However, experimental determination by total reflection X-ray fluorescence requires depositing a small volume of sample on the reflector and evaporation of the solvent until dryness to form a thin film. Because of volatilization of several Hg forms, a procedure to capture these volatile species in liquid samples by using complexing agents is proposed. Acetate, oxalic acid, ethylenediaminetetracetic acid and ammonium pyrrolidine-dithiocarbamate were assayed for trapping the analytes into the solution during the preparation of the sample and onto the reflector during total reflection X-ray fluorescence measurements. The proposed method was applied to evaluate Hg concentration during TiO 2-heterogeneous photocatalysis, one of the most known advanced oxidation technologies. Advanced oxidation technologies are processes for the treatment of effluents in waters and air that involve the generation of very active oxidative and reductive species. In heterogeneous photocatalysis, Hg is transformed to several species under ultraviolet illumination in the presence of titanium dioxide. Total reflection X-ray fluorescence was demonstrated to be applicable in following the extent of the heterogeneous photocatalysis reaction by determining non-transformed Hg in the remaining solution.

  6. Rapid monitoring of grapevine reserves using ATR-FT-IR and chemometrics.

    PubMed

    Schmidtke, Leigh M; Smith, Jason P; Müller, Markus C; Holzapfel, Bruno P

    2012-06-30

    Predictions of grapevine yield and the management of sugar accumulation and secondary metabolite production during berry ripening may be improved by monitoring nitrogen and starch reserves in the perennial parts of the vine. The standard method for determining nitrogen concentration in plant tissue is by combustion analysis, while enzymatic hydrolysis followed by glucose quantification is commonly used for starch. Attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FT-IR) combined with chemometric modelling offers a rapid means for the determination of a range of analytes in powdered or ground samples. ATR-FT-IR offers significant advantages over combustion or enzymatic analysis of samples due to the simplicity of instrument operation, reproducibility and speed of data collection. In the present investigation, 1880 root and wood samples were collected from Shiraz, Semillon and Riesling vineyards in Australia and Germany. Nitrogen and starch concentrations were determined using standard analytical methods, and ATR-FT-IR spectra collected for each sample using a Bruker Alpha instrument. Samples were randomly assigned to either calibration or test data sets representing two thirds and one third of the samples respectively. Signal preprocessing included extended multiplicative scatter correction for water and carbon dioxide vapour, standard normal variate scaling with second derivative and variable selection prior to regression. Excellent predictive models for percent dry weight (DW) of nitrogen (range: 0.10-2.65% DW, median: 0.45% DW) and starch (range: 0.25-42.82% DW, median: 7.77% DW) using partial least squares (PLS) or support vector machine (SVM) analysis for linear and nonlinear regression respectively, were constructed and cross validated with low root mean square errors of prediction (RMSEP). Calibrations employing SVM-regression provided the optimum predictive models for nitrogen (R(2)=0.98 and RMSEP=0.07% DW) compared to PLS regression (R(2)=0.97 and RMSEP=0.08% DW). The best predictive models for starch was obtained using PLS regression (R(2)=0.95 and RSMEP=1.43% DW) compared to SVR (R(2)=0.95; RMSEP=1.56% DW). The RMSEP for both nitrogen and starch is below the reported seasonal flux for these analytes in Vitis vinifera. Nitrogen and starch concentrations in grapevine tissues can thus be accurately determined using ATR-FT-IR, providing a rapid method for monitoring vine reserve status under commercial grape production. PMID:22688030

  7. Analysis of moisture content, total oil and fatty acid composition by NIR reflectance spectroscopy: a review

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Near Infrared (NIR) Reflectance spectroscopy has established itself as an important analytical technique in the field of food and agriculture. It is quicker and easier to use and does not require processing the samples with corrosive chemicals such as acids or hydroxides. However, for a long time t...

  8. Modeling changes in the hemoglobin concentration of skin with total diffuse reflectance spectroscopy

    NASA Astrophysics Data System (ADS)

    Glennie, Diana L.; Hayward, Joseph E.; Farrell, Thomas J.

    2015-03-01

    The ability to monitor changes in the concentration of hemoglobin in the blood of the skin in real time is a key component to personalized patient care. Since hemoglobin has a unique absorption spectrum in the visible light range, diffuse reflectance spectroscopy is the most common approach. Although the collection of the diffuse reflectance spectrum with an integrating sphere (IS) has several calibration challenges, this collection method is sufficiently user-friendly that it may be worth overcoming the initial difficulty. Once the spectrum is obtained, it is commonly interpreted with a log-inverse-reflectance (LIR) or "absorbance" analysis that can only accurately monitor changes in the hemoglobin concentration when there are no changes to the nonhemoglobin chromophore concentrations which is not always the case. We address the difficulties associated with collection of the diffuse reflectance spectrum with an IS and propose a model capable of retrieving relative changes in hemoglobin concentration from the visible light spectrum. The model is capable of accounting for concentration changes in the nonhemoglobin chromophores and is first characterized with theoretical spectra and liquid phantoms. The model is then used in comparison with a common LIR analysis on temporal measurements from blanched and reddened human skin.

  9. Critical coupling layer thickness for positive or negative Goos-Hänchen shifts near the excitation of backward surface polaritons in Otto-ATR systems

    NASA Astrophysics Data System (ADS)

    Zeller, Mariana A.; Cuevas, Mauro; Depine, Ricardo A.

    2015-05-01

    We present a theoretical analysis of the lateral displacement (Goos-Hänchen shift) of spatially limited beams reflected from attenuated total reflection (ATR) devices in the Otto configuration when backward surface plasmon polaritons are excited at the interface between a positive refractive index slab and a semi-infinite metamaterial with a negative refractive index. First, the stationary phase approximation and a phenomenological model based on the properties of the complex poles and zeroes of the reflection coefficient are used to demonstrate that: (i) the excitation of backward surface waves can lead to both negative and positive (and not exclusively negative) Goos-Hänchen shifts, and (ii) the sign of the shift depends on whether the value of the coupling layer thickness is higher or lower than a critical value characteristic of the ATR structure. Then, these findings are verified through rigorous calculations of the spatial structure of the reflected beam. For incident beams with a Gaussian profile, the lateral shift calculated as the first moment of the field distribution of the reflected beam agrees quite well with the predictions of approximate analysis. Near the resonant excitation of the backward surface plasmon polariton, large (negative or positive) Goos-Hänchen shifts are obtained, along with a splitting of the reflected beam.

  10. Controllable transmission and total reflection through an impedance-matched acoustic metasurface

    NASA Astrophysics Data System (ADS)

    Mei, Jun; Wu, Ying

    2014-12-01

    A general design paradigm for a novel type of acoustic metasurface is proposed by introducing periodically repeated supercells on a rigid thin plate, where each supercell contains multiple cut-through slits that are filled with materials possessing different refractive indices but the same impedance as that of the host medium. When the wavelength of the incident wave is smaller than the periodicity, the direction of the transmitted wave with nearly unity transmittance can be chosen by engineering the phase discontinuities along the transverse direction. When the wavelength is larger than the periodicity, even though the metasurface is impedance matched to the host medium, most of the incident energy is reflected back and the remaining portion is converted into a surface-bound mode. We show that both the transmitted wave control and the high reflection with the surface mode excitation can be interpreted by a unified analytic model based on mode-coupling theory. Our general design principle not only supplies the functionalities of reflection-type acoustic metasurfaces, but also exhibits unprecedented flexibility and efficiency in various domains of wave manipulation for possible applications in fields like refracting, collimating, focusing or absorbing wave energy.

  11. Reflections.

    ERIC Educational Resources Information Center

    Noah, Harold J.

    1987-01-01

    A former member of the IEA's global "invisible college" reflects on some aspects of the organization's work and findings, pointing out that international differences in achievement are generally smaller than within-nation differences and that national differences in context and input are associated with broadly similar outcomes. Also reviews and…

  12. ATM and ATR signaling at a glance.

    PubMed

    Awasthi, Poorwa; Foiani, Marco; Kumar, Amit

    2015-12-01

    ATM and ATR signaling pathways are well conserved throughout evolution and are central to the maintenance of genome integrity. Although the role of both ATM and ATR in DNA repair, cell cycle regulation and apoptosis have been well studied, both still remain in the focus of current research activities owing to their role in cancer. Recent advances in the field suggest that these proteins have an additional function in maintaining cellular homeostasis under both stressed and non-stressed conditions. In this Cell Science at a Glance article and the accompanying poster, we present an overview of recent advances in ATR and ATM research with emphasis on that into the modes of ATM and ATR activation, the different signaling pathways they participate in - including those that do not involve DNA damage - and highlight their relevance in cancer. PMID:26567218

  13. An Evaluation of Total Solar Reflectance and Spectral Band Ratioing Techniques for Estimating Soil Water Content

    NASA Technical Reports Server (NTRS)

    Reginato, R. J.; Vedder, J. F.; Idso, S. B.; Jackson, R. D.; Blanchard, M. B.; Goettelman, R.

    1977-01-01

    For several days in March of 1975, reflected solar radiation measurements were obtained from smooth and rough surfaces of wet, drying, and continually dry Avondale loam at Phoenix, Arizona, with pyranometers located 50 cm above the ground surface and a multispectral scanner flown at a 300-m height. The simple summation of the different band radiances measured by the multispectral scanner proved equally as good as the pyranometer data for estimating surface soil water content if the multispectral scanner data were standardized with respect to the intensity of incoming solar radiation or the reflected radiance from a reference surface, such as the continually dry soil. Without this means of standardization, multispectral scanner data are most useful in a spectral band ratioing context. Our results indicated that, for the bands used, no significant information on soil water content could be obtained by band ratioing. Thus the variability in soil water content should insignificantly affect soil-type discrimination based on identification of type-specific spectral signatures. Therefore remote sensing, conducted in the 0.4- to 1.0-micron wavelength region of the solar spectrum, would seem to be much More suited to identifying crop and soil types than to estimating of soil water content.

  14. Approximate analytical solution for waveguide excitation of a plane dielectric layer by a Gaussian beam at frustrated total internal reflection.

    PubMed

    Serdyuk, Vladimir; Rudnitsky, Anton

    2015-05-01

    We present an approximate 2D asymptotic analytic theory of light field excitation in a plane thin dielectric layer under conditions of frustrated total internal reflection, when an inclined Gaussian beam, falling from a triangular prism, excites a decaying field in air spacing between a prism and a plane dielectric. Ignoring the radiation scattering on the sharp edges of a prism, we have obtained the formulas that allow us to compute spatial structures of an electromagnetic field in every point of space and to estimate the integral efficiency of waveguide mode excitation in a plane dielectric layer and the total energy of a reflected beam. It is shown that the width of an initial Gaussian beam has an effect on waveguide mode intensity. PMID:26366908

  15. Compositional features of cotton plant biomass fractions characterized by attenuated total reflection Fourier transform infrared spectroscopy

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Cotton is one of the most important and widely grown crops in the world. In addition to natural textile fiber production as a primary purpose, it yields a high grade vegetable oil for human consumption and also carbohydrate fiber and protein byproducts for animal feed. In this work, attenuated total...

  16. Investigation of effect of different total area coverage values of inks on reflection spectra and color gamut

    NASA Astrophysics Data System (ADS)

    Spiridonov, I.; Shopova, M.; Boeva, R.

    2013-03-01

    The paper presents investigation of the effect of different values of total area coverage of inks (TAC) on reflection spectra and color gamut. Total area coverage is a key factor for achieving of maximal volume of color gamut. The reflection spectra of color surfaces in entire visible spectrum are used for determination the effect of different values of TAC. For study the effect of TAC values on color gamut, we have used special test form that contains many components and test charts with over 1500 color patches. According to measurement of reflectance spectrum of test charts, we have compared the color gamuts with different values of TAC to obtain comprehensive information of all colors, which could be reproduced in the specific conditions. In addition we have converted the reflection spectra data to CIE L*a*b* coordinates, and we have calculated the color difference ΔE* ab to determine the effect of TAC on color reproduction accuracy. The main goal of this study is development of methodology, which gives objective and analytical assessment, for determining the optimal value of total area coverage (TAC). A practical implementation of the correct and optimal value of total area coverage should improve the printability, better ink layers adhesion, biggest number of trapping values and reduce the quantity of process inks. The optimal value of the TAC determined by this new methodology helps to achieve a significant reduction of ink cost and a maximal color gamut volume, i.e. improve the quality of printed image and reduce financial costs.

  17. Methods for the measurement of the refractive index of MeV photons using total internal and external reflection

    NASA Astrophysics Data System (ADS)

    Aginian, M. A.; Ispirian, K. A.; Ispiryan, M.

    2014-05-01

    Recently it has been theoretically and experimentally shown that for 1-10 MeV and 1-2 MeV photons, respectively, the refractive index of Si is greater than 1. Taking into account the difficulties of the carried out experiment it is proposed to measure directly the refractive index of Si and other materials detecting the total internal and external reflections.

  18. A study of surface film formation on LiNi0.8Co0.15Al0.05O2 cathodes u sing attenuated total reflection infrared spectroscopy

    SciTech Connect

    Song, S.-W.; Zhuang, G.V.; Ross Jr., P.N.

    2004-01-19

    The surface films formed on commercial LiNi0.8Co0.15Al0.05O2 cathodes (ATD Gen2) charged from 3.75V to 4.2V vs. Li/Li+ in EC:DEC - 1M LiPF6 were analyzed using ex-situ Fourier transform infrared spectroscopy (FTIR) with the attenuated total reflection (ATR) technique. A surface layer of Li2CO3 is present on the virgin cathode, probably from reaction of the active material with air during the cathode preparation procedure. The Li2CO3 layer disappeared even after soaking in the electrolyte, indicating that the layer dissolved into the electrolyte possibly even before potential cycling of the electrode. IR features only from the binder (PVdF) and a trace of polyamide from the Al current collector were observed on the surfaces of cathodes charged to below 4.2 V, i.e., no surface species from electrolyte oxidation. Some new IR features were, however, found on the cathode charged to 4.2 V and higher. An electrolyte oxidation product was observed that appeared to contain dicarbonyl anhydride and (poly)ester functionalities. The reaction appears to be an indirect electrochemical oxidation with overcharging (removal of > 0.6 Li ions) destabilizing oxygen in the oxide lattice resulting in oxygen transfer to the solvent molecules.

  19. Rydberg and π-π* transitions in film surfaces of various kinds of nylons studied by attenuated total reflection far-ultraviolet spectroscopy and quantum chemical calculations: peak shifts in the spectra and their relation to nylon structure and hydrogen bondings.

    PubMed

    Morisawa, Yusuke; Yasunaga, Manaka; Sato, Harumi; Fukuda, Ryoichi; Ehara, Masahiro; Ozaki, Yukihiro

    2014-10-01

    Attenuated total reflection far-ultraviolet (ATR-FUV) spectra in the 145-260 nm region were measured for surfaces (thickness 50-200 nm) of various kinds of nylons in cast films to explore their electronic transitions in the FUV region. ATR-FUV spectra show two major bands near 150 and 200 nm in the surface condensed phase of nylons. Transmittance (Tr) spectra were also observed in particular for the analysis of valence excitations. Time-dependent density functional theory (TD-DFT/CAM-B3LYP) calculations were carried out using the model systems to provide the definitive assignments of their absorption spectra and to elucidate their peak shifts in several nylons, in particular, focusing on their crystal alignment structures and intermolecular hydrogen bondings. Two major bands of nylon films near 150 and 200 nm are characterized as σ-Rydberg 3p and π-π* transitions of nylons, respectively. These assignments are also coherent with those of liquid n-alkanes (n = 5-14) and liquid amides observed previously. The Rydberg transitions are delocalized over the hydrocarbon chains, while the π-π* transitions are relatively localized at the amide group. Differences in the peak positions and intensity were found in both ATR- and Tr-FUV spectra for different nylons. A red-shift of the π-π* amide band in the FUV spectra of nylon-6 and nylon-6/6 models in α-form is attributed to the crystal structure pattern and the intermolecular hydrogen bondings, which result in the different delocalization character of the π-π* transitions and transition dipole coupling. PMID:25203613

  20. Two-Dimensional Standing Wave Total Internal Reflection Fluorescence Microscopy: Superresolution Imaging of Single Molecular and Biological Specimens

    PubMed Central

    Chung, Euiheon; Kim, Daekeun; Cui, Yan; Kim, Yang-Hyo; So, Peter T. C.

    2007-01-01

    The development of high resolution, high speed imaging techniques allows the study of dynamical processes in biological systems. Lateral resolution improvement of up to a factor of 2 has been achieved using structured illumination. In a total internal reflection fluorescence microscope, an evanescence excitation field is formed as light is total internally reflected at an interface between a high and a low index medium. The <100 nm penetration depth of evanescence field ensures a thin excitation region resulting in low background fluorescence. We present even higher resolution wide-field biological imaging by use of standing wave total internal reflection fluorescence (SW-TIRF). Evanescent standing wave (SW) illumination is used to generate a sinusoidal high spatial frequency fringe pattern on specimen for lateral resolution enhancement. To prevent thermal drift of the SW, novel detection and estimation of the SW phase with real-time feedback control is devised for the stabilization and control of the fringe phase. SW-TIRF is a wide-field superresolution technique with resolution better than a fifth of emission wavelength or ?100 nm lateral resolution. We demonstrate the performance of the SW-TIRF microscopy using one- and two-directional SW illumination with a biological sample of cellular actin cytoskeleton of mouse fibroblast cells as well as single semiconductor nanocrystal molecules. The results confirm the superior resolution of SW-TIRF in addition to the merit of a high signal/background ratio from TIRF microscopy. PMID:17483188

  1. Sensitivity studies for space-based measurement of atmospheric total column carbon dioxide by reflected sunlight.

    PubMed

    Mao, Jianping; Kawa, S Randolph

    2004-02-01

    The feasibility of making space-based carbon dioxide (CO2) measurements for global and regional carbon-cycle studies is explored. With the proposed detection method, we use absorption of reflected sunlight near 1.58 microm. The results indicate that the small (degrees 1%) changes in CO2 near the Earth's surface are detectable provided that an adequate sensor signal-to-noise ratio and spectral resolution are achievable. Modification of the sunlight path by scattering of aerosols and cirrus clouds could, however, lead to systematic errors in the CO2 column retrieval; therefore ancillary aerosol and cloud data are important to reduce errors. Precise measurement of surface pressure and good knowledge of the atmospheric temperature profile are also required. PMID:14960086

  2. Comparison of HEU and LEU Fuel Neutron Spectrum for ATR Fuel Element and ATR Flux-Trap Positions

    SciTech Connect

    G. S. Chang

    2008-10-01

    The Advanced Test Reactor (ATR) is a high power and high neutron flux research reactor operating in the United States. Powered with highly enriched uranium (HEU), the ATR has a maximum thermal power rating of 250 MWth. Because of the high total core power and high neutron flux, the ATR is an ideal candidate for assessing the feasibility of converting an HEU driven reactor to a low-enriched core. An optimized low-enriched uranium (LEU) (U-10Mo) core conversion case, which can meet the project requirements, has been selected. However, LEU contains a significant quantity of high density U-238 (80.3 wt.%), which will harden the neutron spectrum in the core region. Based on the reference ATR HEU and the optimized LEU full core plate-by-plate (PBP) models, the present work investigates and compares the neutron spectra differences in the fuel element (FE), Northeast flux trap (NEFT), Southeast flux trap (SEFT), and East flux trap (EFT) positions. A detailed PBP MCNP ATR core model was developed and validated for fuel cycle burnup comparison analysis. The current ATR core with HEU U 235 enrichment of 93.0wt.% was used as the reference model. Each HEU fuel element contains 19 fuel plates with a fuel meat thickness of 0.508 mm (20 mil). In this work, an optimized LEU (U-10Mo) core conversion case with a nominal fuel meat thickness of 0.330 mm (13 mil) and the U-235 enrichment of 19.7 wt.% was used to calculate the impact of the neutron spectrum in FE and FT positions. MCNP-calculated results show that the neutron spectrum in the LEU FE is slightly harder than in the HEU FE, as expected. However, when neutrons transport through water coolant and beryllium (Be), the neutrons are thermalized to an equilibrium neutron spectrum as a function of water volume fraction in the investigated FT positions. As a result, the neutron spectrum differences of the HEU and LEU in the NEFT, SEFT, and EFT are negligible. To demonstrate that the LEU core fuel cycle performance can meet the Updated Final Safety Analysis Report (UFSAR) safety requirements, additional studies will be necessary to evaluate and compare safety parameters such as void reactivity and Doppler coefficients, control components worth (outer shim control cylinders, safety rods and regulating rod), and shutdown margins between the HEU and LEU cores.

  3. In-situ monitoring of blood glucose level for dialysis machine by AAA-battery-size ATR Fourier spectroscopy

    NASA Astrophysics Data System (ADS)

    Hosono, Satsuki; Sato, Shun; Ishida, Akane; Suzuki, Yo; Inohara, Daichi; Nogo, Kosuke; Abeygunawardhana, Pradeep K.; Suzuki, Satoru; Nishiyama, Akira; Wada, Kenji; Ishimaru, Ichiro

    2015-07-01

    For blood glucose level measurement of dialysis machines, we proposed AAA-battery-size ATR (Attenuated total reflection) Fourier spectroscopy in middle infrared light region. The proposed one-shot Fourier spectroscopic imaging is a near-common path and spatial phase-shift interferometer with high time resolution. Because numerous number of spectral data that is 60 (= camera frame rare e.g. 60[Hz]) multiplied by pixel number could be obtained in 1[sec.], statistical-averaging improvement realize high-accurate spectral measurement. We evaluated the quantitative accuracy of our proposed method for measuring glucose concentration in near-infrared light region with liquid cells. We confirmed that absorbance at 1600[nm] had high correlations with glucose concentrations (correlation coefficient: 0.92). But to measure whole-blood, complex light phenomenon caused from red blood cells, that is scattering and multiple reflection or so, deteriorate spectral data. Thus, we also proposed the ultrasound-assisted spectroscopic imaging that traps particles at standing-wave node. Thus, if ATR prism is oscillated mechanically, anti-node area is generated around evanescent light field on prism surface. By elimination complex light phenomenon of red blood cells, glucose concentration in whole-blood will be quantify with high accuracy. In this report, we successfully trapped red blood cells in normal saline solution with ultrasonic standing wave (frequency: 2[MHz]).

  4. Investigation of Polysaccharide Adsorption on Protein Conditioning Films by Attenuated Total Reflection Infrared Spectrometry.

    PubMed

    Ishida; Griffiths

    1999-05-15

    The study of microorganisms at the aqueous/metal interface is of great interest as their presence is often associated with surface deterioration or corrosion. Surfaces submerged in aquatic environments rapidly become fouled with organic macromolecules, such as proteins and/or glycoproteins. Bacteria adhering to this conditioning film typically produce extracellular polysaccharides that anchor the cells to the substrate. In a previous paper, the kinetics of polysaccharide adsorption and desorption on protein conditioning films formed on bare germanium internal reflection elements (IREs) were investigated in an effort to gain a better understanding of the fouling process. This work has been extended to the study of adsorption phenomena at an aqueous/copper interface. Alginic acid and dextran were exposed to protein-conditioned and untreated copper films. In the absence of a protein biofilm, greater erosion of the Cu film was observed with flowing saline than with a solution of alginic acid in saline, and more Cu was removed at pH 4.8 than at pH 7.0. The neutral polysaccharide was less corrosive than alginic acid. The presence of a film of bovine serum albumin (13.5 nm) conditioning film did not shield the Cu film from the corrosive effects of either polysaccharide. In all experiments, as Cu slowly eroded from the surface of the IRE, metal islands formed leading to the observation of surface-enhanced infrared absorption (SEIRA). The intensity of the C-O stretching band of adsorbed dextran on Cu islands was over an order of magnitude greater than would be observed with a uniform Cu film of the same thickness. Enhancement of the amide II band of BSA was also observed. In general, the effect of SEIRA complicated spectral processing and interpretation and thus interfered with the determination of surface coverage and polysaccharide adsorption/desorption kinetics on protein conditioning films. Copyright 1999 Academic Press. PMID:10222093

  5. Formation of Assemblies Comprising Ru–Polypyridine Complexes and CdSe Nanocrystals Studied by ATR-FTIR Spectroscopy and DFT Modeling

    SciTech Connect

    Koposov, Alexey Y.; Cardolaccia, Thomas; Albert, Victor; Badaeva, Ekaterina; Kilina, Svetlana; Meyer, Thomas J.; Tretiak, Sergei; Sykora, Milan

    2011-07-05

    The interaction between CdSe nanocrystals (NCs) passivated with trioctylphosphine oxide (TOPO) ligands and a series of Ru–polypyridine complexes was studied by attenuated total reflectance FTIR (ATR-FTIR) and modeled using density functional theory (DFT). The results of DFT modeling are consistent with the experiment, showing that for the deprotonated carboxylic acid group the coupling to two Cd atoms via a bridging mode is the energetically most favorable mode of attachment for all nonequivalent NC surface sites and that the attachment of the protonated carboxylic acid is thermodynamically significantly less favorable.

  6. Nonlinear absorbance amplification using a diffuse reflectance cell: total organic carbon monitoring at 214 nm.

    PubMed

    Li, Yin-Huan; Shelor, C Phillip; Dasgupta, Purnendu K

    2015-01-20

    We present an absorption spectrometric method using a polytetrafluoroethylene (PTFE) cell as a diffuse reflector. The system was used for monitoring ultrapure water. All compounds absorb to some degree at low UV wavelengths, and the absorption at 214 nm from a zinc lamp source was monitored using a charge-coupled device (CCD) spectrometer. The absorption was interpreted in terms of total organic carbon present. The cell acts as a nonlinear absorbance amplifier, improving both the limit of detection (LOD) and the dynamic range. Potassium hydrogen phthalate (KHP) and glucose were used to evaluate the system and provided respective LODs of 46.5 ng/L and 4.5 mg/L as carbon. Although the physical path length was 25 cm, a maximum effective path length of 280 cm was observed at the lowest tested KHP concentrations. The system is intended for real-time monitoring of ultrapure water. PMID:25514042

  7. Total reflection X-ray fluorescence analysis of trace-elements in candies marketed in Mexico

    NASA Astrophysics Data System (ADS)

    Martinez, T.; Lartigue, J.; Zarazua, G.; Avila-Perez, P.; Navarrete, M.; Tejeda, S.

    2010-06-01

    Trace metals concentrations in food are significant for nutrition, due either to their nature or toxicity. Sweets, including chewing gum and candies, are not exactly a food, but they usually are unwearied consumed by children, the most vulnerable age-group to any kind of metal contamination in the food chain. The presence of relatively high concentrations of heavy metals such as Lead elicits concern since children are highly susceptible to heavy metals poisoning. Trace-metals concentrations were determined for six different flavors of a Mexican candy by means of Total X-ray Fluorescence Spectrometry. Triplicate samples of the various candy's flavours (strawberry, pineapple, lemon, blackberry, orange and chilli) were digested in 8 mL of a mix of supra-pure HNO 3 and H 2O 2 (6 mL: 2 mL) in a microwave oven MARS-X. Results show the presence of essential and toxic elements such as Ti, Cr, Mn, Fe, Ni, Cu, Zn, Br, Rb, Sr, and Pb. All metal concentrations were higher and significantly different ( α = 0.05) in chilli candy, compared to other candy flavours. Lead concentration fluctuated in the range of 0.102 to 0.342 μg g - 1 . A discussion about risk consumption and concentration allowed by Mexican and International Norms is made. As a part of the Quality Control Program, a NIST standard of "Citrus Leaves" and a blank were treated in the same way.

  8. Total internal reflection sum-frequency generation spectroscopy and dense gold nanoparticles monolayer: a route for probing adsorbed molecules

    NASA Astrophysics Data System (ADS)

    Tourillon, Gérard; Dreesen, Laurent; Volcke, Cedric; Sartenaer, Yannick; Thiry, Paul A.; Peremans, André

    2007-10-01

    We show that sum-frequency generation spectroscopy performed in the total internal reflection configuration (TIR-SFG) combined with a dense gold nanoparticles monolayer allows us to study, with an excellent signal to noise ratio and high signal to background ratio, the conformation of adsorbed molecules. Dodecanethiol (DDT) was used as probe molecules in order to assess the potentialities of the approach. An enhancement of more than one order of magnitude of the SFG signals arising from the adsorbed species is observed with the TIR geometry compared to the external reflection one while the SFG non-resonant contribution remains the same for both configurations. Although further work is required to fully understand the origin of the SFG process on nanoparticles, our work opens new possibilities for studying nanostructures.

  9. Selective detection of the structural changes upon photoreactions of several redox cofactors in photosystem II by means of light-induced ATR-FTIR difference spectroscopy

    NASA Astrophysics Data System (ADS)

    Okubo, Tatsunori; Noguchi, Takumi

    2007-04-01

    Attenuated total reflection Fourier transform infrared (ATR-FTIR) spectroscopy was applied for the first time to detect the structural changes upon photoreactions of redox cofactors in photosystem II (PSII). The PSII-enriched membranes from spinach were adsorbed on the surface of a silicon prism, and FTIR measurements of various redox cofactors were performed for the same sample but under different conditions by exchanging buffers in a flow cell. Light-induced FTIR difference spectra upon redox reactions of the oxygen-evolving Mn cluster, the primary quinone electron acceptor Q A, the redox-active tyrosine Y D, the primary electron acceptor pheophytin, and the primary electron donor chlorophyll P680 were successively recorded in buffers including different redox reagents and inhibitors. All of these cofactors remained active in the PSII membranes on the silicon surface, and the resultant spectra were basically identical to those previously recorded by the conventional transmission method. These ATR-FTIR measurements enable accurate comparison between reactions of different active sites in a single PSII sample. The present results demonstrated that the ATR-FTIR spectroscopy is a useful technique for investigation of the reaction mechanism of PSII.

  10. Design of an efficient Fresnel-type lens utilizing double total internal reflection for solar energy collection.

    PubMed

    Wallhead, Ian; Jiménez, Teresa Molina; Ortiz, Jose Vicente García; Toledo, Ignacio Gonzalez; Toledo, Cristóbal Gonzalez

    2012-11-01

    A novel of Fresnel-type lens for use as a solar collector has been designed which utilizes double total internal reflection (D-TIR) to optimize collection efficiency for high numerical aperture lenses (in the region of 0.3 to 0.6 NA). Results show that, depending on the numerical aperture and the size of the receiver, a collection efficiency theoretical improvement on the order of 20% can be expected with this new design compared with that of a conventional Fresnel lens. PMID:23326849

  11. High accuracy subwavelength distance measurements: A variable-angle standing-wave total-internal-reflection optical microscope

    SciTech Connect

    Haynie, A.; Min, T.-J.; Luan, L.; Mu, W.; Ketterson, J. B.

    2009-04-15

    We describe an extension of the total-internal-reflection microscopy technique that permits direct in-plane distance measurements with high accuracy (<10 nm) over a wide range of separations. This high position accuracy arises from the creation of a standing evanescent wave and the ability to sweep the nodal positions (intensity minima of the standing wave) in a controlled manner via both the incident angle and the relative phase of the incoming laser beams. Some control over the vertical resolution is available through the ability to scan the incoming angle and with it the evanescent penetration depth.

  12. Three-Dimensional Orientation Determination of Stationary Anisotropic Nanoparticles with Sub-Degree Precision under Total Internal Reflection Scattering Microscopy

    SciTech Connect

    Marchuk, Kyle; Fang, Ning

    2013-11-13

    Single-particle and single-molecule orientation determination plays a vital role in deciphering nanoscale motion in complex environments. Previous attempts to determine the absolute three-dimensional orientation of anisotropic particles rely on subjective pattern matching and are inherently plagued by high degrees of uncertainty. Herein, we describe a method utilizing total internal reflection scattering microscopy to determine the 3D orientation of gold nanorods with subdegree uncertainty. The method is then applied to the biologically relevant system of microtubule cargo loading. Finally, we demonstrate the method holds potential for identifying single particles versus proximate neighbors within the diffraction limited area.

  13. A New Method for Axial Decay Function Calibration of Evanescent Field in Multi-Angle Total Internal Reflection Fluorescence Microscopy

    NASA Astrophysics Data System (ADS)

    Wu, Jian; Xiu, Peng; Jin, Luhong; Nan, Di; Kuang, Cuifang; Zheng, Xiaoxiang; Xu, Yingke; Liu, Xu

    2016-01-01

    Three-dimensional image reconstruction in multi-angle total internal reflection fluorescence microscopy relies on actual penetration depths of evanescent wave at various incidence angles. In this paper, we propose a simple and elegant calibration method to calculate the actual axial decay profile of a given evanescent field, for the analytical solution of theoretical equation is hard to solve in complicated conditions. The results calculated by the proposed method agree with the experimental demands in our research. Our calibration method, together with multi-angle TIRF imaging, permits 3D reconstruction of cell surface in superb axial resolution.

  14. Multiplex detection of histone-modifying enzymes by total internal reflection fluorescence-based single-molecule detection.

    PubMed

    Ma, Fei; Liu, Meng; Wang, Zi-yue; Zhang, Chun-yang

    2016-01-21

    We develop a sensitive and selective method for the multiplex detection of histone-modifying enzymes (HMEs) through the integration of antibody-based fluorescence labeling with total internal reflection fluorescence (TIRF)-based single-molecule detection. This method exhibits excellent specificity and high sensitivity with a detection limit of 21 pM for histone acetyltransferase GcN5 and 12 pM for histone methyltransferase G9a, and it can be applied for the screening of HME inhibitors as well. PMID:26608941

  15. An antidot array as an edge for total non-reflection of spin waves in yttrium iron garnet films

    SciTech Connect

    Gieniusz, R. Guzowska, U.; Maziewski, A.; Bessonov, V. D.; Stognii, A. I.

    2014-02-24

    An array of antidots has been used as an edge to create the phenomenon of total non-reflection of spin waves in yttrium iron garnet films. At the critical angle between the line of antidots and the magnetic field, we observe a high-intensity beam of spin waves moving along the line of antidots. The properties of these waves are investigated experimentally by Brillouin light scattering spectroscopy. The conditions required for the occurrence of this phenomenon based on an analysis of the properties of the isofrequency dependencies are presented. The numerical simulations are in good agreement with those of the experimental measurements.

  16. ATR Preferentially Interacts with Common Fragile Site FRA3B and the Binding Requires its Kinase Activity in Response to Aphidicolin Treatment

    PubMed Central

    Wan, Cheng; Kulkarni, Atul; Wang, Yuh-Hwa

    2010-01-01

    The instability of common fragile sites (CFSs) contributes to the development of a variety of cancers. The ATR-dependent DNA damage checkpoint pathway has been implicated in maintaining CFS stability, but the mechanism is incompletely understood. The goal of our study was to elucidate the action of the ATR protein in the CFS-specific ATR-dependent checkpoint response. Using a chromatin immunoprecipitation assay, we demonstrated that ATR protein preferentially binds (directly or through complexes) to fragile site FRA3B as compared to non-fragile site regions, under conditions of mild replication stress. Interestingly, the amount of ATR protein that bound to three regions of FRA3B peaked at 0.4 μM aphidicolin (APH) treatment and decreased again at higher concentrations of APH. The total amounts of cellular ATR and several ATR-interacting proteins remained unchanged, suggesting that ATR binding to the fragile site is guided initially by the level of replication stress signals generated at FRA3B due to APH treatment and then sequestered from FRA3B regions by successive signals from other non-fragile site regions, which are produced at the higher concentrations of APH. This decrease in ATR binding to fragile site FRA3B at the higher concentrations of APH may account for the increasing number of chromosome gaps and breaks observed under the same conditions. Furthermore, inhibition of ATR kinase activity by treatment with 2-aminopurine (2-AP) or by over-expression of a kinase-dead ATR mutant showed that the kinase activity is required for the binding of ATR to fragile DNAs in response to APH treatment. Our results provide novel insight into the mechanism for the regulation of fragile site stability by ATR. PMID:20060399

  17. Cascaded automatic target recognition (Cascaded ATR)

    NASA Astrophysics Data System (ADS)

    Walls, Bradley

    2010-04-01

    The global war on terror has plunged US and coalition forces into a battle space requiring the continuous adaptation of tactics and technologies to cope with an elusive enemy. As a result, technologies that enhance the intelligence, surveillance, and reconnaissance (ISR) mission making the warfighter more effective are experiencing increased interest. In this paper we show how a new generation of smart cameras built around foveated sensing makes possible a powerful ISR technique termed Cascaded ATR. Foveated sensing is an innovative optical concept in which a single aperture captures two distinct fields of view. In Cascaded ATR, foveated sensing is used to provide a coarse resolution, persistent surveillance, wide field of view (WFOV) detector to accomplish detection level perception. At the same time, within the foveated sensor, these detection locations are passed as a cue to a steerable, high fidelity, narrow field of view (NFOV) detector to perform recognition level perception. Two new ISR mission scenarios, utilizing Cascaded ATR, are proposed.

  18. A dynamic thermal ATR-FTIR/chemometric approach to the analysis of polymorphic interconversions. Cimetidine as a model drug.

    PubMed

    Calvo, Natalia L; Maggio, Rubn M; Kaufman, Teodoro S

    2014-04-01

    Crystal polymorphism of active ingredients is relevant to the pharmaceutical industry, since polymorphic changes taking place during manufacture or storage of pharmaceutical formulations can affect critical properties of the products. Cimetidine (CIM) has several relevant solid state forms, including four polymorphs (A, B, C and D), an amorphous form (AM) and a monohydrate (M1). Dehydration of M1 has been reported to yield mixtures of polymorphs A, B and C or just a single form. Standards of the solid forms of CIM were prepared and unequivocally characterized by FTIR spectroscopy, digital microscopy, differential scanning calorimetry and solid state (13)C NMR spectroscopy. Multivariate curve resolution with alternating least squares (MCR-ALS) was coupled to variable temperature attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR) to dynamically characterize the behavior of form M1 of CIM over a temperature range from ambient to 160C, without sample pretreatment. MCR-ALS analysis of ATR-FTIR spectra obtained from the tested solid under variable temperature conditions unveiled the pure spectra of the species involved in the polymorphic transitions. This allowed the simultaneous observation of thermochemical and thermophysical events associated to the changes involved in the solid forms, enabling their unequivocal identification and improving the understanding of their thermal behavior. It was demonstrated that under the experimental conditions, dehydration of M1 initially results in the formation of polymorph B; after melting and upon cooling, the latter yields an amorphous solid (AM). It was concluded that the ATR-FTIR/MCR association is a promising and useful technique for monitoring solid-state phase transformations. PMID:24509287

  19. Screening a random mutagenesis library of a fungal β-fructofuranosidase using FT-MIR ATR spectroscopy and multivariate analysis.

    PubMed

    Trollope, K M; Nieuwoudt, H H; Görgens, J F; Volschenk, H

    2014-05-01

    Short-chain fructooligosaccharides (scFOS) are valuable health-promoting food additives. During the batch production of scFOS from sucrose the β-fructofuranosidase catalyst is subject to product inhibition by glucose. Engineering the enzyme for reduced sensitivity to glucose could improve product yields or process productivity while preserving the simple industrial batch design. Random mutagenesis is a useful technique for engineering proteins but should be coupled to a relevant high-throughput screen. Such a screen for sucrose and scFOS quantification remains elusive. This work presents the development of a screening method displaying potential high-throughput capacity for the evaluation of β-fructofuranosidase libraries using Fourier transform mid-infrared attenuated total reflectance (FT-MIR ATR) spectroscopy and multivariate analysis. A calibration model for the quantification of sucrose in enzyme assay samples ranged from 5 to 200 g/l and the standard error of prediction was below 13 g/l. A library of the Aspergillus japonicus fopA gene was generated by error prone PCR and screened in Saccharomyces cerevisiae. Using FT-MIR ATR spectroscopy, potential hits were identified as those variants that converted more sucrose in the presence of the glucose inhibitor than the parent. Subsequent analysis of reaction products generated by top performers using high-performance liquid chromatography identified a variant producing higher scFOS levels than the parent. At the peak difference in performance the variant produced 28 % more scFOS from the same amount of sucrose. This study highlights the application of FT-MIR ATR spectroscopy to a variant discovery pipeline in the directed evolution of a β-fructofuranosidase for enhanced scFOS production. PMID:24323289

  20. Determination of optical parameters of pulp suspensions by time-resolved detection of photoacoustic signals and total diffuse reflectance measurements

    NASA Astrophysics Data System (ADS)

    Zhao, Zuomin; Törmänen, Matti; Myllylä, Risto

    2010-04-01

    Time-resolved photoacoustics were used to measure the optical parameters of pulp suspensions for the first time. Reconstructing stress distribution along the direction of the incident laser light allows the effective attenuation coefficient of these suspensions to be determined. Simultaneously, the total diffuse reflectance of the suspensions was measured by the same laser source. Based on the effective attenuation coefficient and total diffuse reflectance, the absorption and reduced scattering coefficients of pulp suspensions can be calculated. In this study, three kinds of pulp suspensions with different kappa number (2, 13, and 16), a measure of lignin content in pulp fibers, were diluted with water to make samples with a consistency range from 1% to 5%, and studied at 355 nm wavelength. The results showed that the optical coefficients were approximately proportional to pulp consistency; on the other hand, the absorption coefficient was linearly correlated with kappa number, but the reduced scattering coefficient was not. Therefore, by determining its optical parameters, it is possible to extract the consistency and kappa number of an unknown pulp suspension.

  1. Live Imaging of Cellular Internalization of Single Colloidal Particle by Combined Label-Free and Fluorescence Total Internal Reflection Microscopy.

    PubMed

    Byrne, Gerard D; Vllasaliu, Driton; Falcone, Franco H; Somekh, Michael G; Stolnik, Snjezana

    2015-11-01

    In this work we utilize the combination of label-free total internal reflection microscopy and total internal reflectance fluorescence (TIRM/TIRF) microscopy to achieve a simultaneous, live imaging of single, label-free colloidal particle endocytosis by individual cells. The TIRM arm of the microscope enables label free imaging of the colloid and cell membrane features, while the TIRF arm images the dynamics of fluorescent-labeled clathrin (protein involved in endocytosis via clathrin pathway), expressed in transfected 3T3 fibroblasts cells. Using a model polymeric colloid and cells with a fluorescently tagged clathrin endocytosis pathway, we demonstrate that wide field TIRM/TIRF coimaging enables live visualization of the process of colloidal particle interaction with the labeled cell structure, which is valuable for discerning the membrane events and route of colloid internalization by the cell. We further show that 500 nm in diameter model polystyrene colloid associates with clathrin, prior to and during its cellular internalization. This association is not apparent with larger, 1 μm in diameter colloids, indicating an upper particle size limit for clathrin-mediated endocytosis. PMID:26402436

  2. 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. PMID:26717839

  3. FTIR-ATR determination of solid non fat (SNF) in raw milk using PLS and SVM chemometric methods.

    PubMed

    Bassbasi, M; Platikanov, S; Tauler, R; Oussama, A

    2014-03-01

    Fourier transform infrared spectroscopy (FTIR) attenuated total reflectance (ATR) spectroscopy, coupled with chemometrics methods have been applied to the fast and non-destructive quantitative determination of solid non fat (SNF) content in raw milk. Partial least squares regression (PLS) and support vector machine (SVM) regression methods were used to model and predict SNF contents in raw milk based on FTIR spectral transmission measurements. Both methods, PLS and SVM, showed good performances in SNF prediction with relative prediction errors in the external validation of between 0.2% and 0.3% depending on the spectral range and regression method. Coefficient of determination of the global fit was always above 0.99. Since, the relative prediction errors were low, it can be concluded that FTIR-ATR with chemometrics can be used for accurate quantitative determinations of SNF contents in raw milk within the investigated calibration range of 79-100g/L. The proposed procedure is fast, non-destructive, simple and easy to implement. PMID:24176339

  4. In situ ATR-IR spectroscopic and electron microscopic analyses of settlement secretions of Undaria pinnatifida kelp spores

    PubMed Central

    Petrone, L.; Easingwood, R.; Barker, M. F.; McQuillan, A. J.

    2011-01-01

    Knowledge about the settlement of marine organisms on substrates is important for the development of environmentally benign new methods for control of marine biofouling. The adhesion to substrates by spores of Undaria pinnatifida, a kelp species that is invasive to several countries, was studied by scanning electron and transmission electron microscopies (SEM/TEM) as well as by in situ attenuated total reflection infrared (ATR-IR) spectroscopy. The IR spectra showed that adhesive secretion began approximately 15 min after initial settlement and that the adhesive bulk material contained protein and anionic polysaccharides. Energy dispersive X-ray microanalysis of the adhesive identified sulphur and phosphorus as well as calcium and magnesium ions, which facilitate the gelation of the anionic polysaccharides in the sea water. The adhesive may be secreted from Golgi bodies in the spore, which were imaged by TEM of spore thin sections. Additionally, an in situ settlement study on TiO2 particle film by ATR-IR spectroscopy revealed the presence of phosphorylated moieties directly binding the substrate. The presence of anionic groups dominating the adhesive suggests that inhibition of spore adhesion will be favoured by negatively charged surfaces. PMID:20685693

  5. Focusing and matching properties of the ATR transfer line

    SciTech Connect

    Tsoupas, N.; Fischer, W.; Kewisch, J.; MacKay, W.W.; Peggs, S.; Pilat, F.; Tepikian, S.; Wei, J.

    1997-07-01

    The AGS to RHIC (AtR) beam transfer line has been constructed and will be used to transfer beam bunches from the AGS machine into the RHIC machine which is presently under construction at BNL. The original design of the AtR line has been modified. This article will present the optics of the various sections of the existing AtR beam line, as well as the matching capabilities of the AtR line to the RHIC machine.

  6. Mapping of healthy oral mucosal tissue using diffuse reflectance spectroscopy: ratiometric-based total hemoglobin comparative study.

    PubMed

    Hafez, Razan; Hamadah, Omar; Bachir, Wesam

    2015-11-01

    The objective of this study is to clinically evaluate the diffuse reflectance spectroscopy (DRS) ratiometric method for differentiation of normal oral mucosal tissues with different histological natures and vascularizations in the oral cavity. Twenty-one healthy patients aged 20-44 years were diagnosed as healthy and probed with a portable DRS system. Diffuse reflectance spectra were recorded in vivo in the range (450-650 nm). In this study, the following three oral mucosal tissues were considered: masticatory mucosa, lining mucosa, and specialized mucosa. Spectral features based on spectral intensity ratios were determined at five specific wavelengths (512, 540, 558, 575, and 620 nm). Total hemoglobin based on spectral ratios for the three anatomical regions have also been evaluated. The three studied groups representing different anatomical regions in the oral cavity were compared using analysis of variance and post hoc least significant difference tests. Statistical analysis showed a significant difference in the mean of diffuse spectral ratios between the groups (P < 0.05). Post hoc test detected significant difference between masticatory mucosa group and lining mucosa group (P < 0.05) and between masticatory mucosa group and specialized mucosa group (P = 0.000, at ratio 558/620 and P = 0.000, at ratio 575/620). Significant difference was also found between the lining mucosa group and specialized mucosa group (P = 0.000, at ratio 512/558 and P = 0.000, at ratio 512/575). It has also been shown that spectral ratios at wavelengths 558, 575, and 620 nm reveal the greatest difference among the main oral sites in terms of total hemoglobin content. Diffuse reflectance spectroscopy might be used for creating a DRS databank of normal oral mucosal tissue with specific spectral ratios featuring the total hemoglobin concentrations. That would further enhance the discrimination of oral tissue for examining the histological nature of oral mucosa and diagnosis of early precancerous changes in the oral cavity based on non-invasive monitoring of neovascularization. PMID:25987341

  7. Embedded multilayer thin film stacks as polarizing beam splitters and wave retarders operating under condition of frustrated total internal reflection

    NASA Astrophysics Data System (ADS)

    Perla, Siva Reddy

    The polarization properties of embedded centro-symmetric and periodic multilayer stacks under conditions of frustrated total internal reflection (FTIR) are considered. The centro-symmetric multilayer stack consists of a high-index center layer sandwiched between two identical low-index films and high-index - low-index bilayers repeated on both sides of the central trilayer maintaining the symmetry of the entire stack. The periodic multilayer consists of periodically repeated low-index - high-index bilayers. Each multilayer stack is embedded in a high-index prism. Embedded centro-symmetric multilayer stacks are designed to function as efficient polarizers or polarizing beam splitters (PBSs) under conditions of FTIR over an extended range of incidence angles. For a given set of refractive indices, all possible solutions for the thicknesses of the layers that suppress the reflection of p-polarized light at a specified angle, and the associated reflectance of the system for the orthogonal s polarization, are determined. The angular and spectral sensitivities of polarizing multilayer stacks employing 3, 7, 11, 15 and 19 layers of BaF 2 and PbTe thin films embedded in a ZnS prism, operating at lambda = 10.6 mum, are presented. Embedded centro-symmetric multilayer stacks are also designed to function as complete-transmission quarter-wave or half-wave retardation (QWR or HWR) devices under conditions of FTIR. QWR and HWR designs at lambda =1.55 mum are presented that employ 11 and 7 layers of Si and SiO2 thin films embedded in GaP and Si cube prisms, respectively. The angular and spectral sensitivities of these devices are also considered. Embedded centro-symmetric multilayer stacks under FTIR conditions are also designed to produce various 50%-50% beam splitters. Embedded periodic multilayer stacks are designed to function as polarizers and PBSs at discrete multiple angles of incidence and wavelengths under condition of FTIR. For a given set of refractive indices, all possible solutions for the thicknesses of the layers that suppress the reflection of p-polarized light at a specified angle, and the associated reflectance of the system for the orthogonal s polarization, are determined. The angular and spectral sensitivities of polarizing multilayer stacks employing 4, 6, 8, 10, 12, 14, 16 and 18 layers of BaF2 and PbTe thin films embedded in a ZnS prism, operating at lambda = 10.6 mum, are presented.

  8. Analysis of trace metals in thin silicon nitride films by total-reflection X-ray fluorescence

    NASA Astrophysics Data System (ADS)

    Vereecke, G.; Arnauts, S.; Van Doorne, P.; Kenis, K.; Onsia, B.; Verstraeten, K.; Schaekers, M.; Van Hoeymissen, J. A. B.; Heyns, M. M.

    2001-11-01

    The validity of a matrix withdrawal method for the analysis of trace metals in silicon nitride films on silicon wafers by total-reflection X-ray fluorescence has been evaluated with samples contaminated with diluted standard solutions of eight metals (Ca, V, Cr, Fe, Ni, Cu, Ta, W). The nitride matrix was removed by a decomposition step with HF vapor at ambient conditions followed by the vaporization of the product at a temperature higher than 240°C. The recovery of added metals was determined first directly after vaporization and secondly after preconcentration by the droplet collection (DC) method. The recovery of metals after vaporization at a temperature of 300±50°C was generally close to 100%, except for Cu whose recovery was approximately 40%. The efficiency of the DC step was approximately 50% for most metals but only 10-20% for Cu and Cr. Thus for most metals the total recovery was close to 50%, which is acceptable for analytical purpose. The recovery of Cu and Cr was studied in more detail considering the influence of the thickness of the nitride film, the vaporization temperature, and the composition of the DC solution. The total recovery of Cu increased from approximately 10 to 40% by lowering the temperature of the vaporization step and using a more concentrated DC solution. The recovery of Cr by DC was markedly influenced by the thickness of the nitride film with no great benefit of using a more concentrated DC solution.

  9. Overview of the ATR Power Supplies

    NASA Astrophysics Data System (ADS)

    Bruno, D.; Soukas, A.; Toldo, F.; Lambiase, B.

    1997-05-01

    The AGS to RHIC transfer Line (ATR) transports a variety of beams from the Alternating Gradient Synchrotron (AGS) which gets its input from the Booster Synchrotron. In turn, the Booster receives input beams from either a Tandem Van de Graaff (heavy ions) or a Linac(protons). The AGS extracts beam bunches, up to a rate of 30 Hertz, to the ATR which will eventually feed the Relativistic Heavy Ion Collider (RHIC) starting with the sextant test in January of 1996. The ATR is made up of the upgraded U line and the new W, X and Y lines. A test in 1995 transported beam to the end of the W line. During normal operation, a pulsed switching magnet at the end of the W line will bend the beam into the X line or the Y line so that the two rings in RHIC are filled with counter rotating beams. The ATR line is comprised of 80 power supplies (PS's), 17 of which are upgraded AGS PS's. The remaining 63 PS's were newly purchased. These PS's range from bipolar 600 watt linear type trim magnet PS's to 1 Megawatt, thyristor, dipole PS's. Results of the commissioning runs will be presented, as well as descriptions of regulation, filtering, and analog and digital controls.

  10. Overview of the ATR power supplies

    SciTech Connect

    Bruno, D.; Soukas, A.; Toldo, F.; Lambiase, R.F.

    1997-07-01

    The AGS to RHIC transfer line (ATR) transports a variety of beams from the Alternating Gradient Synchrotron (AGS) which gets its input from the Booster Synchrotron. In turn, the Booster receives input beams from either a Tandem Van de Graaff (heavy ions) or a Linac (protons). The AGS extracts beam bunches, up to a rate of 30 Hertz, to the ATR which feeds the Relativistic Heavy Ion Collider (RHIC) starting with the sextant test in January of 1997. The ATR is made up of the upgraded U line and the new W, X, and Y lines. A test in 1995 transported beam to the end of the W line. During normal operation, a pulsed switching magnet at the end of the W line will bend the beam into the X line or the Y line so that the two storage rings in RHIC are filled with counter rotating beams. The ATR line is comprised of 80 power supplies (PS`s), 17 of which are upgraded AGS PS`s. The remaining 63 PS`s were newly purchased. These PS`s range from bipolar 600 watt linear type trim magnet PS`s to 1 Megawatt, thyristor, dipole PS`s. Results of the commissioning runs will be presented, as well as descriptions of regulation, filtering, and analog and digital controls.

  11. Seasonal variation in trace and minor elements in Brazilian honey by total reflection X-ray fluorescence.

    PubMed

    de Oliveira Resende Ribeiro, Roberta; Mársico, Eliane Teixeira; da Silva Carneiro, Carla; Simoes, Julia Siqueira; da Silva Ferreira, Micheli; de Jesus, Edgar Francisco Oliveira; Almeida, Eduardo; Junior, Carlos Adam Conte

    2015-03-01

    Honey is used as an alternative medicine and is a constituent of a healthy diet worldwide. Its composition is associated with botanical origin and, to some extent, geographical origin because soil and climate characteristics determine the melliferous flora. Also, the elements content in honey samples could give an indication of environmental pollution or geographical origin. The main purpose of this study was to evaluate seasonal patterns of essential elements of Brazilian honey. Honey was collected during spring, summer, autumn, and winter for 2 years to quantify K, Ca, Ti, Cr, Mn, Fe, Ni, Cu, Zn, Se, Br, and Sr using total reflection X-ray fluorescence spectroscopy (TXRF). Our results indicate no seasonal differences in concentration of Cr, Ni, Se, and Ti, although there were significant seasonal patterns in the composition of essential elements in honey, with higher concentrations of minor and trace elements, especially K and Ca of samples collected in spring and summer. PMID:25663399

  12. In-situ analysis of fruit anthocyanins by means of total internal reflectance, continuous wave and time-resolved spectroscopy

    NASA Astrophysics Data System (ADS)

    Zude, Manuela; Spinelli, Lorenzo; Dosche, Carsten; Torricelli, Alessandro

    2009-08-01

    In sweet cherry (Prunus avium), the red pigmentation is correlated with the fruit maturity stage and can be measured by non-invasive spectroscopy. In the present study, the influence of varying fruit scattering coefficients on the fruit remittance spectrum (cw) were corrected with the effective pathlength and refractive index in the fruit tissue obtained with distribution of time-of-flight (DTOF) readings and total internal reflection fluorescence (TIRF) analysis, respectively. The approach was validated on fruits providing variation in the scattering coefficient outside the calibration sample set. In the validation, the measuring uncertainty when non-invasively analyzing fruits with cw method in comparison with combined application of cw, DTOF, and TIRF measurements showed an increase in r2 up to 22.7 % with, however, high errors in all approaches.

  13. Determination of copper, iron and zinc in spirituous beverages by total reflection X-ray fluorescence spectrometry

    NASA Astrophysics Data System (ADS)

    Capote, T.; Marcó, L. M.; Alvarado, J.; Greaves, E. D.

    1999-10-01

    The concentration of copper in traditional homemade alcoholic distillates produced in Venezuela (Cocuy de Penca) were determined by total reflection X-ray fluorescence (TXRF) using vanadium as internal standard. The results were compared to those obtained by flame atomic absorption spectrometry (FAAS). Three preparative methods of addition of vanadium were compared: classical internal standard addition, 'layer on layer' internal standard addition and in situ addition of internal standard. The TXRF procedures were accurate and the precision was comparable to that obtained by the FAAS technique. Copper levels were above the maximum allowed limits for similar beverages. Zinc and iron in commercial and homemade distilled beverages were also analyzed by TXRF with in situ addition of internal standard demonstrating the usefulness of this technique for trace metal determination in distillates.

  14. Use of total-reflection X-ray fluorescence in search of a biomonitor for environmental pollution in Vietnam

    NASA Astrophysics Data System (ADS)

    Brauer, Hans; Wagner, Annemarie; Boman, Johan; Viet Binh, Doan

    2001-11-01

    The concentration of trace elements in tissues of several animals collected in the Ha Nam province, approximately 40 km south of Hanoi, Vietnam, has been investigated using total-reflection X-ray fluorescence analysis. We find that the freshwater mussel is probably the optimal choice of biomonitor for the pollution situation in Vietnam, but the freshwater crab, the toad and the catfish are also good candidates. The krait is probably also well suited for this purpose. It is shown that since several elements show a more or less pronounced accumulation tendency in a particular tissue it can be of great use to determine the levels in different tissues. When selecting an organism to be used as a biomonitor, other factors besides the mere concentration of trace elements must be considered, for instance the abundance and feeding habits.

  15. Determination of heavy metals in macrozoobenthos from the rivers Tisza and Szamos by total reflection X-ray fluorescence spectrometry

    NASA Astrophysics Data System (ADS)

    Woelfl, S.; Mages, M.; Óvári, M.; Geller, W.

    2006-11-01

    In 2000, accidents in the Romanian mining industry in key catchment areas led to heavy metal contamination of the Hungarian rivers Tisza and Szamos resulting in substantial heavy metal loads in several sediments of the upper river basins. This enhanced metal content might have been bioaccumulated in benthic organisms during the following years. Therefore, the aim of this study was to test, whether the zoobenthic fauna showed an enhanced metal content 3 years after the industrial accident. Macrozoobenthic insect larvae (chironomids) were sampled 100 m below and above the confluent site of the rivers Tisza and Szamos during summer 2003 and for comparison purpose also in the river Maros, a tributary of the Tisza river, during 2005. In order to determine their heavy metal content, single specimens were prepared and analysed by Total Reflection X-ray Fluorescence Spectrometry (TRXF) according to the modified dry method. Fe was much lower and Mn and Zn much higher concentrated in benthos from the more contaminated Szamos river compared to the Tisza and Maros rivers. In this sense, the benthic organisms reflected very well the enhanced metal concentrations in the contaminated rivers being suitable as bioindicators of metal contamination. However, the sediment bioaccumulation factor was low at all sampling sites indicating a low bioavailability of trace metals for benthic organisms.

  16. Micrometer-Sized Supported Lipid Bilayer Arrays for Bacterial Toxin Binding Studies through Total Internal Reflection Fluorescence Microscopy

    PubMed Central

    Moran-Mirabal, Jose M.; Edel, Joshua B.; Meyer, Grant D.; Throckmorton, Dan; Singh, Anup K.; Craighead, Harold G.

    2005-01-01

    In this article, we present the use of micron-sized lipid domains, patterned onto planar substrates and within microfluidic channels, to assay the binding of bacterial toxins via total internal reflection fluorescence microscopy. The lipid domains were patterned using a polymer lift-off technique and consisted of ganglioside-populated distearoylphosphatidylcholine:cholesterol supported lipid bilayers (SLBs). Lipid patterns were formed on the substrates by vesicle fusion followed by polymer lift-off, which revealed micron-sized SLBs containing either ganglioside GT1b or GM1. The ganglioside-populated SLB arrays were then exposed to either cholera toxin B subunit or tetanus toxin C fragment. Binding was assayed on planar substrates by total internal reflection fluorescence microscopy down to 100 pM concentration for cholera toxin subunit B and 10 nM for tetanus toxin fragment C. Apparent binding constants extracted from three different models applied to the binding curves suggest that binding of a protein to a lipid-based receptor is influenced by the microenvironment of the SLB and the substrate on which the bilayer is formed. Patterning of SLBs inside microfluidic channels also allowed the preparation of lipid domains with different compositions on a single device. Arrays within microfluidic channels were used to achieve segregation and selective binding from a binary mixture of the toxin fragments in one device. The binding and segregation within the microfluidic channels was assayed with epifluorescence as proof of concept. We propose that the method used for patterning the lipid microarrays on planar substrates and within microfluidic channels can be easily adapted to proteins or nucleic acids and can be used for biosensor applications and cell stimulation assays under different flow conditions. PMID:15833994

  17. Serum Cystatin C Reflects Angiographic Coronary Collateralization in Stable Coronary Artery Disease Patients with Chronic Total Occlusion

    PubMed Central

    Zhang, Rui Yan; Zhang, Qi; Lu, Lin; Shen, Wei Feng

    2015-01-01

    Objective We investigated whether and to what extent cystatin C was associated with angiographic coronary collateralization in patients with stable coronary artery disease and chronic total occlusion. Methods Serum levels of cystatin C and high-sensitive C-reactive protein (hsCRP) and glomerular filtration rate (GFR) were determined in 866 patients with stable angina and angiographic total occlusion of at least one major coronary artery. The degree of collaterals supplying the distal aspect of a total occlusion from the contra-lateral vessel was graded as poor (Rentrop score of 0 or 1) or good coronary collateralization (Rentrop score of 2 or 3). Results In total, serum cystatin C was higher in patients with poor collateralization than in those with good collateralization (1.08 ± 0.32 mg/L vs. 0.90 ± 0.34 mg/L, P < 0.001), and correlated inversely with Rentrop score (adjusted Spearmen’s r = -0.145, P < 0.001). The prevalence of poor coronary collateralization increased stepwise with increasing cystatin C quartiles (P for trend < 0.001). After adjusting for age, gender, risk factors for coronary artery disease, GFR and hsCRP, serum cystatin C ≥ 0.97 mg/L remained independently associated with poor collateralization (OR 2.374, 95% CI 1.660 ~ 3.396, P < 0.001). The diagnostic value of cystatin C levels for detecting poor coronary collateralization persisted regardless of age, gender, presence or absence of diabetes, hypertension or renal dysfunction. Conclusions Serum cystatin C reflects angiographic coronary collateralization in patients with stable coronary artery disease, and cystatin C ≥ 0.97 mg/L indicates a great risk of poor coronary collaterals. PMID:26402227

  18. ATR-FTIR Spectroscopy for the Assessment of Biochemical Changes in Skin Due to Cutaneous Squamous Cell Carcinoma

    PubMed Central

    Lima, Cássio A.; Goulart, Viviane P.; Côrrea, Luciana; Pereira, Thiago M.; Zezell, Denise M.

    2015-01-01

    Nonmelanoma skin cancers represent 95% of cutaneous neoplasms. Among them, squamous cell carcinoma (SCC) is the more aggressive form and shows a pattern of possible metastatic profile. In this work, we used Fourier transform infrared spectroscopy (FTIR) spectroscopy to assess the biochemical changes in normal skin caused by squamous cell carcinoma induced by multi-stage chemical carcinogenesis in mice. Changes in the absorption intensities and shifts were observed in the vibrational modes associated to proteins, indicating changes in secondary conformation in the neoplastic tissue. Hierarchical cluster analysis was performed to evaluate the potential of the technique to differentiate the spectra of neoplastic and normal skin tissue, so that the accuracy obtained for this classification was 86.4%. In this sense, attenuated total reflection (ATR)-FTIR spectroscopy provides a useful tool to complement histopathological analysis in the clinical routine for the diagnosis of cutaneous squamous cell carcinoma. PMID:25811925

  19. Direct determination of niflumic acid in a pharmaceutical gel by ATR/FTIR spectroscopy and PLS calibration.

    PubMed

    Boyer, C; Brégère, B; Crouchet, S; Gaudin, K; Dubost, J P

    2006-02-13

    A simple, rapid and convenient analytical method without sample handling procedure is proposed for the determination of niflumic acid in a pharmaceutical gel with attenuated total reflectance/Fourier transform infrared spectroscopy (ATR/FTIR). A partial least square (PLS) calibration model for the prediction of niflumic acid contents was developed using 81 and 27 spectra of standard gels as training and validation sets, respectively. The used spectral range of niflumic acid for the establishment of this model was 2300-1100 cm(-1). All spectra were obtained in the transmittance mode, then normalized and first derivative transformed. The model yielded a regression coefficient R2 equal to 1 for the training set and a root mean square error of prediction (RMSEP) equal to 0.2 for the validation set. The percentage recoveries of the method for the analysis of Niflugel ranged from 96.60 to 101.02%. PMID:16122895

  20. Formulation and drug-content assay of microencapsulated antisense oligonucleotide to NF-κB using ATR-FTIR

    NASA Astrophysics Data System (ADS)

    Siwale, Rodney; Meadows, Fred; Mody, Vicky V.; Shah, Samit

    2013-09-01

    Antisense oligonucleotide to NF-κB sequence: 5‧-GGA AAC ACA TCC TCC ATG-3‧, was microencapsulated in an albumin matrix by the method of spray dryingTM. Spectral analysis was performed on varying drug loading formulations of both drugs by mid-IR attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR). An out of plane O-H bending vibration at 948 cm-1, unique to both the native and microencapsulated drugs was identified. The calculated peak areas corresponded to the drug loadings in the microsphere formulations. A standard curve could then be used to determine the drug content of an unknown microsphere formulation. Accuracy and precision were determined to be comparable to other analytical techniques such as HPLC.

  1. Cellulose acetate-lithium bis(trifluoromethanesulfonyl)imide solid polymer electrolyte: ATR-FTIR and ionic conductivity behavior

    NASA Astrophysics Data System (ADS)

    Mohd Razalli, Siti Masyitah; Sheikh Mohd Saaid, Siti Irma Yuana; Marwan Ali, Ab Malik; Hassan, Oskar Hasdinor; Yahya, Muhd Zu Azhan

    2015-05-01

    Solid polymer electrolytes (SPEs) based on cellulose acetate (CA) doped with lithium bis(trifluoromethanesulfonyl)imide (LiTFSI) salt are prepared by solution cast technique. Attenuated total reflectance-Fourier transform infrared (ATR-FTIR) spectroscopy of the polymer salt complexes are recorded in the frequency range between 400 cm-1 and 4000 cm-1. The shifting of carbonyl band (C=O) at 1737 cm-1 to a lower wavenumber confirms the occurrence of complexation between the polymer and the salt. The electrochemical impedance spectroscopy (EIS) analysis discovered that the film with 25 wt.% of salt shows the highest ionic conductivity at room temperature. The change in real dielectric permittivity (ɛr) as a function of frequency at different salt concentrations which exhibits a dispersive behavior at low frequencies and decays at higher frequencies, shows the electrode polarization and space charge effect. The real modulus formalism (Mr) analysis shows that the polymer electrolytes in this work are ionic conductors.

  2. Monitoring the distribution of surfactants in the stratum corneum by combined ATR-FTIR and tape-stripping experiments.

    PubMed

    Hoppel, Magdalena; Holper, Evelyn; Baurecht, Dieter; Valenta, Claudia

    2015-01-01

    Combined ATR-FTIR (attenuated total reflection-Fourier transform infrared) spectroscopy and tape-stripping experiments in vitro on porcine ear skin were used to investigate the spatial distribution of different surfactants in the stratum corneum (SC). To reveal a possible connection between the size of the formed micelles and skin penetration, dynamic light-scattering measurements of the aqueous surfactant solutions were also taken. Compared to an alkyl polyglycoside and sucrose laurate, a deeper skin penetration of the anionic surfactants sodium dodecyl sulfate (SDS) und sodium lauryl ether sulfate (SLES) could be related to a smaller size of the formed micelles. Beside the differences in spatial distribution, a link between the physical presence of anionic surfactants in the SC and a decrease of skin hydration was found. Furthermore, the incorporation of SDS and SLES into the SC, even after a brief, consumer-orientated washing procedure with commercially available hair shampoos, was confirmed. PMID:25612540

  3. How polyelectrolyte adsorption depends on history: A combined Fourier transform infrared spectroscopy in attenuated total reflection and surface forces study

    SciTech Connect

    Sukhishvili, S.A.; Dhinojwala, A.; Granick, S.

    1999-11-23

    The authors present a systematic study of how adsorption history affects the thickness, surface forces, and interfacial rheology of a model cationic polymer. The polymer was quaternized poly-4-vinylpyridine, QPVP (weight average degree of polymerization n{sub w} = 325 and 98% quaternized with ethyl bromide). The main comparisons concerned one-step adsorption from solution at a variable salt concentration up to 0.5 NaCl, versus two-step adsorption (initial adsorption from buffer solution without added salt, then NaCl added later). The aqueous solutions were buffered at pH = 9.2 such that the surfaces (mica in the case of surfaces forces (SFA) experiments, oxidized silicon in the case of in situ infrared (FTIR-ATR) experiments) in each case carried a large negative charge. The SFA and FTIR-ATR experiments gave consistent estimates of the amount of polymer adsorbed, confirming the expectation that adsorption should be driven by electrostatic attraction to the surface of large opposite charge. The adsorbed amount showed little dependence on path, validating the common assumption of equilibration in this respect. However the layer thickness measured by surface forces, the shear nanorheology response at a given surface force, and the dichroism of pendant side groups of the polymer all showed a pronounced dependence on the path to reach the adsorbed state. The authors interpret the measurements to suggest that two-step adsorption produces an inhomogeneous layer comprised of a dense layer of segments closest to the solid surface and a sparse outer layer. In particular, two-step adsorption produced thicker layers and a greater tendency to decouple shear forces from those that resist compression in the normal direction, thereby lessening the shear forces at a given level of normal force.

  4. The distribution of atrazine (ATR) and ATR metabolites in the Wistar rat following gestational/lactational exposures

    EPA Science Inventory

    Gestational/lactational exposure to ATR is reported to alter reproductive/developmental function, yet our understanding of the transfer of ATR and/or its metabolites from the dam to the fetus/offspring is limited. Previously we examined the lactational transfer of CI4-ATR, but sp...

  5. 77 FR 67557 - Special Conditions: ATR-GIE Avions de Transport Regional, Models ATR42-500 and ATR72-212A...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2012-11-13

    ...These special conditions are issued for the ATR-GIE Avions de Transport Regional Models ATR42-500 and ATR72-212A airplanes. These airplanes will have novel or unusual design features associated with the architecture and connectivity capabilities of the airplanes' computer systems and networks, which may allow access to or by external computer systems and networks. Connectivity to, or access......

  6. Use of attenuated total reflection Fourier transform infrared (ATR FT-IR) spectroscopy in direct, non-destructive, and rapid assessment of developmental cotton fibers grown in planta and in culture

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Cotton fibers are routinely harvested from cotton plants (in planta), and their end-use qualities depend on their development stages. Cotton fibers are also cultured at controlled laboratory environments, so that cotton researchers can investigate many aspects of experimental protocols in cotton bre...

  7. The correlation of attenuated total reflectance infrared (ATR-FTIR) spectroscopic data with X-ray diffraction (XRD) parameters and its potential use for mineral identification and quantification in drilling cores: examples from the Pannonian Basin, Hungar

    NASA Astrophysics Data System (ADS)

    Udvardi, Beatrix; Kovács, István; Viczián, István; Hámor-Vidó, Mária; Mihály, Judith; Németh, Csaba

    2013-04-01

    Four thick sediment sequences in the following boreholes, Vízvár-I (0,0-2965,0 m) in the Dráva Basin, Som-I (999,5-1150,6 m) in southern Transdanubia, and two other boreholes, Doboz-I (3490-4434 m) and Doboz-III (2190-3400 m) in the Békés Basin, Hungary, were investigated in detail. Each drillings cut across Neogene sequences and contain shales, carbonates and clay rocks (Tanács & Viczián, 1995). The selection of these cores is due to the various amounts of smectite, illite and kaolinite minerals that are well manifested during comparison of infrared spectroscopic and former XRD dataset. During preparation, powdered core samples were settled (

  8. A Simplified Shuttle Irradiation Facility for ATR

    SciTech Connect

    A. J. Palmer; S. T. Laflin

    1999-08-01

    During the past fifteen years there has been a steady increase in the demand for radioisotopes in nuclear medicine and a corresponding decline in the number of reactors within the U.S. capable of producing them. The Advanced Test Reactor (ATR) is the largest operating test reactor in the U.S., but its isotope production capabilities have been limited by the lack of an installed isotope shuttle irradiation system. A concept for a simple "low cost" shuttle irradiation facility for ATR has been developed. Cost were reduced (in comparison to previous ATR designs) by using a shielded trough of water installed in an occupiable cubicle as a shielding and contamination control barrier for the send and receive station. This shielding concept also allows all control valves to be operated by hand and thus the need for an automatic control system was eliminated. It was determined that 4-5 ft of water would be adequate to shield the isotopes of interest while shuttles are transferred to a small carrier. An additional feature of the current design is a non-isolatable by-pass line, which provides a minimum coolant flow to the test region regardless of which control valves are opened or closed. This by-pass line allows the shuttle facility to be operated without bringing reactor coolant water into the cubicle except for send and receive operations.

  9. Automated rapid training of ATR algorithms

    NASA Astrophysics Data System (ADS)

    McBride, Jonah; Lowell, Jessica; Snorrason, Magnús; Eaton, Ross; Irvine, John

    2009-05-01

    Computer vision methods, such as automatic target recognition (ATR) techniques, have the potential to improve the accuracy of military systems for weapon deployment and targeting, resulting in greater utility and reduced collateral damage. A major challenge, however, is training the ATR algorithm to the specific environment and mission. Because of the wide range of operating conditions encountered in practice, advanced training based on a pre-selected training set may not provide the robust performance needed. Training on a mission-specific image set is a promising approach, but requires rapid selection of a small, but highly representative training set to support time-critical operations. To remedy these problems and make short-notice seeker missions a reality, we developed Learning and Mining using Bagged Augmented Decision Trees (LAMBAST). LAMBAST examines large databases and extracts sparse, representative subsets of target and clutter samples of interest. For data mining, LAMBAST uses a variant of decision trees, called random decision trees (RDTs). This approach guards against overfitting and can incorporate novel, mission-specific data after initial training via perpetual learning. We augment these trees with a distribution modeling component that eliminates redundant information, ignores misrepresentative class distributions in the database, and stops training when decision boundaries are sufficiently sampled. These augmented random decision trees enable fast investigation of multiple images to train a reliable, mission-specific ATR. This paper presents the augmented random decision tree framework, develops the sampling procedure for efficient construction of the sample, and illustrates the procedure using relevant examples.

  10. 10 CFR 830 Major Modification Determination for Replacement of ATR Primary Coolant Pumps and Motors

    SciTech Connect

    Noel Duckwitz

    2011-05-01

    The continued safe and reliable operation of the ATR is critical to the Department of Energy (DOE) Office of Nuclear Energy (NE) mission. While ATR is safely fulfilling current mission requirements, a variety of aging and obsolescence issues challenge ATR engineering and maintenance personnel’s capability to sustain ATR over the long term. First documented in a series of independent assessments, beginning with an OA Environmental Safety and Health Assessment conducted in 2003, the issues were validated in a detailed Material Condition Assessment (MCA) conducted as a part of the ATR Life Extension Program in 2007.Accordingly, near term replacement of aging and obsolescent original ATR equipment has become important to ensure ATR capability in support of NE’s long term national missions. To that end, a mission needs statement has been prepared for a non-major system acquisition which is comprised of three interdependent subprojects. The first project will replace the existent diesel-electrical bus (E-3), switchgear, and the 50-year-old obsolescent marine diesels with commercial power that is backed with safety related emergency diesel generators, switchgear, and uninterruptible power supply (UPS). The second project, the subject of this major modification determination, will replace the four, obsolete, original primary coolant pumps (PCPs) and motors. Completion of this and the two other age-related projects (replacement of the ATR diesel bus [E-3] and switchgear and replacement of the existent emergency firewater injection system) will resolve major age-related operational issues plus make a significant contribution in sustaining the ATR safety and reliability profile. The major modification criteria evaluation of the project pre-conceptual design identified several issues that lead to the conclusion that the project is a major modification: 1. Evaluation Criteria #3 (Change of existing process). The proposed strategy for equipping the replacement PCPs with VFDs and having the PCPs also function as ECPs will require significant safety basis changes requiring DOE approval. 2. Evaluation Criteria #4 (Use of new technology). The use of VFD and VFD “pump catcher” technology for the PCPs is not currently in use and has not been previously formally reviewed/approved by DOE for ATR. It is noted that VFD technology has several decades of commercial use and experience. However, the ATR probabilistic risk assessment will have to be updated, reflecting the changes for supplying ECP flows including VFD reliability, to confirm that the proposed activity maintains or reduces the CDF for the ATR. 3. Evaluation Criteria #5 (Create the need for new or revised safety SSCs). It is expected that the proposed activity will result in a revised list of safety-related SSCs. Specifically, as currently proposed, the existing ECPs will be deleted from the list. The PCPs and their associated components, picking up the ECP function, will be classified as safety-related active Seismic Category I.

  11. Function of the ATR N-terminal domain revealed by an ATM/ATR chimera

    SciTech Connect

    Chen Xinping; Zhao Runxiang; Glick, Gloria G.; Cortez, David . E-mail: david.cortez@vanderbilt.edu

    2007-05-01

    The ATM and ATR kinases function at the apex of checkpoint signaling pathways. These kinases share significant sequence similarity, phosphorylate many of the same substrates, and have overlapping roles in initiating cell cycle checkpoints. However, they sense DNA damage through distinct mechanisms. ATR primarily senses single stranded DNA (ssDNA) through its interaction with ATRIP, and ATM senses double strand breaks through its interaction with Nbs1. We determined that the N-terminus of ATR contains a domain that binds ATRIP. Attaching this domain to ATM allowed the fusion protein (ATM*) to bind ATRIP and associate with RPA-coated ssDNA. ATM* also gained the ability to localize efficiently to stalled replication forks as well as double strand breaks. Despite having normal kinase activity when tested in vitro and being phosphorylated on S1981 in vivo, ATM* is defective in checkpoint signaling and does not complement cellular deficiencies in either ATM or ATR. These data indicate that the N-terminus of ATR is sufficient to bind ATRIP and to promote localization to sites of replication stress.

  12. Determination of some heavy metals (Fe, Cu, Zn and Pb) in blood by total reflection X-ray fluorescence

    NASA Astrophysics Data System (ADS)

    Bounakhla, M.; Doukkali, A.; Lalaoui, K.; Aguenaou, H.; Mokhtar, N.; Attrassi, B.

    2003-05-01

    The main purpose of this study is the interaction between nutrition (micronutrients heavy metals: Fe, Zn, Cu) and toxic heavy metals such as Pb in blood of children living in Gharb region of Morocco. This region receives all pollution carried by the Sebou river coming mainly from industrial activities. A rapid and simple analytical procedure was used for the determination of Fe, Cu and Zn trace amounts in blood by total-reflection X-ray fluorescence technique. This method is an energy dispersive XRF technique in a special geometry of primary beam, sample and detector. The sample is deposited on a plane polished surface of a suitable reflector material. It is presented as a few drops (25 μl) from a solution of blood digested in a mixture of HNO3 and H2O2 using a microwaves accelerated reaction system. The accuracy of measurements has been investigated by using certified materials. The concentration of Cu was found to be normal in all samples (\\cong1 ppm) which ruled out any interaction between this element and the others. On the other hand, amounts of Fe and Zn are very variables, suggesting an interaction between Fe and Zn. However, amounts of Pb in blood are inferior to 50 ppb, suggesting that no interaction exist with this metal and micronutrients.

  13. Pharmacokinetic detection of penicillin excreted in urine using a totally internally reflected resonance light scattering technique with cetyltrimethylammonium bromide.

    PubMed

    Huang, Cheng Zhi; Feng, Ping; Li, Yuan Fang; Tan, Ke Jun

    2005-05-01

    A quantitative analysis method for penicillins including ampicillin (AmP), benzyl penicillin (BP), oxacillin (OA) and amoxycillin (AmO) is proposed that makes use of the totally internally reflected resonance light scattering (TIR-RLS) signal from the penicillin at the H2O/CCl4 interface in the presence of cetyltrimethylammonium bromide (CTMAB), and enables the pharmacokinetics of penicillin taken orally and excreted through urine to be monitored. Penicillin is coadsorbed with CTMAB at the H2O/CCl4 interface in neutral solution, resulting in the formation of ion associates that display greatly enhanced TIR-RLS signals (maximum at 368-372 nm). This enhanced TIR-RLS intensity was found to be proportional to the penicillin concentration over the range 0.2 x 10(-6) to 2.2 x 10(-6) mol L(-1), with limits of determination (3sigma) of 5.0 x 10(-8) to 7.0 x 10(-8) mol L(-1). Pharmacokinetics studies performed using the present method show that the excretion of orally-taken ampicillin through urine has a half-time of 1.05 h and an excremental quantum over 8 h of 49.3%, respectively. PMID:15900456

  14. A total internal reflection ellipsometry and atomic force microscopy study of interactions between Proteus mirabilis lipopolysaccharides and antibodies.

    PubMed

    Gleńska-Olender, J; Sęk, S; Dworecki, K; Kaca, W

    2015-07-01

    Specific antigen-antibody interactions play a central role in the human immune system. The objective of this paper is to detect immune complexes using label-free detection techniques, that is, total internal reflection ellipsometry (TIRE) and atomic force microscopy (AFM)-based topography and recognition imaging. Interactions of purified rabbit immunoglobulin G (IgG) antibodies with bacterial endotoxins (Proteus mirabilis S1959 O3 lipopolysaccharides) were studied. Lipopolysaccharide was adsorbed on gold surface for TIRE. In the AFM imaging experiments, LPS was attachment to the PEG linker (AFM tip modification). The mica surface was covered by IgG. In TIRE, the optical parameters Ψ and Δ change when a complex is formed. It was found that even highly structured molecules, such as IgG antibodies (anti-O3 LPS rabbit serum), preserve their specific affinity to their antigens (LPS O3). LPS P. mirabilis O3 response of rabbit serum anti-O3 was also tested by topography and recognition imaging. Both TIRE and AFM techniques were recruited to check for possible detection of antigen-antibody recognition event. The presented data allow for determination of interactions between a variety of biomolecules. In future research, this technique has considerable potential for studying a wide range of antigen-antibody interactions and its use may be extended to other biomacromolecular systems. PMID:25854960

  15. An in situ attenuated total reflection infrared study of a chiral catalytic solid-liquid interface: cinchonidine adsorption on pt.

    PubMed

    Ferri, D; Bürgi, T

    2001-12-01

    An in situ attenuated total reflection study of the chiral solid-liquid interface created by cinchonidine adsorption on a Pt/Al(2)O(3) model catalyst is presented. Experiments were performed in the presence of dissolved hydrogen, that is under conditions used for the heterogeneous enantioselective hydrogenation of alpha-functionalized ketones. Cinchonidine adsorbs via the quinoline moiety. The adsorption mode is coverage dependent and several species coexist on the surface. At low concentration (10(-6)M) a predominantly flat adsorption mode prevails. At increasing coverage two different tilted species, alpha-H abstracted and N lone pair bonded cinchonidine, are observed. The latter is only weakly bound and in a fast dynamic equilibrium with dissolved cinchonidine. At high concentration (10(-4)-10(-3) M) all three species coexist on the Pt surface. A slow transition from an adsorbate layer with a high fraction of alpha-H abstracted cinchonidine to one with a high fraction of N lone pair bonded cinchonidine is observed with the cinchonidine concentration being the driving force for the process. The reverse transition in the absence of dissolved cinchonidine is fast. Cinchonidine competes with solvent decomposition products for adsorption sites on the Pt, which may contribute to the observed solvent dependence of the heterogeneous enantioselective hydrogenation of ketones by cinchonidine-modified Pt. PMID:11724616

  16. Intelligent Simultaneous Quantitative Online Analysis of Environmental Trace Heavy Metals with Total-Reflection X-Ray Fluorescence

    PubMed Central

    Ma, Junjie; Wang, Yeyao; Yang, Qi; Liu, Yubing; Shi, Ping

    2015-01-01

    Total-reflection X-ray fluorescence (TXRF) has achieved remarkable success with the advantages of simultaneous multi-element analysis capability, decreased background noise, no matrix effects, wide dynamic range, ease of operation, and potential of trace analysis. Simultaneous quantitative online analysis of trace heavy metals is urgently required by dynamic environmental monitoring and management, and TXRF has potential in this application domain. However, it calls for an online analysis scheme based on TXRF as well as a robust and rapid quantification method, which have not been well explored yet. Besides, spectral overlapping and background effects may lead to loss of accuracy or even faulty results during practical quantitative TXRF analysis. This paper proposes an intelligent, multi-element quantification method according to the established online TXRF analysis platform. In the intelligent quantification method, collected characteristic curves of all existing elements and a pre-estimated background curve in the whole spectrum scope are used to approximate the measured spectrum. A novel hybrid algorithm, PSO-RBFN-SA, is designed to solve the curve-fitting problem, with offline global optimization and fast online computing. Experimental results verify that simultaneous quantification of trace heavy metals, including Cr, Mn, Fe, Co, Ni, Cu and Zn, is realized on the online TXRF analysis platform, and both high measurement precision and computational efficiency are obtained. PMID:25954949

  17. Influenza hemagglutinin assumes a tilted conformation during membrane fusion as determined by attenuated total reflection FTIR spectroscopy.

    PubMed Central

    Tatulian, S A; Hinterdorfer, P; Baber, G; Tamm, L K

    1995-01-01

    Fusion of influenza virus with target membranes is mediated by an acid-induced conformational change of the viral fusion protein hemagglutinin (HA) involving an extensive reorganization of the alpha-helices. A 'spring-loaded' displacement over at least 100 A provides a mechanism for the insertion of the fusion peptide into the target membrane, but does not explain how the two membranes are brought into fusion contact. Here we examine, by attenuated total reflection Fourier transform infrared spectroscopy, the secondary structure and orientation of HA reconstituted in planar membranes. At neutral pH, the orientation of the HA trimers in planar membranes is approximately perpendicular to the membrane. However, at the pH of fusion, the HA trimers are tilted 55-70 degrees from the membrane normal in the presence or absence of bound target membranes. In the absence of target membranes, the overall secondary structure of HA at the fusion pH is similar to that at neutral pH, but approximately 50-60 additional residues become alpha-helical upon the conformational change in the presence of bound target membranes. These results are discussed in terms of a structural model for the fusion intermediate of influenza HA. Images PMID:8521808

  18. Concept and setup for intraoperative imaging of tumorous tissue via Attenuated Total Reflection spectrosocopy with Quantum Cascade Lasers

    NASA Astrophysics Data System (ADS)

    Geiger, Florian B.; Koerdel, Martin; Schick, Anton; Heimann, Axel; Matiasek, Kaspar; Herkommer, Alois M.

    2015-03-01

    A major challenge in tumor surgery is the differentiation between normal and malignant tissue. Since an incompletely resected tumor easily leads to recidivism, the gold standard is to remove malignant tissue with a sufficient safety margin and send it to pathology for examination with patho-histological techniques (rapid section diagnosis). This approach, however, exhibits several disadvantages: The removal of additional tissue (safety margin) means additional stress to the patient; the correct interpretation of proper tumor excision relies on the pathologist's experience and the waiting time between resection and pathological result can be more than 45 minutes. This last aspect implies unnecessary occupation of cost-intensive operating room staff as well as longer anesthesia for the patient. Various research groups state that hyperspectral imaging in the mid-infrared, especially in the so called "fingerprint region", allows spatially resolved discrimination between normal and malignant tissue. All these experiments, though, took place in a laboratory environment and were conducted on dried, ex vivo tissue and on a microscopic scale. It is therefore our aim to develop a system incorporating the following properties: Intraoperatively and in vivo applicable, measurement time shorter than one minute, based on mid infrared spectroscopy, providing both spectral and spatial information and no use of external fluorescence markers. Theoretical assessment of different concepts and experimental studies show that a setup based on a tunable Quantum Cascade Laser and Attenuated Total Reflection seems feasible for in vivo tissue discrimination via imaging. This is confirmed by experiments with a first demonstrator.

  19. The use of total reflectance X-ray fluorescence (TXRF) for the determination of metals in the pharmaceutical industry.

    PubMed

    Antosz, Frederick J; Xiang, Yanqiao; Diaz, Angel R; Jensen, Andrew J

    2012-03-25

    The control of residual metals in active pharmaceutical ingredients (API's) and intermediates is critical because of their potential toxic effects. A variety of technologies are available to measure residual metals in pharmaceutical compounds including, AAS, ICP-AES, and ICP-MS. The newest technology is total reflectance X-ray fluorescence spectroscopy (TXRF) which uses primary X-rays to excite atoms which then emit secondary X-rays. The emitted X-rays are characteristic of the individual elements present, and the intensities of the emitted X-rays are proportional to the concentrations of the elements present in the sample. The benefits of TXRF are that it is essentially unaffected by matrix effects, is very sensitive (ppb's), requires small amounts of sample (5-10 mg), and requires very little sample preparation time. During this study, TXRF was used to quantitatively measure residual metals in API's and intermediates and such topics as sample preparation, sensitivity, linearity, reproducibility and accuracy are discussed. The results obtained by TXRF were compared with those obtained by ICP-MS for the same samples for Pd and Cu measurement, and statistical analysis indicated that the results obtained by the two technologies are equivalent at the 95% confidence level. A comparison is also made of the capabilities of the instruments using a tungsten (W) or a molybdenum (Mo) source for excitation. Both instruments could be used for the quantitative determination of residual metals in pharmaceuticals. PMID:22316622

  20. Total reflection X-ray fluorescence analysis of light elements with synchrotron radiation and special X-ray tubes

    NASA Astrophysics Data System (ADS)

    Streli, Christina; Wobrauschek, P.; Bauer, V.; Kregsamer, P.; Görgl, R.; Pianetta, P.; Ryon, R.; Pahlke, S.; Fabry, L.

    1997-07-01

    Total reflection X-ray fluorescence analysis (TXRF) of light elements, such as C, O and Al (atomic numbers 5-13) generally has poor sensitivity and detection limits due to poor excitation and low fluorescent yields. Special excitation sources are necessary to compensate for these physical limitations. Synchrotron radiation is the ideal source for TXRF due to its high intensity and wide spectral range extending into the low energy region required for light elements. For more routine use, special X-ray tubes can be constructed. Experiments have been performed at the Stanford Synchrotron Radiation Laboratory (SSRL) using beamline III-4, which is specially designed for the use of low energy photons. Light elements on Si wafers have been analyzed, leading to detection limits below 100 fg for Na, Mg and Al, which corresponds to about 10 9 atoms. A new vacuum chamber is introduced meeting the requirements of wafer handling without the risk of contamination and offering the possibility of scanning a certain area of the wafer. Boron was detected on a wafer with 10 14 atoms cm -2 implanted in the surface layer. A special windowless X-ray tube with Mo, Al and Si as anode materials was also tested. With the optimization of anode geometry, beam path and excitation conditions, a detection limit of 5 pg (corresponds to 10 11 atoms) for Al was achieved.

  1. A novel total reflection X-ray fluorescence procedure for the direct determination of trace elements in petrochemical products.

    PubMed

    Cinosi, Amedeo; Andriollo, Nunzio; Pepponi, Giancarlo; Monticelli, Damiano

    2011-01-01

    A total reflection X-ray fluorescence (TXRF) procedure was developed for the determination of metal traces in petrochemical end products or intermediates for surfactant synthesis. The method combines a fast and straightforward sample preparation, i.e. deposition on the sample holder and evaporation of the sample matrix, with an efficient quantification method based on internal standardization (organic gallium standard). The method developed showed detection limits below 0.05?gg(-1) and in most cases below 0.005?gg(-1). Fifteen elements (Ca, Cd, Co, Cr, Cu, Fe, Mn, Mo, Ni, Pb, Rh, Sn, Sr, V and Zn) were determined in matrices such as paraffins, n-olefins, linear alkylbenzenes, long-chain alkyl alcohols and esters: typical metal contents were below 1?gg(-1). The results were compared with the reference method ASTM D5708 (test method B) based on inductively coupled plasma optical emission spectroscopy: advantages and drawbacks of the two procedures were critically evaluated. The TXRF method developed showed comparable precision and absence of bias with respect to the reference method. A comparison of the performances of the two methods is presented. PMID:21046076

  2. Determination of platinum group metal catalyst residues in active pharmaceutical ingredients by means of total reflection X-ray spectrometry

    NASA Astrophysics Data System (ADS)

    Marguí, Eva; Queralt, Ignasi; Hidalgo, Manuela

    2013-08-01

    The control of metal catalyst residues (i.e., platinum group metals (PGMs)) in different stages of the manufacturing processes of the active pharmaceutical ingredients (APIs) and, especially, in the final product is crucial. For API specimens, there are strict guidelines to limit the levels of metal residues based on their individual levels of safety concern. For PGMs the concentration limit has been established at 10 mg/kg in the API. Therefore great effort is currently being devoted to the development of new and simple procedures to control metals in pharmaceuticals. In the present work, an analytical methodology based on benchtop total reflection X-ray fluorescence spectrometry (TXRF) has been developed for the rapid and simple determination of some PGM catalyst impurities (Rh, Pd, Ir and Pt) in different types of API samples. An evaluation of different sample treatments (dissolution and digestion of the solid pharmaceutical samples) has been carried out and the developed methodologies have been validated according to the analytical parameters to be considered and acceptance criteria for PGM determination according to the United States Pharmacopeia (USP). Limits of quantification obtained for PGM metals were in the range of 2-4 mg/kg which are satisfactory according to current legislation. From the obtained results it is shown that the developed TXRF method can be implemented in the pharmaceutical industries to increase productivity of the laboratory; offering an interesting and complementary analytical tool to other atomic spectroscopic methods.

  3. Vapor phase decomposition droplet collection total reflection X-ray fluorescence spectrometry for metallic contamination analysis on Ge wafers

    NASA Astrophysics Data System (ADS)

    Hellin, D.; Geens, V.; Teerlinck, I.; Van Steenbergen, J.; Rip, J.; Laureyn, W.; Raskin, G.; Mertens, P. W.; De Gendt, S.; Vinckier, C.

    2005-02-01

    Ge substrates are recently being reconsidered as a candidate material for the replacement of Si substrates in advanced semiconductor devices. The reintroduction of this material requires reengineering of the standard IC processing steps. In this paper, we present the extension of the methodology of vapor phase decomposition-droplet collection-total reflection X-ray fluorescence spectrometry (VPD-DC-TXRF) for metallic contamination analysis towards Ge substrates. A first step that asked for adaptation was the collection chemistry as the Ge wafers surface is not hydrophobic after the VPD treatment. The contact angle could be significantly increased using a concentrated HCl solution. This chemistry has been proved to perform well in the collection of metals from intentionally contaminated Ge wafers. A second step that needed optimization was the matrix removal method as a sample preparation step prior to the TXRF analysis. First, the upper limits of TXRF on Ge containing solutions have been characterized. The accuracy of TXRF is found to be acceptable for Ge contents lower than 1×10 14 atoms (250 ppb in 50 μL) but decreases systematically with higher Ge contents. Fortunately, Ge can be volatilized at low temperatures as GeCl 4 by the addition of HCl. The parameters within this method have been investigated with respect to the removal of Ge and the recovery of metal traces. Finally, the full VPD-DC-TXRF method has been applied on intentionally contaminated Ge wafers and proved to be very accurate.

  4. Assessment of serum selenium levels in 2-month-old sucking calves using total reflection X-ray fluorescence technique

    NASA Astrophysics Data System (ADS)

    Buoso, M. C.; Ceccato, D.; Moschini, G.; Bernardini, D.; Testoni, S.; Torboli, A.; Valdes, M.

    2001-11-01

    The assessment of selenium status of livestock plays an important role in the production of medicine since low serum Se levels influence disease resistance in ruminants. It has been proved that Se deficiency may cause muscular dystrophy, cardiomyopathy and even death. Serum level has been widely used to evaluate the Se short-term status in animals since there is a good association between serum Se level and the dietary intake of the element over a wide range. The purpose of this work was to determine the Se serum concentration in a population of 78 sucking 2-month-old calves, in order to corroborate a clinical diagnosis of severe deficiency status. The samples were analyzed by total reflection X-ray fluorescence (TXRF) at the ITAL STRUCTURES Research Laboratory. The results obtained from the serum samples presented Se concentrations varying from 10 to 66 ng/ml. The comparison between the obtained values and the expected serum selenium values (60-80 ng/ml), confirmed a mild to severe deficiency status in the investigated population.

  5. Inorganic pigment study of the San Pedro Gonzalez Telmo Sibyls using total reflection X-ray fluorescence

    NASA Astrophysics Data System (ADS)

    Vázquez, Cristina; Custo, Graciela; Barrio, Néstor; Burucúa, José; Boeykens, Susana; Marte, Fernando

    2010-09-01

    This article describes the study carried out on a series of oil paintings on canvas from the eighteenth century that were restored at Centro de Producción e Investigación en Restauración y Conservación Artística y Bibliográfica - Tarea (CEIRCAB-Tarea), Buenos Aires, Argentina: the San Pedro González Telmo Sibyls. Experimental study was undertaken to identify inorganic pigments and the technique used in their confection; and, in this way, try to add information about their local origin. Therefore special emphasis was put to infer technologies used in the manufacturing of these paintings. Elemental analysis was performed by total reflection X-ray fluorescence spectrometry (TXRF) and complemented by optical and polarized light microscopy. Microsampling was carefully done over areas of the paintings which were damaged and where a small additional loss will not be noticed. This investigation has shown that a variety of pigments were used, namely earth pigments (red and yellow ochres), white lead, vermilion, etc., and they were used either pure or in mixtures. This characterization helped conservators in their decisions regarding a better understanding of the deterioration processes. In addition, this research about the material composition allowed the art historians and restorers the possibility to obtain information about where, when or by whom The San Pedro González Telmo Sibyls may have been painted.

  6. ATR promotes cilia signalling: links to developmental impacts.

    PubMed

    Stiff, Tom; Casar Tena, Teresa; O'Driscoll, Mark; Jeggo, Penny A; Philipp, Melanie

    2016-04-15

    Mutations inATR(ataxia telangiectasia and RAD3-related) cause Seckel syndrome (ATR-SS), a microcephalic primordial dwarfism disorder. Hitherto, the clinical manifestation of ATR deficiency has been attributed to its canonical role in DNA damage response signalling following replication fork stalling/collapse. Here, we show that ATR regulates cilia-dependent signalling in a manner that can be uncoupled from its function during replication. ATR-depleted or patient-derived ATR-SS cells form cilia of slightly reduced length but are dramatically impaired in cilia-dependent signalling functions, including growth factor and Sonic hedgehog signalling. To better understand the developmental impact of ATR loss of function, we also used zebrafish as a model. Zebrafish embryos depleted of Atr resembled ATR-SS morphology, showed a modest but statistically significant reduction in cilia length and other morphological features indicative of cilia dysfunction. Additionally, they displayed defects in left-right asymmetry including ambiguous expression ofsouthpaw, incorrectly looped hearts and randomized localization of internal organs including the pancreas, features typically conferred by cilia dysfunction. Our findings reveal a novel role for ATR in cilia signalling distinct from its canonical function during replication and strengthen emerging links between cilia function and development. PMID:26908596

  7. ATR promotes cilia signalling: links to developmental impacts

    PubMed Central

    Stiff, Tom; Casar Tena, Teresa; O'Driscoll, Mark; Jeggo, Penny A.; Philipp, Melanie

    2016-01-01

    Mutations in ATR (ataxia telangiectasia and RAD3-related) cause Seckel syndrome (ATR-SS), a microcephalic primordial dwarfism disorder. Hitherto, the clinical manifestation of ATR deficiency has been attributed to its canonical role in DNA damage response signalling following replication fork stalling/collapse. Here, we show that ATR regulates cilia-dependent signalling in a manner that can be uncoupled from its function during replication. ATR-depleted or patient-derived ATR-SS cells form cilia of slightly reduced length but are dramatically impaired in cilia-dependent signalling functions, including growth factor and Sonic hedgehog signalling. To better understand the developmental impact of ATR loss of function, we also used zebrafish as a model. Zebrafish embryos depleted of Atr resembled ATR-SS morphology, showed a modest but statistically significant reduction in cilia length and other morphological features indicative of cilia dysfunction. Additionally, they displayed defects in left-right asymmetry including ambiguous expression of southpaw, incorrectly looped hearts and randomized localization of internal organs including the pancreas, features typically conferred by cilia dysfunction. Our findings reveal a novel role for ATR in cilia signalling distinct from its canonical function during replication and strengthen emerging links between cilia function and development. PMID:26908596

  8. Classification of agents using Syrian hamster embryo (SHE) cell transformation assay (CTA) with ATR-FTIR spectroscopy and multivariate analysis.

    PubMed

    Ahmadzai, Abdullah A; Trevisan, Jlio; Pang, Weiyi; Riding, Matthew J; Strong, Rebecca J; Llabjani, Valon; Pant, Kamala; Carmichael, Paul L; Scott, Andrew D; Martin, Francis L

    2015-09-01

    The Syrian hamster embryo (SHE) cell transformation assay (pH 6.7) has a reported sensitivity of 87% and specificity of 83%, and an overall concordance of 85% with in vivo rodent bioassay data. To date, the SHE assay is the only in vitro assay that exhibits multistage carcinogenicity. The assay uses morphological transformation, the first stage towards neoplasm, as an endpoint to predict the carcinogenic potential of a test agent. However, scoring of morphologically transformed SHE cells is subjective. We treated SHE cells grown on low-E reflective slides with 2,6-diaminotoluene, N-nitroso-N-ethylnitroguanidine, N-nitroso-N-methylurea, N-nitroso-N-ethylurea, EDTA, dimethyl sulphoxide (DMSO; vehicle control), methyl methanesulfonate, benzo[e]pyrene, mitomycin C, ethyl methanesulfonate, ampicillin or five different concentrations of benzo[a]pyrene. Macroscopically visible SHE colonies were located on the slides and interrogated using attenuated total reflection Fourier-transform infrared (ATR-FTIR) spectroscopy acquiring five spectra per colony. The acquired IR data were analysed using Fisher's linear discriminant analysis (LDA) followed by principal component analysis (PCA)-LDA cluster vectors to extract major and minor discriminating wavenumbers for each treatment class. Each test agent vs. DMSO and treatment-induced transformed cells vs. corresponding non-transformed were classified by a unique combination of major and minor discriminating wavenumbers. Alterations associated with Amide I, Amide II, lipids and nucleic acids appear to be important in segregation of classes. Our findings suggest that a biophysical approach of ATR-FTIR spectroscopy with multivariate analysis could facilitate a more objective interrogation of SHE cells towards scoring for transformation and ultimately employing the assay for risk assessment of test agents. PMID:25925069

  9. Hyperspectral Sensing for Turbid Water Quality Monitoring in Freshwater Rivers: Empirical Relationship between Reflectance and Turbidity and Total Solids

    PubMed Central

    Wu, Jiunn-Lin; Ho, Chung-Ru; Huang, Chia-Ching; Srivastav, Arun Lal; Tzeng, Jing-Hua; Lin, Yao-Tung

    2014-01-01

    Total suspended solid (TSS) is an important water quality parameter. This study was conducted to test the feasibility of the band combination of hyperspectral sensing for inland turbid water monitoring in Taiwan. The field spectral reflectance in the Wu river basin of Taiwan was measured with a spectroradiometer; the water samples were collected from the different sites of the Wu river basin and some water quality parameters were analyzed on the sites (in situ) as well as brought to the laboratory for further analysis. To obtain the data set for this study, 160 in situ sample observations were carried out during campaigns from August to December, 2005. The water quality results were correlated with the reflectivity to determine the spectral characteristics and their relationship with turbidity and TSS. Furthermore, multiple-regression (MR) and artificial neural network (ANN) were used to model the transformation function between TSS concentration and turbidity levels of stream water, and the radiance measured by the spectroradiometer. The value of the turbidity and TSS correlation coefficient was 0.766, which implies that turbidity is significantly related to TSS in the Wu river basin. The results indicated that TSS and turbidity are positively correlated in a significant way across the entire spectrum, when TSS concentration and turbidity levels were under 800 mg·L−1 and 600 NTU, respectively. Optimal wavelengths for the measurements of TSS and turbidity are found in the 700 and 900 nm range, respectively. Based on the results, better accuracy was obtained only when the ranges of turbidity and TSS concentration were less than 800 mg·L−1 and less than 600 NTU, respectively and used rather than using whole dataset (R2 = 0.93 versus 0.88 for turbidity and R2 = 0.83 versus 0.58 for TSS). On the other hand, the ANN approach can improve the TSS retrieval using MR. The accuracy of TSS estimation applying ANN (R2 = 0.66) was better than with the MR approach (R2 = 0.58), as expected due to the nonlinear nature of the transformation model. PMID:25460816

  10. Hyperspectral sensing for turbid water quality monitoring in freshwater rivers: Empirical relationship between reflectance and turbidity and total solids.

    PubMed

    Wu, Jiunn-Lin; Ho, Chung-Ru; Huang, Chia-Ching; Srivastav, Arun Lal; Tzeng, Jing-Hua; Lin, Yao-Tung

    2014-01-01

    Total suspended solid (TSS) is an important water quality parameter. This study was conducted to test the feasibility of the band combination of hyperspectral sensing for inland turbid water monitoring in Taiwan. The field spectral reflectance in the Wu river basin of Taiwan was measured with a spectroradiometer; the water samples were collected from the different sites of the Wu river basin and some water quality parameters were analyzed on the sites (in situ) as well as brought to the laboratory for further analysis. To obtain the data set for this study, 160 in situ sample observations were carried out during campaigns from August to December, 2005. The water quality results were correlated with the reflectivity to determine the spectral characteristics and their relationship with turbidity and TSS. Furthermore, multiple-regression (MR) and artificial neural network (ANN) were used to model the transformation function between TSS concentration and turbidity levels of stream water, and the radiance measured by the spectroradiometer. The value of the turbidity and TSS correlation coefficient was 0.766, which implies that turbidity is significantly related to TSS in the Wu river basin. The results indicated that TSS and turbidity are positively correlated in a significant way across the entire spectrum, when TSS concentration and turbidity levels were under 800 mg·L(-1) and 600 NTU, respectively. Optimal wavelengths for the measurements of TSS and turbidity are found in the 700 and 900 nm range, respectively. Based on the results, better accuracy was obtained only when the ranges of turbidity and TSS concentration were less than 800 mg·L(-1) and less than 600 NTU, respectively and used rather than using whole dataset (R(2) = 0.93 versus 0.88 for turbidity and R(2) = 0.83 versus 0.58 for TSS). On the other hand, the ANN approach can improve the TSS retrieval using MR. The accuracy of TSS estimation applying ANN (R(2) = 0.66) was better than with the MR approach (R(2) = 0.58), as expected due to the nonlinear nature of the transformation model. PMID:25460816

  11. Deposition from dopamine solutions at Ge substrates: an in situ ATR-FTIR study.

    PubMed

    Müller, Martin; Kessler, Bernd

    2011-10-18

    Deposition from dopamine (DA) solutions at germanium (Ge) model substrates was monitored under stationary conditions using surface sensitive in situ attenuated total reflection Fourier transform infrared (ATR-FTIR) spectroscopy. ATR-FTIR spectra of the interfacial organic layer formed upon contact of TRIS buffered aqueous DA solutions to a Ge internal reflection element (IRE) showed conveniently strong diagnostic IR absorption bands, which were increasing with deposition time up to at least 6 h. Comparison of IR spectra of unreacted pristine DA, surface reacted, and bulk reacted material confirmed chemical reactions of DA to a polymerizate according to the literature. The found IR bands could be assigned to aromatic as well as C-O single bond moieties. The kinetic courses of the diagnostic band integrals showed an initial increase and saturation of the deposition after around 300 min, which could be empirically represented by an exponential damping function revealing a rather small kinetic constant. Highest deposition levels were found at pH = 8.5 (TRIS buffer or NaOH) in contrast to pH = 6.2, where no deposition occurred. Minor deposition was found in the presence of salt or at ZnSe instead of Ge due to the absence of reactive hydroxyl groups. The concentration dependence of DA deposition showed an initial increase and a saturation beginning at around 0.4 mg/mL (0.0022 M), where around 50 nm thick films featuring granular surface morphologies are formed. The adsorbed species are suggested to be smaller bulk reacted DA polymerizate particles with reactive end groups. Rinsing the formed films by pure TRIS buffer resulted in a time dependent release of deposited organic material by ≈23%, which could be represented by an exponential decay function. A saturation of the release after around 100 min and a larger kinetic constant compared to deposition could be determined. The released material is suggested to be larger aggregated bulk reacted DA polymerizate particles loosely bound to the surface by weak interaction forces. PMID:21866968

  12. [Estimating total nitrogen content in reclaimed water based on hyperspectral reflectance information from emergent plants: a case study of Mencheng Lake Wetland Park in Beijing, China].

    PubMed

    Liu, Hui; Gong, Zhao-ning; Zhao, Wen-ji

    2014-12-01

    Hyperspectral reflectance information is a crucial method to detect total nitrogen content in plant leaves, meanwhile, vegetation nitrogen content has a strong relationship with nitrogen in water. Taking Mencheng Lake Wetland Park supplied with reclaimed water as study area, the vegetation hyperspectral data (Phragmites australis and Typha angustifolia), and the content of total nitrogen in water were detected to investigate the feasibility of estimating total nitrogen content in reclaimed water based on hyperspectral reflectance information from emergent plants. We established simple linear regression model, stepwise multiple linear regression model and partial least square regression model based on four hyperspectral indices (spectral indices, normalized difference indices, trilateral parameters, absorption feature parameters), respectively. The accuracy of these models was coefficient of determination (R2) and root mean square error (RMSE). The results showed that stepwise multiple linear regression model and partial least square regression model predicted more accurately than simple linear regression model, and the accuracy of prediction models based on P. australis reflectance spectra was higher than those on T. angustifolia. Partial least square regression model was the most useful explorative tool for unraveling the relationship between spectral reflectance of P. australis and total nitrogen content in water with R2 of 0.854 and RMSE of 0.647. 500-700 nm was the best band range for detecting water total nitrogen content. The reflectance ratio of green peak and red valley could be effectively predicted by the absorption feature parameters. PMID:25876415

  13. Total reflection X-ray fluorescence analysis of oral fluids of women affected by osteoporosis and osteopenia

    NASA Astrophysics Data System (ADS)

    Sánchez, Héctor Jorge; Valentinuzzi, María Cecilia; Grenón, Miram; Abraham, José

    2008-12-01

    Osteoporosis is a disease characterized by low bone mass and microarchitectural deterioration of bone tissue, leading to bone fragility and an increased susceptibility to fractures; the early stage of decreased bone density is called osteopenia. More than 200 million people are affected and about 50% of post-menopausic women are expected to develop the disease. Osteoporosis, osteopenia and periodontal disease have in common several risk factors, being hyperthyroidism and smoking habits the most important ones. There is scarce information in the literature about the association between periodontal disease and osteoporosis and/or osteopenia. Some works suggest that osteoporotic women are susceptible to a higher loss of periodontal insertion, alveolar bones, and teeth. Thirty adult post-menopausic women were studied; some of them were healthy (control group) and the rest of them were undergoing some stage of osteoporosis or osteopenia. All the subjects were healthy, non-smokers, not having dental implants, and with communitarian periodontal index higher than 1(CPI > 1). Samples of saliva and gingival crevice fluid were extracted with calibrated micro-capillaries and deposited on Si reflectors. Known amounts of Ga were added to the samples in order to act as internal standard for quantification by the total reflection x-ray fluorescence technique. Experimental concentrations of several elements (P, S, Cl, K, Ca, Cr, Fe, NI, Cu, and Zn) were determined. The concentration of some elements in saliva showed different behavior as compared to gingival crevice fluid. Some critical elements of bone composition, such as Ca and Zn, present very distinguishable behavior. Improvements in the statistics are required for a better assessment of a routine method and to establish some correlation with periodontal disease. TXRF seems to be a promising method to evaluate the evolution of osteoporosis.

  14. Analysis of low Z elements in various environmental samples with total reflection X-ray fluorescence (TXRF) spectrometry

    NASA Astrophysics Data System (ADS)

    Hoefler, H.; Streli, C.; Wobrauschek, P.; Óvári, M.; Záray, Gy.

    2006-11-01

    Recently there is a growing interest in low Z elements such as carbon, oxygen up to sulphur and phosphorus in biological specimen. Total reflection X-ray fluorescence (TXRF) spectrometry is a suitable technique demanding only very small amounts of sample. On the other side, the detection of low Z elements is a critical point of this analytical technique. Besides other effects, self absorption may occur in the samples, because of the low energy of the fluorescence radiation. The calibration curves might be not linear any longer. To investigate this issue water samples and samples from human cerebrospinal fluid were used to examine absorption effects. The linearity of calibration curves in dependence of sample mass was investigated to verify the validity of the thin film approximation. The special requirements to the experimental setup for low Z energy dispersive fluorescence analysis were met by using the Atominstitute's TXRF vacuum chamber. This spectrometer is equipped with a Cr-anode X-ray tube, a multilayer monochromator and a SiLi detector with 30 mm 2 active area and with an ultrathin entrance window. Other object on this study are biofilms, living on all subaqueous surfaces, consisting of bacteria, algae and fungi embedded in their extracellular polymeric substances (EPS). Many trace elements from the water are bound in the biofilm. Thus, the biofilm is a useful indicator for polluting elements. For biomonitoring purposes not only the polluting elements but also the formation and growth rate of the biofilm are important. Biofilms were directly grown on TXRF reflectors. Their major elements and C-masses correlated to the cultivation time were investigated. These measured masses were related to the area seen by the detector, which was experimentally determined. Homogeneity of the biofilms was checked by measuring various sample positions on the reflectors.

  15. Reversible and Irreversible Adhesion of Motile Escherichia coli Cells Analyzed by Total Internal Reflection Aqueous Fluorescence Microscopy

    PubMed Central

    Vigeant, Margot A.-S.; Ford, Roseanne M.; Wagner, Michael; Tamm, Lukas K.

    2002-01-01

    The initial events in bacterial adhesion are often explained as resulting from electrostatic and van der Waals forces between the cell and the surface, as described by DLVO theory (developed by Derjaguin, Landau, Verwey, and Overbeek). Such a theory predicts that negatively charged bacteria will experience greater attraction toward a negatively charged surface as the ionic strength of the medium is increased. In the present study we observed both smooth-swimming and nonmotile Escherichia coli bacteria close to plain, positively, and hydrophobically coated quartz surfaces in high- and low-ionic-strength media by using total internal reflection aqueous fluorescence microscopy. We found that reversibly adhering cells (cells which continue to swim along the surface for extended periods) are too distant from the surface for this behavior to be explained by DLVO-type forces. However, cells which had become immobilized on the surface did seem to be affected by electrostatic interactions. We propose that the “force” holding swimming cells near the surface is actually the result of a hydrodynamic effect, causing the cells to swim at an angle along the glass, and that DLVO-type forces are responsible only for the observed immobilization of irreversibly adhering cells. We explain our observations within the context of a conceptual model in which bacteria that are interacting with the surface may be thought of as occupying one of three compartments: bulk fluid, near-surface bulk, and near-surface constrained. A cell in these compartments feels either no effect of the surface, only the hydrodynamic effect of the surface, or both the hydrodynamic and the physicochemical effects of the surface, respectively. PMID:12039734

  16. Application of CO2 Snow Jet Cleaning in Conjunction with Laboratory Based Total Reflection X-Ray Fluorescence

    NASA Technical Reports Server (NTRS)

    Schmeling, M.; Burnett, D. S.; Allton, J. H.; Rodriquez, M.; Tripa, C. E.; Veryovkin, I. V.

    2013-01-01

    The Genesis mission was the first mission returning solar material to Earth since the Apollo program [1,2]. Unfortunately the return of the space craft on September 8, 2004 resulted in a crash landing, which shattered the samples into small fragments and exposed them to desert soil and other debris. Thus only small fragments of the original collectors are available, each having different degrees of surface contamination. Thorough surface cleaning is required to allow for subsequent analysis of solar wind material embedded within. An initial cleaning procedure was developed in coordination with Johnson Space Center which focused on removing larger sized particulates and a thin film organic contamination acquired during collection in space [3]. However, many of the samples have additional residues and more rigorous and/or innovative cleaning steps might be necessary. These cleaning steps must affect only the surface to avoid leaching and re-distribution of solar wind material from the bulk of the collectors. To aid in development and identification of the most appropriate cleaning procedures each sample has to be thoroughly inspected before and after each cleaning step. Laboratory based total reflection X-ray fluorescence (TXRF) spectrometry lends itself to this task as it is a non-destructive and surface sensitive analytical method permitting analysis of elements from aluminum onward present at and near the surface of a flat substrate [4]. The suitability of TXRF has been demonstrated for several Genesis solar wind samples before and after various cleaning methods including acid treatment, gas cluster ion beam, and CO2 snow jet [5 - 7]. The latter one is non-invasive and did show some promise on one sample [5]. To investigate the feasibility of CO2 snow jet cleaning further, several flown Genesis samples were selected to be characterized before and after CO2 snow application with sample 61052 being discussed below.

  17. Determination of trace elements in freshwater rotifers and ciliates by total reflection X-ray fluorescence spectrometry

    NASA Astrophysics Data System (ADS)

    Woelfl, S.; Óvári, M.; Nimptsch, J.; Neu, T. R.; Mages, M.

    2016-02-01

    Element determination in plankton is important for the assessment of metal contamination of aquatic environments. Until recently, it has been difficult to determine elemental content in rotifers or ciliates derived from natural plankton samples because of the difficulty in handling and separation of these fragile organisms. The aim of this study was to evaluate methods for separation of rotifers and large ciliates from natural plankton samples (μg range dry weight) and subsequent analysis of their elemental content using total-reflection X-ray fluorescence spectrometry (TXRF). Plankton samples were collected from different aquatic environments (three lakes, one river) in Chile, Argentina and Hungary. From one to eighty specimens of five rotifer species (Brachionus calyciflorus, Brachionus falcatus, Asplanchna sieboldii, Asplanchna sp., Philodina sp.) and four to twelve specimens of one large ciliate (Stentor amethystinus) were prepared according to the dry method originally developed for microcrustaceans, and analysed by TRXF following in situ microdigestion. Our results demonstrated that it possible to process these small and fragile organisms (individual dry mass: 0.17-9.39 μg ind- 1) via careful washing and preparation procedures. We found species-dependent differences of the element mass fractions for some of the elements studied (Cr, Mn, Fe, Ni, Cu, Zn, As, Pb), especially for Cu, Fe and Mn. One large rotifer species (A. sieboldii) also showed a negative correlation between individual dry weight and the element content for Pb, Ni and Cr. We conclude that our application of the in situ microdigestion-TRXF method is suitable even for rotifers and ciliates, greatly expanding the possibilities for use of plankton in biomonitoring of metal contamination in aquatic environments.

  18. Calibration of straight total reflection X-ray fluorescence spectrometry — results of a European Round Robin test

    NASA Astrophysics Data System (ADS)

    Rink, I.; Rostam-Khani, P.; Knoth, J.; Schwenke, H.; de Gendt, S.; Wortelboer, R.

    2001-11-01

    Calibration of straight total reflection X-ray fluorescence measurements (TXRF) is a matter of discussion for those TXRF users who apply a droplet standard for straight TXRF measurements, at the angle of incidence where particle and film-type contamination show the same fluorescence intensity — the so-called iso-angle as Round Robin tests in the past showed. In order to gain more insight into the differences between several TXRF-equipment types and calibration methods a European Round Robin test was started in 1998 in which 12 companies participated. The Round Robin test comprises 20 different TXRF-tools and one Synchrotron Radiation (SR)-TXRF. Rutherford Back-Scattering measurements (RBS) were performed as absolute reference. Silicon wafers intentionally contaminated by spin-coating and dipping in a spiked NH 4OH/H 2O 2-solution (SC1), respectively, served as test-targets. With exception of one outlier, the results of the comparative analyses can be classified into three groups with similar values. The first group includes the RBS-results, the results of one very old Atomika tool, the results of one Rigaku-tool and those measurements based on special film-type standard wafers or an absolute TXRF calibration method. The second group, including most of the tools from the new Atomika generation, the TREX and the ESRF-beam line, shows an average deviation compared to group 1 by a factor of 1.4, and the third group, containing most of the older Atomika-tools, shows a deviation of 1.8. From these results, it can be concluded that a good calibration of straight TXRF-measurements is mainly determined by the accordance of contamination type on the calibration wafer and the unknown sample. For offsets between these, the application of the bulk sample calibration method or the use of a correction factor is needed.

  19. Combining Mass Spectrometry and ATR-FTIR Spectroscopy to Study Phase, Diffusion and Composition of Secondary Organic Aerosol from the Ozonolysis of α-pinene

    NASA Astrophysics Data System (ADS)

    Perraud, V. M.; Finlayson-Pitts, B. J.; Waring-Kidd, C.

    2014-12-01

    Secondary organic aerosol (SOA) is ubiquitous in the atmosphere and composes a large fraction of the total aerosol budget. Recent reports from field measurements and laboratory studies show that some SOA particles are better represented by a semi-solid low viscosity tar-like material rather than a ideal liquid often assumed in regional and global models. Characterizing the phase of SOA is crucial to understanding how particles interact with trace gases and how it ultimately impacts their growth and evolution in the atmosphere. We report here laboratory studies carried out in the unique UCI large-volume, slow-flow, aerosol flow reactor. Particles from the ozonolysis of a-pinene were formed at various relative humidities (RH from < 3% to 90%) and collected onto a custom ATR-FTIR impactor. The observed impaction pattern provided insights into changes in phase/viscosity of the SOA as a function of relative humidity. In addition, attenuated total reflectance FTIR and mass spectrometry measurements provided information on simultaneous changes on composition. Application of ATR-FTIR combined with PTR-MS provided additional data on the volatility of the SOA at room temperature and diffusion coefficients of two key components pinonaldehyde and acetic acid present in the SOA. Implication for modeling the growth and ultimately the lifetime of SOA in the atmosphere will be discussed.

  20. Structural characterization of nylon 7 by solid-state NMR, DSC, and ATR-FTIR

    NASA Astrophysics Data System (ADS)

    Johnson, C. G.; Mathias, L. J.

    1993-06-01

    Samples of commercial nylon 7 were given different thermal or precipitation histories. Structure and crystallinity were followed by DSC, solid-state NMR, and attenuated total reflectance FTIR (ATR-FTIR). Delta H and T(sub m) values ranged from 52 to 93 J/g and 228 to 242 C, respectively. Surprisingly, annealing did not give material with the greatest delta H although it possessed the highest melting point. Solid-state C-13 and N-15 NMR methods were used to observe the amorphous and crystalline fractions. For example, the amide nitrogens show resonances near 86.5 ppm in amorphous domains, near 84 ppm in alpha-crystals, and near 89 ppm in gamma-crystals. N-15 CP/MAS spectra of solution cast samples contained peaks consistent with all three domains in various intensity ratios but with the gamma-peak being the most intense for most samples. Solid-state C-13 spectra contained peaks which supported the presence of these phases but with the alpha-phase peaks predominating.

  1. Computer analysis of ATR-FTIR spectra of paint samples for forensic purposes

    NASA Astrophysics Data System (ADS)

    Szafarska, Małgorzata; Woźniakiewicz, Michał; Pilch, Mariusz; Zięba-Palus, Janina; Kościelniak, Paweł

    2009-04-01

    A method of subtraction and normalization of IR spectra (MSN-IR) was developed and successfully applied to extract mathematically the pure paint spectrum from the spectrum of paint coat on different bases, both acquired by the Attenuated Total Reflectance Fourier Transform Infrared (ATR-FTIR) technique. The method consists of several stages encompassing several normalization and subtraction processes. The similarity of the spectrum obtained with the reference spectrum was estimated by means of the normalized Manhattan distance. The utility and performance of the method proposed were tested by examination of five different paints sprayed on plastic (polyester) foil and on fabric materials (cotton). It was found that the numerical algorithm applied is able - in contrast to other mathematical approaches conventionally used for the same aim - to reconstruct a pure paint IR spectrum effectively without a loss of chemical information provided. The approach allows the physical separation of a paint from a base to be avoided, hence a time and work-load of analysis to be considerably reduced. The results obtained prove that the method can be considered as a useful tool which can be applied to forensic purposes.

  2. In situ ATR-FTIR study of the early stages of fly ash geopolymer gel formation.

    PubMed

    Rees, Catherine A; Provis, John L; Lukey, Grant C; van Deventer, Jannie S J

    2007-08-14

    The kinetics of geopolymer formation are monitored using a novel in situ attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectroscopic technique. Reaction rates are determined from the intensity variation of the bands related to the geopolymer gel network and the unreacted fly ash particles. Comparison with deuterated geopolymer samples provides critical information regarding peak assignments. An initial induction (lag) period is observed to occur for hydroxide-activated geopolymers, followed by gel evolution according to an approximately linear reaction profile. The length of the lag period is reduced by increasing the concentration of NaOH. An increase in the rate of network formation also occurs with increasing NaOH concentration up to a maximum point, beyond which an increased NaOH concentration leads to a reduced rate of network formation. This trend is attributed to the competing effects of increased alkalinity and stronger ion pairing with an increase in NaOH concentration. In situ analysis also shows that the rate of fly ash dissolution is similar for all moderate- to high-alkali geopolymer slurries, which is attributed to the very highly water-deficient nature of these systems and is contrary to predictions from classical glass dissolution chemistry. This provides for the first time detailed kinetic information describing fly ash geopolymer formation kinetics. PMID:17658864

  3. ATR-FTIR spectroscopic studies of boric acid adsorption on hydrous ferric oxide

    NASA Astrophysics Data System (ADS)

    Peak, Derek; Luther, George W.; Sparks, Donald L.

    2003-07-01

    Boron is an important micronutrient for plants, but high B levels in soils are often responsible for toxicity effects in plants. It is therefore important to understand reactions that may affect B availability in soils. In this study, Attenuated Total Reflectance Fourier transform Infrared (ATR-FTIR) spectroscopy was employed to investigate mechanisms of boric acid (B(OH) 3) and borate (B(OH) 4-) adsorption on hydrous ferric oxide (HFO). On the HFO surface, boric acid adsorbs via both physical adsorption (outer-sphere) and ligand exchange (inner-sphere) reactions. Both trigonal (boric acid) and tetrahedral (borate) boron are complexed on the HFO surface, and a mechanism where trigonal boric acid in solution reacts to form either trigonal or tetrahedral surface complexes is proposed based upon the spectroscopic results. The presence of outer-sphere boric acid complexes can be explained based on the Lewis acidity of the B metal center, and this complex has important implications for boron transport and availability. Outer-sphere boric acid is more likely to leach downward in soils in response to water flow. Outer-sphere boron would also be expected to be more available for plant uptake than more strongly bound boron complexes, and may more readily return to the soil solution when solution concentrations decrease.

  4. Oriented 1,2-dimyristoyl-sn-glycero-3-phosphorylcholine/ganglioside membranes: a Fourier transform infrared attenuated total reflection spectroscopic study. Band assignments; orientational, hydrational, and phase behavior; and effects of Ca2+ binding.

    PubMed Central

    Mller, E; Giehl, A; Schwarzmann, G; Sandhoff, K; Blume, A

    1996-01-01

    Fourier transform infrared (FTIR) attenuated total reflection (ATR) spectroscopy was used to elucidate the hydration behavior and molecular order of phospholipid/ganglioside bilayers. We examined dry and hydrated films of the gangliosides GM1, deacetyl-GM1, lyso-GM1, deacetyllyso-GM1, and GM3 and oriented mixed films of these gangliosides with 1,2-dimyristoyl-sn-glycero-3-phosphorylcholine (DMPC) using polarized light. Analysis of the amide I frequencies reveals that the amide groups are involved in intermolecular interactions via hydrogen bonds of varying strengths. The tilt angle of the acyl chains of the lipids in mixed films was determined as a function of ganglioside structure. Deacetylation of the sialic acid in the headgroup has a stronger influence on the tilt angle than the removal of the ganglioside fatty acid. The phase behavior was examined by FTIR ATR spectroscopy and by differential scanning calorimetry (DSC) measurements on lipid suspensions. At the same molar concentration, lyso-gangliosides have less effect on changes of transition temperature compared to the double-chain analogs. Distinct differences in the amide band shapes were observed between mixtures with lyso-gangliosides and normal double-chain gangliosides. Determined from the dicroic ratio RATR, the orientation of the COO- group in all DMPC/ganglioside mixtures was found to be relatively fixed with respect to the membrane normal. In 4:1 mixtures of DMPC with GM1 and deacetyl-GM1, the binding of Ca2+ leads to a slight decrease in chain tilt in the gel phase, probably caused by a dehydration of the membrane-water interface. In mixtures of DMPC with GM3 and deacetyl-lyso-GM1, a slight increase in chain tilt is observed. The chain tilt in DMPC/lyso-GM1 mixtures is unchanged. Analysis of the COO- band reveals that Ca2+ does not bind to the carboxylate group of the sialic acid of GM1 and deacetyl-GM1, the mixtures in which a decrease in chain tilt was observed. Binding to the sialic acid was only observed for mixtures of DMPC with GM3, lyso-GM1, and deacetyl-lyso-GM1. Ca2+ obviously accumulates at the bilayer-water interface and leads to partial dehydration of the headgroup region in the gel as well as in the liquid-crystalline phase. This can be concluded from the changes in the amide I band shapes. With the exception of DMPC/deacetyl-GM1, the effects on the ester C==O bands are small. The addition of Ca2+ has minor effects on the phase behavior, with the exception of the DMPC/GM1 mixture. PMID:8874015

  5. [Spectral analysis of ball pen script by FTIR microscope with ATR objective].

    PubMed

    Huang, Tao-Hong; Wu, Tian-Ming

    2007-11-01

    Inspection of ball pen script is very important in public security and justice field. It is difficult to get a good spectrum directly by infrared microscope reflectance mode because of low reflectivity of paper and dark gray in color. The best way to measure low reflectivity sample is by infrared microscope with ATR objective method. Measurement with the microscopic ATR method involves bringing the trace of ball pen ink into contact with the prism. By this method, some mixed spectra of ball pen ink and paper fiber were obtained from one of the actual sample. The spectrum of the paper was subtracted from those mixed spectra and a pure spectrum of the ball pen ink was obtained. In this spectrum, three strong peaks were found 1 581, 1 361 and 1 172 cm(-1) respectively, all from crystal violet, a typical triphenylmethane pigment. Another strong peak at 1 724 cm(-1) is contributed by carbonyl vibration from oil reagent alkyd. A 3D graph, showing the distribution of peak 1 581 cm(-1) in this area, was set up by using mapping software. In the 3D distribution graph, the figure of ball pen trace vividly appeared. This infrared microscope ATR method makes it available to nondestructively inspect original ball pen script. PMID:18260394

  6. On revealing the vertical structure of nanoparticle films with elemental resolution: A total external reflection X-ray standing waves study

    NASA Astrophysics Data System (ADS)

    Zargham, Ardalan; Schmidt, Thomas; Flege, Jan Ingo; Sauerbrey, Marc; Hildebrand, Radowan; Röhe, Sarah; Bäumer, Marcus; Falta, Jens

    2010-02-01

    We present a promising combination of methods to precisely determine the morphology of nanostructures, drawing on the example of monodisperse CoPt nanoparticle films deposited by spin coating and dip coating techniques on functionalized Au substrates. Ex-situ X-ray standing waves in total external reflection combined with X-ray reflectivity measurements were employed to determine element-specific atomic-density distributions in vertical direction.

  7. Impulsive solar X-ray bursts. 4: Polarization, directivity and spectrum of the reflected and total bremsstrahlung radiation from a beam of electrons directed toward the photosphere

    NASA Technical Reports Server (NTRS)

    Langer, S. H.; Petrosian, V.

    1976-01-01

    A Monte Carlo method is described for evaluation of the spectrum, directivity and polarization of X-rays diffusely reflected from stellar photospheres. the accuracy of the technique is evaluated through comparison with analytic results. Using the characteristics of the incident X-rays of the model for solar X-ray flares, the spectrum, directivity and polarization of the reflected and the total X-ray fluxes are evaluated. The results are compared with observations.

  8. Advanced miniature processing handware for ATR applications

    NASA Technical Reports Server (NTRS)

    Chao, Tien-Hsin (Inventor); Daud, Taher (Inventor); Thakoor, Anikumar (Inventor)

    2003-01-01

    A Hybrid Optoelectronic Neural Object Recognition System (HONORS), is disclosed, comprising two major building blocks: (1) an advanced grayscale optical correlator (OC) and (2) a massively parallel three-dimensional neural-processor. The optical correlator, with its inherent advantages in parallel processing and shift invariance, is used for target of interest (TOI) detection and segmentation. The three-dimensional neural-processor, with its robust neural learning capability, is used for target classification and identification. The hybrid optoelectronic neural object recognition system, with its powerful combination of optical processing and neural networks, enables real-time, large frame, automatic target recognition (ATR).

  9. Hollow optical-fiber based infrared spectroscopy for measurement of blood glucose level by using multi-reflection prism

    PubMed Central

    Kino, Saiko; Omori, Suguru; Katagiri, Takashi; Matsuura, Yuji

    2016-01-01

    A mid-infrared attenuated total reflection (ATR) spectroscopy system employing hollow optical fibers and a trapezoidal multi-reflection ATR prism has been developed to measure blood glucose levels. Using a multi-reflection prism brought about higher sensitivity, and the flat and wide contact surface of the prism resulted in higher measurement reproducibility. An analysis of in vivo measurements of human inner lip mucosa revealed clear signatures of glucose in the difference spectra between ones taken during the fasting state and ones taken after ingestion of glucose solutions. A calibration plot based on the absorption peak at 1155 cm−1 that originates from the pyranose ring structure of glucose gave measurement errors less than 20%. PMID:26977373

  10. Hollow optical-fiber based infrared spectroscopy for measurement of blood glucose level by using multi-reflection prism.

    PubMed

    Kino, Saiko; Omori, Suguru; Katagiri, Takashi; Matsuura, Yuji

    2016-02-01

    A mid-infrared attenuated total reflection (ATR) spectroscopy system employing hollow optical fibers and a trapezoidal multi-reflection ATR prism has been developed to measure blood glucose levels. Using a multi-reflection prism brought about higher sensitivity, and the flat and wide contact surface of the prism resulted in higher measurement reproducibility. An analysis of in vivo measurements of human inner lip mucosa revealed clear signatures of glucose in the difference spectra between ones taken during the fasting state and ones taken after ingestion of glucose solutions. A calibration plot based on the absorption peak at 1155 cm(-1) that originates from the pyranose ring structure of glucose gave measurement errors less than 20%. PMID:26977373

  11. A physically-based model for Total Suspended Matter retrieval via hyperspectral reflectance inversion in turbid waters

    NASA Astrophysics Data System (ADS)

    Pitarch, Jaime; Kawka, Marcin; Odermatt, Daniel; Wüest, Alfred

    2013-04-01

    We present an approach to estimate the vertical distribution of total suspended matter (TSM) from above-surface radiometric measurements in inland waters. To obtain the needed ground-truth data, a field campaign was carried out in Lake Constance on May 25, 2012. In spring, Lake Constance receives massive input of suspended particles due to a discharge peak from the Alpine Rhine caused by intensive snow melting. Due to density differences between lake's and river's waters, and also to lake currents, TSM shows with complicated horizontal and vertical variation. We made a transect consisting of 26 points, covering the east part of the lake. We measured light transmissivity along a 10 cm path at the wavelength 650 nm, which was converted to beam attenuation c(z) (1/m). Additionally, we made gravimetric measurements of TSM from surface water TSM(0), which ranged between 0 and 14 mg/l. The regression line c(0)-TSM(0) (r2=0.96) was used as a calibration curve to build TSM(z).Chlorophyll-a was measured with a Trilux fluorometer, from Chelsea Technologies Group. Absorption by CDOM was supposed known, having exponential decay with depth and wavelength. We also took above-surface radiometric measurements with a hand-held spectrometer. Using optical theory, we modelled the water inherent optical properties (IOPs) as formed by four components: pure water, dissolved coloured organic matter (CDOM), chlorophyll-bearing particles and mineral particles. Radiative transfer code (Hydrolight) was used to model the light field. As a derived quantity, the simulated remote sensing reflectance was matched to the measured one. The possibilities of this technique are evaluated and discussed. In particular, how much vertical information can be retrieved from above-surface measurements, having also the physical limitation of light penetration. This work is part of the validation activities for the FP-7 project 263.287 FreshMon (High Resolution Freshwater Monitoring: FreshMon GMES Downstream Services) (www.freshmon.eu), which develops a new service line for the continuous provision of Earth Observation based products, integrated with in situ and hydrodynamic modelling components, for water quality monitoring.

  12. Direct determination of trace elements in boron nitride powders by slurry sampling total reflection X-ray fluorescence spectrometry

    NASA Astrophysics Data System (ADS)

    Amberger, Martin A.; Hltig, Michael; Broekaert, Jos A. C.

    2010-02-01

    The use of slurry sampling total reflection X-ray fluorescence spectrometry (SlS-TXRF) for the direct determination of Ca, Cr, Cu, Fe, Mn and Ti in four boron nitride powders has been described. Measurements of the zeta potential showed that slurries with good stabilities can be obtained by the addition of polyethylenimine (PEI) at a concentration of 0.1 wt.% and by adjusting the pH at 4. For the optimization of the concentration of boron nitride in the slurries the net line intensities and the signal to background ratios were determined for the trace elements Ca and Ti as well as for the internal standard element Ga in the case of concentrations of boron nitride ranging from 1 to 30 mg mL -1. As a compromise with respect to high net line intensities and high signal to background ratios, concentrations of 5 mg mL -1 of boron nitride were found suitable and were used for all further measurements. The limits of detection of SlS-TXRF for the boron nitride powders were found to range from 0.062 to 1.6 ?g g - 1 for Cu and Ca, respectively. Herewith, they are higher than those obtained in solid sampling and slurry sampling graphite furnace atomic absorption spectrometry (SoS-GFAAS, SlS-GFAAS) as well as those of solid sampling electrothermal evaporation inductively coupled plasma optical emission spectrometry (SoS-ETV-ICP-OES). For Ca and Fe as well as for Cu and Fe, however, they were found to be lower than for GFAAS and for ICP-OES subsequent to wet chemical digestion, respectively. The universal applicability of SlS-TXRF to the analysis of samples with a wide variety of matrices could be demonstrated by the analysis of certified reference materials such as SiC, Al 2O 3, powdered bovine liver and borate ore with a single calibration. The correlation coefficients of the plots for the values found for Ca, Fe and Ti by SlS-TXRF in the boron nitride powders as well as in the before mentioned samples versus the reference values for the respective samples over a concentration range from 2.5 to 1470 ?g g - 1 were found to be 0.995, 0.991 and 0.997, respectively.

  13. Orientation of specifically 13C=O labeled phosphatidylcholine multilayers from polarized attenuated total reflection FT-IR spectroscopy.

    PubMed Central

    Hübner, W; Mantsch, H H

    1991-01-01

    Oriented multilayers of 1-myristoyl-2(1-13C)-myristoyl-sn-glycero-3-phosphatidylcholine (2[1-13C]DMPC) and 1-palmitoyl-2(1-13C)-palmitoyl-sn-glycero-3-phosphatidylcholine (2[1-13C]DPPC) were investigated by use of attenuated total reflection infrared spectroscopy with polarized light. Experiments were performed with the aim to determine the orientation of the two ester groups in these phospholipids in the solid state and in the hydrated state at temperatures below and above the respective gel to liquid-crystalline phase transitions. Substitution of the naturally occurring 12C carbonyl carbon atom by 13C in the ester group of the sn-2 chain of DMPC and DPPC shifts the infrared absorption of the carbonyl double bond stretching vibration to lower frequency. This results in two well-resolved ester C=O bands which can be assigned unequivocally to the sn-1 and sn-2 chains as they are separated by more than 40 cm-1. The two ester CO-O single bond stretching vibrations of the molecular fragments-CH2CO-OC-are also affected and the corresponding infrared absorption band shifts by 20 cm-1 on 13C-labeling of the carbonyl carbon atom. From the dichroic ratios of the individual ester bands in 2(1-13C)DMPC and 2(1-13C)DPPC we were able to demonstrate that the sn-1 and sn-2 ester C=O groups are similarly oriented with respect to the bilayer plane, with an angle greater than or equal to 60 degrees relative to the bilayer normal. The two CO-O single bonds on the other hand have very different orientations. The CH2CO-OC fragment of the sn-1 chain is oriented along the direction of the all-trans methylene chain, whereas the same molecular segment of the sn-2 carbon chain is directed toward the bilayer plane. This orientation of the ester groups is retained in the liquid-crystalline phase. The tilt angle of the hydrocarbon all-trans chains, relative to the membrane normal, is 25 degrees in the solid state of DMPC and DPPC multibilayers. In the hydrated gel state this angle varies between 26 degrees and 30 degrees, depending on temperature. Neither the orientation of the phosphate group, nor that of the choline group varies significantly in the different physical states of these phospholipids. PMID:1873463

  14. The effect of surface reflection and clouds on the estimation of total ozone from satellite measurements. [of ultraviolet sunlight scattered from the earth

    NASA Technical Reports Server (NTRS)

    Fraser, R. S.; Ahmad, Z.

    1979-01-01

    The total amount of ozone in a vertical column is being measured by Nimbus 4 and 7 observations of the intensity of ultraviolet sunlight scattered from the earth. The algorithm for deriving the amount of ozone from the observations uses the assumption that the surface reflects the light isotropically and the albedo is independent of wavelength. The effects of anisotropic surfaces and clouds on the estimate of total ozone are computed for models of the earth-atmosphere system.

  15. ATR evaluation through the synthesis of multiple performance measures

    NASA Astrophysics Data System (ADS)

    Bassham, Christopher B.; Klimack, William K.; Bauer, Kenneth W., Jr.

    2002-07-01

    This research demonstrates the application of decision analysis (DA) techniques to decisions made within Automatic Target Recognition (ATR) technology development. This work is accomplished to improve the means by which ATR technologies are evaluated. The first step in this research was to create a flexible decision analysis framework that could be applied to several decisions across different ATR programs evaluated by the Comprehensive ATR Scientific Evaluation (COMPASE) Center of the Air Force Research Laboratory (AFRL). For the purposes of this research, a single COMPASE Center representative provided the value, utility, and preference functions for the DA framework. The DA framework employs performance measures collected during ATR classification system (CS) testing to calculate value and utility scores. The authors gathered data from the Moving and Stationary Target Acquisition and Recognition (MSTAR) program to demonstrate how the decision framework could be used to evaluate three different ATR CSs. A decision-maker may use the resultant scores to gain insight into any of the decisions that occur throughout the lifecycle of ATR technologies. Additionally, a means of evaluating ATR CS self-assessment ability is presented. This represents a new criterion that emerged from this study, and no present evaluation metric is known.

  16. ATR phosphorylates SMARCAL1 to prevent replication fork collapse

    PubMed Central

    Couch, Frank B.; Bansbach, Carol E.; Driscoll, Robert; Luzwick, Jessica W.; Glick, Gloria G.; Btous, Rmy; Carroll, Clinton M.; Jung, Sung Yun; Qin, Jun; Cimprich, Karlene A.; Cortez, David

    2013-01-01

    The DNA damage response kinase ataxia telangiectasia and Rad3-related (ATR) coordinates much of the cellular response to replication stress. The exact mechanisms by which ATR regulates DNA synthesis in conditions of replication stress are largely unknown, but this activity is critical for the viability and proliferation of cancer cells, making ATR a potential therapeutic target. Here we use selective ATR inhibitors to demonstrate that acute inhibition of ATR kinase activity yields rapid cell lethality, disrupts the timing of replication initiation, slows replication elongation, and induces fork collapse. We define the mechanism of this fork collapse, which includes SLX4-dependent cleavage yielding double-strand breaks and CtIP-dependent resection generating excess single-stranded template and nascent DNA strands. Our data suggest that the DNA substrates of these nucleases are generated at least in part by the SMARCAL1 DNA translocase. Properly regulated SMARCAL1 promotes stalled fork repair and restart; however, unregulated SMARCAL1 contributes to fork collapse when ATR is inactivated in both mammalian and Xenopus systems. ATR phosphorylates SMARCAL1 on S652, thereby limiting its fork regression activities and preventing aberrant fork processing. Thus, phosphorylation of SMARCAL1 is one mechanism by which ATR prevents fork collapse, promotes the completion of DNA replication, and maintains genome integrity. PMID:23873943

  17. Quantitative determination of two polymorphic forms of imatinib mesylate in a drug substance and tablet formulation by X-ray powder diffraction, differential scanning calorimetry and attenuated total reflectance Fourier transform infrared spectroscopy.

    PubMed

    Bellur Atici, Esen; Karlığa, Bekir

    2015-10-10

    Imatinib has been identified as a tyrosine kinase inhibitor that selectively inhibits the Abl tyrosine kinases, including Bcr-Abl. The active substance used in drug product is the mesylate salt form of imatinib, a phenylaminopyrimidine derivative and chemically named as N-(3-(4-(pyridin-3-yl) pyrimidin-2-ylamino)-4-methylphenyl)-4-((4-methylpiperazin-1-yl) methyl)-benzamide methanesulfonic acid salt. It exhibits many polymorphic forms and most stable and commercialized polymorphs are known as α and β forms. Molecules in α and β polymorphic forms exhibit significant conformational differences due to their different intra- and intermolecular interactions, which stabilize their molecular conformations and affect their physicochemical properties such as bulk density, melting point, solubility, stability, and processability. The manufacturing process of a drug tablet included granulation, compression, coating, and drying may cause polymorphic conversions. Therefore, polymorphic content of the drug substance should be controlled during quality control and stability testing. Attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectroscopy, differential scanning calorimetry (DSC), and powder X-ray diffraction (PXRD) methods were evaluated for determination of the polymorphic content of the drug substance and drug product; and PXRD was the most accurate technique and selected as preferred method and validated. Prior to development of a quantification method, pure α and β polymorphs were characterized and used throughout the method development and validation studies. Mixtures with different ratios of α and β forms were scanned using X-ray diffractometer with a scan rate of 0.250°/min over an angular range of 19.5-21.0° 2θ and the peak heights for characteristic peak of β form at 20.5 ± 0.2° 2θ diffraction angle were used to generate a calibration curve. The detection limit of β polymorph in α form imatinib mesylate tablets was found as 4% and the linear regression analysis data for the calibration plots showed good linear relationship with correlation coefficient of 0.992 with respect to relative peak height in the concentration range of 12-75 wt% β form containing tablet mixtures. The obtained results at each stage of the validation study proved that the method is specific, repeatable, precise and accurate, and could be used for determination of β polymorph content in tablets produced by using α polymorph of imatinib mesylate. The developed PXRD quantification method was used to monitor the polymorphic purity of α form drug substance and corresponding drug products during the quality control analyses and stability studies, and the results indicated that α form was stable and not converted to β form during the manufacturing process and stability period. PMID:26099262

  18. ATR-FTIR Spectroscopic Evidence for Biomolecular Phosphorus and Carboxyl Groups Facilitating Bacterial Adhesion to Iron Oxides

    PubMed Central

    Parikh, Sanjai J.; Mukome, Fungai N.D.; Zhang, Xiaoming

    2014-01-01

    Attenuated total reflectance (ATR) Fourier transform infrared (FTIR) spectroscopy has been used to probe the binding of bacteria to hematite (α-Fe2O3) and goethite (α-FeOOH). In situ ATR-FTIR experiments with bacteria (Pseudomonas putida, P. aeruginosa, Escherichia coli), mixed amino acids, polypeptide extracts, deoxyribonucleic acid (DNA), and a suite of model compounds were conducted. These compounds represent carboxyl, catecholate, amide, and phosphate groups present in siderophores, amino acids, polysaccharides, phospholipids, and DNA. Due in part to the ubiquitous presence of carboxyl groups in biomolecules, numerous IR peaks corresponding to outer-sphere or unbound (1400 cm−1) and inner-sphere (1310-1320 cm−1) coordinated carboxyl groups are noted following reaction of bacteria and biomolecules with α-Fe2O3 and α-FeOOH. However, the data also reveal that the presence of low-level amounts (i.e., 0.45-0.79%) of biomolecular phosphorous groups result in strong IR bands at ~1043 cm−1, corresponding to inner-sphere Fe-O-P bonds, underscoring the importance of bacteria associated P-containing groups in biomolecule and cell adhesion. Spectral comparisons also reveal slightly greater P-O-Fe contributions for bacteria (Pseudomonad, E. coli) deposited on α-FeOOH, as compared to α-Fe2O3. This data demonstrates that slight differences in bacterial adhesion to Fe oxides can be attributed to bacterial species and Fe-oxide minerals. However, more importantly, the strong binding affinity of phosphate in all bacteria samples to both Fe-oxides results in the formation of inner-sphere Fe-O-P bonds, signifying the critical role of biomolecular P in the initiation of bacterial adhesion. PMID:24859052

  19. Characterization of attenuated total reflection infrared spectral intensity variations of immature and mature cotton fibers by two-dimensional correlation analysis

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Two-dimensional (2D) correlation analysis was applied to characterize the ATR spectral intensity fluctuations of immature and mature cotton fibers. Prior to 2D analysis, the spectra were leveled to zero at the peak intensity of 1800 cm-1 and then were normalized at the peak intensity of 660 cm-1 to ...

  20. Molecular cloning of AtRS4, a seed specific multifunctional RFO synthase/galactosylhydrolase in Arabidopsis thaliana

    PubMed Central

    Gangl, Roman; Behmüller, Robert; Tenhaken, Raimund

    2015-01-01

    Stachyose is among the raffinose family oligosaccharides (RFOs) one of the major water-soluble carbohydrates next to sucrose in seeds of a number of plant species. Especially in leguminous seeds, e.g. chickpea, stachyose is reported as the major component. In contrast to their ambiguous potential as essential source of carbon for germination, RFOs are indigestible for humans and can contribute to diverse abdominal disorders. In the genome of Arabidopsis thaliana, six putative raffinose synthase genes are reported, whereas little is known about these putative raffinose synthases and their biochemical characteristics or their contribution to the RFO physiology in A. thaliana. In this paper, we report on the molecular cloning, functional expression in Escherichia coli and purification of recombinant AtRS4 from A. thaliana and the biochemical characterisation of the putative stachyose synthase (AtSTS, At4g01970) as a raffinose and high affinity stachyose synthase (Km for raffinose 259.2 ± 21.15 μM) as well as stachyose and galactinol specific galactosylhydrolase. A T-DNA insertional mutant in the AtRS4 gene was isolated. Only semi-quantitative PCR from WT siliques showed a specific transcriptional AtRS4 PCR product. Metabolite measurements in seeds of ΔAtRS4 mutant plants revealed a total loss of stachyose in ΔAtRS4 mutant seeds. We conclude that AtRS4 is the only stachyose synthase in the genome of A. thaliana that AtRS4 represents a key regulation mechanism in the RFO physiology of A. thaliana due to its multifunctional enzyme activity and that AtRS4 is possibly the second seed specific raffinose synthase beside AtRS5, which is responsible for Raf accumulation under abiotic stress. PMID:26483807

  1. ATR for 3D medical imaging

    NASA Astrophysics Data System (ADS)

    Jannson, Tomasz; Kostrzewski, Andrew; Paki Amouzou, P.

    2007-09-01

    This paper presents a novel concept of Automatic Target Recognition (ATR) for 3D medical imaging. Such 3D imaging can be obtained from X-ray Computerized Tomography (CT), Magnetic Resonance Imaging (MRI), Positron Emission Tomography (PET), Ultrasonography (USG), functional MRI, and others. In the case of CT, such 3D imaging can be derived from 3D-mapping of X-ray linear attenuation coefficients, related to 3D Fourier transform of Radon transform, starting from frame segmentation (or contour definition) into an object and background. Then, 3D template matching is provided, based on inertial tensor invariants, adopted from rigid body mechanics, by comparing the mammographic data base with a real object of interest, such as a malignant breast tumor. The method is more general than CAD breast mammography.

  2. ATR FTIR Mapping of Leather Fiber Panels

    NASA Astrophysics Data System (ADS)

    Tondi, G.; Grünewald, T.; Petutschnigg, A.; Schnabel, T.

    2015-01-01

    Leather fiber panels are very promising materials for many applications, not only for the easy availability of the constituents but also for their outstanding fi re-retardant properties. These innovative composite panels can be an excellent material for building insulation, and in recent times, the interest of industries in this composite board has considerably arisen. For this reason the discrimination of the components in the leather fiber panels is becoming fundamental in order to ensure their homogeneous properties. A method to characterize the surface of these materials is then required. An ATR FTIR mapping system for the leather fiber panels has been performed with a Perkin-Elmer microscope coupled with a Frontier FTIR spectrometer. The system has successfully allowed transforming the optical image to a chemical one. This technique can be considered as a right tool for routine controls of the surface quality, especially when the leather shavings cannot be optically distinguished.

  3. Association Mapping of Total Carotenoids in Diverse Soybean Genotypes Based on Leaf Extracts and High-Throughput Canopy Spectral Reflectance Measurements

    PubMed Central

    Dhanapal, Arun Prabhu; Ray, Jeffery D.; Singh, Shardendu K.; Hoyos-Villegas, Valerio; Smith, James R.; Purcell, Larry C.; King, C. Andy; Fritschi, Felix B.

    2015-01-01

    Carotenoids are organic pigments that are produced predominantly by photosynthetic organisms and provide antioxidant activity to a wide variety of plants, animals, bacteria, and fungi. The carotenoid biosynthetic pathway is highly conserved in plants and occurs mostly in chromoplasts and chloroplasts. Leaf carotenoids play important photoprotective roles and targeted selection for leaf carotenoids may offer avenues to improve abiotic stress tolerance. A collection of 332 soybean [Glycine max (L.) Merr.] genotypes was grown in two years and total leaf carotenoid content was determined using three different methods. The first method was based on extraction and spectrophotometric determination of carotenoid content (eCaro) in leaf tissue, whereas the other two methods were derived from high-throughput canopy spectral reflectance measurements using wavelet transformed reflectance spectra (tCaro) and a spectral reflectance index (iCaro). An association mapping approach was employed using 31,253 single nucleotide polymorphisms (SNPs) to identify SNPs associated with total carotenoid content using a mixed linear model based on data from two growing seasons. A total of 28 SNPs showed a significant association with total carotenoid content in at least one of the three approaches. These 28 SNPs likely tagged 14 putative loci for carotenoid content. Six putative loci were identified using eCaro, five loci with tCaro, and nine loci with iCaro. Three of these putative loci were detected by all three carotenoid determination methods. All but four putative loci were located near a known carotenoid-related gene. These results showed that carotenoid markers can be identified in soybean using extract-based as well as by high-throughput canopy spectral reflectance-based approaches, demonstrating the utility of field-based canopy spectral reflectance phenotypes for association mapping. PMID:26368323

  4. Investigation of the effect of atmospheric dust on the determination of total ozone from the earth's ultraviolet reflectivity measurements, 1

    NASA Technical Reports Server (NTRS)

    Dave, J. V.

    1976-01-01

    Two computer algorithms are described. These algorithms were used for computing the aximuth-independent component of the intensity of the monochromatic radiation emerging at the top of a pseudo-spherical atmosphere with arbitrary vertical distribution of ozone, and with any arbitrary height distribution of up to two different kinds of aerosol. This atmospheric model was assumed to rest on a surface obeying Lambert's law of reflection.

  5. Impulsive solar X-ray bursts. III - Polarization, directivity, and spectrum of the reflected and total bremsstrahlung radiation from a beam of electrons directed toward the photosphere

    NASA Technical Reports Server (NTRS)

    Langer, S. H.; Petrosian, V.

    1977-01-01

    The paper presents the spectrum, directivity, and state of polarization of the bremsstrahlung radiation expected from a beam of high-energy electrons spiraling along radial magnetic field lines toward the photosphere. A Monte Carlo method is then described for evaluation of the spectrum, directivity, and polarization of X-rays diffusely reflected from stellar photospheres. The accuracy of the technique is evaluated through comparison with analytic results. The calculated characteristics of the incident X-rays are used to evaluate the spectrum, directivity, and polarization of the reflected and total X-ray fluxes. The results are compared with observations.

  6. ATR-FTIR spectroscopy reveals polycyclic aromatic hydrocarbon contamination despite relatively pristine site characteristics: Results of a field study in the Niger Delta.

    PubMed

    Obinaju, Blessing E; Martin, Francis L

    2016-01-01

    Fourier-transform infrared (FTIR) spectroscopy is an emerging technique to detect biochemical alterations in biological tissues, particularly changes due to sub-lethal exposures to environmental contaminants. We have previously shown the potential of attenuated total reflection FTIR (ATR-FTIR) spectroscopy to detect real-time exposure to contaminants in sentinel organisms as well as the potential to relate spectral alterations to the presence of specific environmental agents. In this study based in the Niger Delta (Nigeria), changes occurring in fish tissues as a result of polycyclic aromatic hydrocarbon (PAH) exposure at contaminated sites are compared to the infrared (IR) spectra of the tissues obtained from a relatively pristine site. Multivariate analysis revealed that PAH contamination could be occurring at the pristine site, based on the IR spectra and significant (P<0.0001) differences between sites. The study provides evidence of the IR spectroscopy techniques' sensitivity and supports their potential application in environmental biomonitoring. PMID:26826366

  7. FTIR-ATR study of the influence of the pyrimidine analog of fluphenazine on the chain-melting phase transition of sphingomyelin membranes

    NASA Astrophysics Data System (ADS)

    Kuć, Marta; Cieślik-Boczula, Katarzyna; Świątek, Piotr; Jaszczyszyn, Agata; Gąsiorowski, Kazimierz; Malinka, Wiesław

    2015-09-01

    The membrane perturbing potency of the highly effective anti-multidrug resistance (MDR) pyrimidine analog of fluphenazine (FPh-prm), has been studied using attenuated total reflectance Fourier-transfer infrared spectroscopy (FTIR-ATR). The temperature- and FPh-prm-dose-dependent evolutions of the infrared spectra of FPh-prm/sphingomyelin (SM) mixtures were analyzed using principal component analysis (PCA). It has been postulated that the distinct anti-MDR activity of FPh-prm could be related to its ability to affect the modification of SM membranes. A reduction in the temperature of the chain-melting phase transition was observed in FPh-prm-mixed SM membranes together with the loosing of the phase transition cooperativity. Increasing the temperature led to the trans to gauche isomerization of FPh-prm-rich lipid membranes, which resulted in the gradual release of FPh-prm from the lipid membrane to the water phase.

  8. ATR inhibition rewires cellular signaling networks induced by replication stress.

    PubMed

    Wagner, Sebastian A; Oehler, Hannah; Voigt, Andrea; Dalic, Denis; Freiwald, Anja; Serve, Hubert; Beli, Petra

    2016-02-01

    The slowing down or stalling of replication forks is commonly known as replication stress and arises from multiple causes such as DNA lesions, nucleotide depletion, RNA-DNA hybrids, and oncogene activation. The ataxia telangiectasia and Rad3-related kinase (ATR) plays an essential role in the cellular response to replication stress and inhibition of ATR has emerged as therapeutic strategy for the treatment of cancers that exhibit high levels of replication stress. However, the cellular signaling induced by replication stress and the substrate spectrum of ATR has not been systematically investigated. In this study, we employed quantitative MS-based proteomics to define the cellular signaling after nucleotide depletion-induced replication stress and replication fork collapse following ATR inhibition. We demonstrate that replication stress results in increased phosphorylation of a subset of proteins, many of which are involved in RNA splicing and transcription and have previously not been associated with the cellular replication stress response. Furthermore, our data reveal the ATR-dependent phosphorylation following replication stress and discover novel putative ATR target sites on MCM6, TOPBP1, RAD51AP1, and PSMD4. We establish that ATR inhibition rewires cellular signaling networks induced by replication stress and leads to the activation of the ATM-driven double-strand break repair signaling. PMID:26572502

  9. [Osteosarcoma and ATR-16 syndrome: association or coincidence?].

    PubMed

    Regueiro Garca, A; Saborido Fiao, R; Gonzlez Calvete, L; Vzquez Donsin, M; Couselo Snchez, J M; Fernndez Sanmartn, M

    2015-01-01

    ATR-16 syndrome is due to alterations on chromosome 16p13.3, and is usually accompanied by alpha-thalassemia, mild-moderate mental retardation, dysmorphic facial features, skeletal and genitourinary malformations. There are no references of the combination of ATR-16 syndrome and osteosarcoma in the literature. Osteosarcoma usually has a complex karyotype, characterized by a high degree of heterogeneity of chromosomal aberrations, among which is the involvement of chromosome 16. We report a case of a patient with ATR-16 syndrome diagnosed with femoral osteosarcoma. PMID:24631100

  10. Direct analysis of blood serum by total reflection X-ray fluorescence spectrometry and application of an artificial neural network approach for cancer diagnosis*1

    NASA Astrophysics Data System (ADS)

    Hernández-Caraballo, Edwin A.; Marcó-Parra, Lué M.

    2003-12-01

    Iron, copper, zinc and selenium were determined directly in serum samples from healthy individuals ( n=33) and cancer patients ( n=27) by total reflection X-ray fluorescence spectrometry using the Compton peak as internal standard [L.M. Marcó P. et al., Spectrochim. Acta Part B 54 (1999) 1469-1480]. The standardized concentrations of these elements were used as input data for two-layer artificial neural networks trained with the generalized delta rule in order to classify such individuals according to their health status. Various artificial neural networks, comprising a linear function in the input layer, a hyperbolic tangent function in the hidden layer and a sigmoid function in the output layer, were evaluated for such a purpose. Of the networks studied, the (4:4:1) gave the highest estimation (98%) and prediction rates (94%). The latter demonstrates the potential of the total reflection X-ray fluorescence spectrometry/artificial neural network approach in clinical chemistry.

  11. Attenuated total reflection-Fourier transform infrared spectroscopy as a possible method to investigate biophysical parameters of stratum corneum in vivo.

    PubMed

    Brancaleon, L; Bamberg, M P; Sakamaki, T; Kollias, N

    2001-03-01

    We investigated the use of attenuated total reflection-Fourier transform infrared spectroscopy as a method to study differences in the molecular components of human stratum corneum in vivo. These variations as a function of the anatomic site and of the depth into its layered structure are important to understand the biology and physiology of the tissue. In this preliminary study we have investigated spectroscopic changes in 18 healthy individuals. Total reflection-Fourier transform infrared spectroscopy represents a potentially powerful tool to study biophysical properties of surfaces. We observed that, in vivo, biophysical parameters of the stratum corneum (such as hydration, lipid composition, and conformation of the aliphatic chains) are indeed dependent on the anatomic site. As in total reflection-Fourier transform infrared spectroscopy experiments the penetration depth of the evanescent field into the stratum corneum is comparable with the thickness of a layer of corneocytes, this technique can be used to follow the distribution of lipids, water, and proteins as a function of depth into the tissue. We found that, in vivo, these molecular components are non-uniformly distributed, in agreement with the presence of water and lipid reservoirs as observed with ex vivo ultrastructural investigations. Composition and conformational order of lipids are also a function of depth into the stratum corneum. Finally we compared the in vivo superficial hydration measured using the infrared absorption of the OH stretch of water, with the hydration measured using the Skicon hygrometer. Our results indicate that total reflection-Fourier transform infrared spectroscopy might be useful to measure important chemical and biophysical parameters of stratum corneum in vivo. PMID:11231311

  12. Evidence of acid-base interactions between amines and model indoor surfaces by ATR-FTIR spectroscopy

    NASA Astrophysics Data System (ADS)

    Destaillats, Hugo; Singer, Brett C.; Gundel, Lara A.

    Molecular associations of pyridine with cellulose and gypsum, surrogates for common indoor surface materials, were studied using an attenuated total reflection (ATR)-Fourier transform infrared (FTIR) spectrophotometric method. The purpose of this study was to gain insight into the molecular interactions of amines with well-characterized materials that affect their partitioning between indoor air and surfaces. The experimental results suggest the presence of at least two sorptive states for volatile and semivolatile amines, attributed to the chemisorbed species and to a more labile surface state (i.e., physisorbed pyridine). Both exhibited spectroscopic signatures corresponding to aromatic C-H stretching modes (2950-3100 cm -1) in the studied spectral region. Chemisorbed pyridine could be identified by the presence of additional IR signals in the N-H and O-H stretching region of the spectrum (2900-3600 cm -1). During desorption under a stream of N 2, surface enrichment in the chemisorbed species was evidenced by a slower reduction of the absorbance of the broad band at 2900-3600 cm -1 in relation to the total pyridine absorbance change. This spectroscopic evidence for acid-base interactions between amines and surfaces is consistent with the desorption behavior observed in previous work for nicotine from model surfaces.

  13. Investigation of the effect of atmospheric dust on the determination of total ozone from the earth's ultraviolet reflectivity measurements

    NASA Technical Reports Server (NTRS)

    Dave, J. V.

    1977-01-01

    Results are presented on the effect of atmospheric aerosols on the value of total ozone, in an atmospheric column of the terrestrial atmosphere, estimated from the simulated measurements of the ultraviolet radiation back scattered by the earth atmosphere models. Simulated measurements were used in five (configuration of the BUV experiment of Nimbus-4 satellite), and in six (configuration of the TOMS section of the SBUV/TOMS experiment on Nimbus-G) narrow spectral regions in the ultraviolet part of the spectrum.

  14. LWRS ATR Irradiation Testing Readiness Status

    SciTech Connect

    Kristine Barrett

    2012-09-01

    The Light Water Reactor Sustainability (LWRS) Program was established by the U.S. Department of Energy Office of Nuclear Energy (DOE-NE) to develop technologies and other solutions that can improve the reliability, sustain the safety, and extend the life of the current reactors. The LWRS Program is divided into four R&D Pathways: (1) Materials Aging and Degradation; (2) Advanced Light Water Reactor Nuclear Fuels; (3) Advanced Instrumentation, Information and Control Systems; and (4) Risk-Informed Safety Margin Characterization. This report describes an irradiation testing readiness analysis in preparation of LWRS experiments for irradiation testing at the Idaho National Laboratory (INL) Advanced Test Reactor (ATR) under Pathway (2). The focus of the Advanced LWR Nuclear Fuels Pathway is to improve the scientific knowledge basis for understanding and predicting fundamental performance of advanced nuclear fuel and cladding in nuclear power plants during both nominal and off-nominal conditions. This information will be applied in the design and development of high-performance, high burn-up fuels with improved safety, cladding integrity, and improved nuclear fuel cycle economics

  15. ATR National Scientific User Facility 2009 Annual Report

    SciTech Connect

    Todd R. Allen; Mitchell K. Meyer; Frances Marshall; Mary Catherine Thelen; Jeff Benson

    2010-11-01

    This report describes activities of the ATR NSUF from FY-2008 through FY-2009 and includes information on partner facilities, calls for proposals, users week and education programs. The report also contains project information on university research projects that were awarded by ATR NSUF in the fiscal years 2008 & 2009. This research is university-proposed researcher under a user facility agreement. All intellectual property from these experiments belongs to the university per the user agreement.

  16. Total reflection X-ray fluorescence spectrometric determination of elements in water hyacinth from the Lerma River

    NASA Astrophysics Data System (ADS)

    Tejeda, S.; Zarazúa, G.; Ávila-Pérez, P.; Carapia-Morales, L.; Martínez, T.

    2010-06-01

    The Lerma River is one of the most polluted body water in Mexico. For this reason, only the highly resistant organisms such as water hyacinth are able to reproduce in this river. The aim of this work was to evaluate the concentration of K, S, Fe, Ca, Mn, Ti, Zn, Sr, Rb, Cu, Cr, Ni, Pb and Br in roots of water hyacinth ( Eichhornia crassipes) from the Lerma River. The samples were collected from five sites in the river and analyzed in triplicate using a TXRF Spectrometer 'TX-2000 Ital Structures' with a Si(Li) detector and a resolution of 140 eV (FWHM) at Mn Kα. A Mo tube (40 kV, 30 mA) with 17.4 KeV excitation energy was used for a counting time of 500 s. Results show that the average metal concentration in the water hyacinth roots decrease in the following order: K (9698.2 µg/g) > S (7593.3 µg/g) > Fe (4406.6 µg/g) > Ca (2601.8 µg/g) > Mn (604.2 µg/g) > Ti (230.7 µg/g) > Zn (51.65 µg/g) > Sr (43.55 µg/g) > Rb (18.61 µg/g) > Cu (12.78 µg/g) > Cr (6.45 µg/g) > Ni (4.68 µg/g) > Pb (4.32 µg/g) > Br (4.31 µg/g) and the bioconcentration factors in the water hyacinth decrease in the sequence: Ti > Fe > Mn > Cu > Ni > Zn > S > Pb > Rb > K > Cr > Sr > Br > Ca. The concentrations in roots of water hyacinth reflect the high pollution level of the river.

  17. Estimation of direct, diffuse, and total FPARs from Landsat surface reflectance data and ground-based estimates over six FLUXNET sites

    NASA Astrophysics Data System (ADS)

    Li, Wenjuan; Fang, Hongliang

    2015-04-01

    The fraction of photosynthetically active radiation (PAR) absorbed by green elements (FPAR) is an essential climate variable (ECV) in quantifying canopy absorbed PAR (APAR) and gross and net primary production. It has been demonstrated that FPAR is larger under totally diffuse than clear sky conditions because all canopy parts can absorb lights effectively under diffuse conditions. The direct and diffuse FPARs are defined, therefore, as the FPAR values obtained under clear (most sunny) and overcast (most cloudy) conditions, respectively, and FPAR represents the summed canopy absorption efficiency for both direct and diffuse PAR. Satellite FPAR products, such as MODIS, GEOV1, MERIS, and JRC-TIP, have been generated at different temporal and spatial resolutions. Except for JRC-TIP which generates direct and diffuse FPARs separately, all the other products typically correspond to the instantaneous black-sky FPAR under direct illumination only. However, even under fully clear sky conditions, the proportion of diffuse PAR over the surface cannot be ignored. Otherwise, FPAR will be underestimated, especially for small leaf area index (LAI) region. To address this, the present study developed a new approach to estimate direct, diffuse, and total FPARs, separately, from Landsat 30m surface reflectance data. Field-measured direct and diffuse FPARs were first derived for crops, deciduous broadleaf forests, and evergreen needleleaf forests at six FLUXNET sites. Then, a coupled soil-leaf-canopy (SLC) radiative transfer model was used to simulate surface reflectance under direct and diffuse illumination conditions, respectively. Direct, diffuse, and total FPARs were estimated by comparing Landsat-5 Thematic Mapper (TM) data and simulated surface reflectances using a lookup table approach. The differences between the Landsat-estimated and the field-measured FPARs are less than 0.05 (10%). The diffuse FPAR is higher than the direct FPAR by up to 19.38%, whereas the total FPAR is larger than the direct FPAR by up to 16.07%. The direct APAR is higher than the diffuse APAR under clear-sky conditions, but underestimates the total APAR by -277.72 μmol s-1 m-2 on average. We recommend that the total FPAR should be generated from current satellite sensors, and the differences in FPAR definitions should be considered in the estimation of APAR in vegetation models. More frequent field measurements are necessary to improve the accuracy of ground FPAR measurements and to validate instantaneous satellite products. The approach described here can be extended to estimate direct, diffuse, and total FPARs from other satellite data, and the obtained FPAR variables could be helpful to improve modeling of vegetation processes.

  18. Study on the refractive index matching effect of ultrasound on optical clearing of bio-tissues based on the derivative total reflection method.

    PubMed

    Zeng, Huanhuan; Wang, Jin; Ye, Qing; Deng, Zhichao; Mei, Jianchun; Zhou, Wenyuan; Zhang, Chunping; Tian, Jianguo

    2014-10-01

    In recent years, the tissue optical clearing (OC) technique in the biomedicine field has drawn lots of attention. Various physical and chemical methods have been introduced to improve the efficacy of OC. In this study, the effect of the combination of glycerol and ultrasound treatment on OC of in vitro porcine muscle tissues has been investigated. The refractive index (RI) matching mechanism of OC was directly observed based on the derivative total reflection method. A theoretical model was used to simulate the proportion of tissue fluid in the illuminated area. Moreover, the total transmittance spectra have been obtained by a spectrometer over the range from 450 nm to 700 nm. The administration of glycerol and ultrasound has led to an increase of the RI of background medium and a more RI matching environment was achieved. The experimental results support the validity of the ultrasound treatment for OC. The RI matching mechanism has been firstly quantitatively analyzed based on the derivative total reflection method. PMID:25360366

  19. Application of the total reflection X-ray fluorescence method to the elemental analysis of brain tumors of different types and grades of malignancy

    NASA Astrophysics Data System (ADS)

    Lankosz, M. W.; Grzelak, M.; Ostachowicz, B.; Wandzilak, A.; Szczerbowska-Boruchowska, M.; Wrobel, P.; Radwanska, E.; Adamek, D.

    2014-11-01

    The process of carcinogenesis may influence normal biochemical reactions leading to alterations in the elemental composition of the tissue. Total reflection X-ray fluorescence analysis (TXRF) was applied to the elemental analysis of different brain tumors. The following elements were present in all the neoplastic tissues analyzed: K, Ca, Fe, Cu, Zn and Rb. The results of the analysis showed that the elemental composition of a relatively small fragment of tissue represents satisfactorily the biochemical “signature” of a cancer. On the basis of the element concentrations determined, it was possible to differentiate between some types of brain tumors.

  20. Determination of ultra trace contaminants on silicon wafer surfaces using total-reflection X-ray fluorescence TXRF 'state-of-the-art'

    NASA Astrophysics Data System (ADS)

    Pahlke, S.; Fabry, L.; Kotz, L.; Mantler, C.; Ehmann, T.

    2001-11-01

    In a well balanced system of highly motivated, well trained personnel and automated equipment, pure reagents and bulk media, cleanrooms and integrated data management, total-reflection X-ray fluorescence (TXRF) can and must contribute to quality assurance and process stability, support and canalize creative engineering by continuous learning about materials and processes. TXRF has the advantage of controlled one-point calibration, a linear dynamic range of three orders of magnitude, high grade of automation in operation and data management, high up-time, and a simple control of data plausibility.

  1. Direct real-time observation of actin filament branching mediated by Arp2/3 complex using total internal reflection fluorescence microscopy

    PubMed Central

    Amann, Kurt J.; Pollard, Thomas D.

    2001-01-01

    Existing methods for studying actin filament dynamics have allowed analysis only of bulk samples or individual filaments after treatment with the drug phalloidin, which perturbs filament dynamics. Total internal reflection fluorescence microscopy with rhodamine-labeled actin allowed us to observe polymerization in real time, without phalloidin. Direct measurements of filament growth confirmed the rate constants measured by electron microscopy and established that rhodamine actin is a kinetically inactive tracer for imaging. In the presence of activated Arp2/3 complex, growing actin filaments form branches at random sites along their sides, rather than preferentially from their barbed ends. PMID:11742068

  2. Multielement determination in sediments, pore water and river water of Upper Austrian rivers by total-reflection X-ray fluorescence

    NASA Astrophysics Data System (ADS)

    Miesbauer, Hermann

    1997-07-01

    Multielement determination in sediments, pore water and river water has been carried out using total-reflection X-ray fluorescence (TXRF), electrothermal atomic absorption spectrometry (ETAAS) and hydride generation atomic absorption spectrometry (Hyd-AAS). TXRF in particular facilitates multielement determination by allowing easy quantification with internal one-element standardization, and is therefore central to these investigations. In connection with the simplicity of sample preparation an attractive analytical procedure for routine analyses has been worked out. It allows a quick and accurate multielement determination on the <40 μm fraction of river sediment and on pore water and river water.

  3. Achromatic angle-insensitive infrared quarter-wave retarder based on total internal reflection at the Si-SiO2 interface.

    PubMed

    Azzam, R M A; Spinu, Cristina L

    2004-10-01

    An achromatic infrared (lambda = 1.2-4 microm), Si-prism quarter-wave retarder (QWR) is described that uses total internal reflection at a buried Si-SiO2 interface at an angle of incidence phi near 33 degrees, where deltaDelta/deltaphi = 0. The retardance delta deviates from 90 degrees by < +/- 2 degrees within a field of view of +/- 10 degrees (in air) over the entire bandwidth. Because the SiO2 layer at the base of the prism is optically thick, this QWR is unaffected by environmental contamination. PMID:15497430

  4. Validation of ATR Fission Power Deposition Fraction in HEU and LEU Fuel Plates

    SciTech Connect

    G. S. Chang

    2008-09-01

    The Advanced Test Reactor (ATR) is a high power (250 MW), high neutron flux research reactor operating in the United States. Powered with highly enriched uranium (HEU), the ATR has a maximum unperturbed thermal neutron flux rating of 1.0 x 1015 n/cm2–s. Because of its high power and large test volumes located in high flux areas, the ATR is an ideal candidate for assessing the feasibility of converting an HEU driven reactor to a low-enriched core. A detailed plate-by-plate MCNP ATR full core model has been developed and validated for the low-enriched uranium (LEU) fuel conversion feasibility study. Using this model, an analysis has been performed to determine the LEU density and U-235 enrichment required in the fuel meat to yield equivalent K-eff versus effective full power days (EFPDs) between the HEU and LEU cores. This model has also been used to optimize U-235 content of the LEU core, minimizing the differences in K-eff and heat flux profile between the HEU and LEU cores at 115 MW total core power for 125 EFPDs. The LEU core conversion feasibility study evaluated foil type (U-10Mo) fuel with the LEU reference design of 19.7 wt% U-235 enrichment. The LEU reference design has a fixed fuel meat thickness of 0.330 mm and can sustain the same operating cycle length as the HEU fuel. Heat flux and fission power density are parameters that are proportional to the fraction of fission power deposited in fuel. Thus, the accurate determination of the fraction of fission power deposited in the fuel is important to ATR nuclear safety. In this work, a new approach was developed and validated, the Tally Fuel Cells Only (TFCO) method. This method calculates and compares the fission power deposition fraction between HEU and LEU fuel plates. Due to the high density of the U-10Mo LEU fuel, the fission ?-energy deposition fraction is 37.12%, which is larger than the HEU’s ?-energy deposition fraction of 19.7%. As a result, the fuel decay heat cooling will need to be improved. During the power operation, the total fission energy (200 MeV per fission) deposition fraction of LEU and HEU are 90.9% and 89.1%, respectively.

  5. 76 FR 47520 - Airworthiness Directives; ATR-GIE Avions de Transport Régional Model ATR42 and ATR72 Airplanes

    Federal Register 2010, 2011, 2012, 2013, 2014

    2011-08-05

    ... continued.airworthiness@atr.fr ; Internet http://www.aerochain.com . You may review copies of the referenced... section. Include ``Docket No. FAA-2011-0721; Directorate Identifier 2010-NM-217-AD'' at the beginning of..., has issued EASA Airworthiness Directive 2010-0138, dated July 1, 2010 (referred to after this as...

  6. Perfluoroalkylated Substance Effects in Xenopus laevis A6 Kidney Epithelial Cells Determined by ATR-FTIR Spectroscopy and Chemometric Analysis.

    PubMed

    Gorrochategui, Eva; Lacorte, Sílvia; Tauler, Romà; Martin, Francis L

    2016-05-16

    The effects of four perfluoroalkylated substances (PFASs), namely, perfluorobutanesulfonate (PFBS), perfluorooctanoic acid (PFOA), perfluorooctanesulfonate (PFOS), and perfluorononanoic acid (PFNA) were assessed in Xenopus laevis A6 kidney epithelial cells by attenuated total reflection Fourier-transform infrared (ATR-FTIR) spectroscopy and chemometric analysis. Principal component analysis-linear discriminant analysis (PCA-LDA) was used to visualize wavenumber-related alterations and ANOVA-simultaneous component analysis (ASCA) allowed data processing considering the underlying experimental design. Both analyses evidenced a higher impact of low-dose PFAS-treatments (10(-9) M) on A6 cells forming monolayers, while there was a larger influence of high-dose PFAS-treatments (10(-5) M) on A6 cells differentiated into dome structures. The observed dose-response PFAS-induced effects were to some extent related to their cytotoxicity: the EC50-values of most influential PFAS-treatments increased (PFOS < PFNA < PFOA ≪ PFBS), and higher-doses of these chemicals induced a larger impact. Major spectral alterations were mainly attributed to DNA/RNA, secondary protein structure, lipids, and fatty acids. Finally, PFOS and PFOA caused a decrease in A6 cell numbers compared to controls, whereas PFBS and PFNA did not significantly change cell population levels. Overall, this work highlights the ability of PFASs to alter A6 cells, whether forming monolayers or differentiated into dome structures, and the potential of PFOS and PFOA to induce cell death. PMID:27078751

  7. Perfluoroalkylated Substance Effects in Xenopus laevis A6 Kidney Epithelial Cells Determined by ATR-FTIR Spectroscopy and Chemometric Analysis

    PubMed Central

    2016-01-01

    The effects of four perfluoroalkylated substances (PFASs), namely, perfluorobutanesulfonate (PFBS), perfluorooctanoic acid (PFOA), perfluorooctanesulfonate (PFOS), and perfluorononanoic acid (PFNA) were assessed in Xenopus laevis A6 kidney epithelial cells by attenuated total reflection Fourier-transform infrared (ATR-FTIR) spectroscopy and chemometric analysis. Principal component analysis–linear discriminant analysis (PCA-LDA) was used to visualize wavenumber-related alterations and ANOVA-simultaneous component analysis (ASCA) allowed data processing considering the underlying experimental design. Both analyses evidenced a higher impact of low-dose PFAS-treatments (10–9 M) on A6 cells forming monolayers, while there was a larger influence of high-dose PFAS-treatments (10–5 M) on A6 cells differentiated into dome structures. The observed dose–response PFAS-induced effects were to some extent related to their cytotoxicity: the EC50-values of most influential PFAS-treatments increased (PFOS < PFNA < PFOA ≪ PFBS), and higher-doses of these chemicals induced a larger impact. Major spectral alterations were mainly attributed to DNA/RNA, secondary protein structure, lipids, and fatty acids. Finally, PFOS and PFOA caused a decrease in A6 cell numbers compared to controls, whereas PFBS and PFNA did not significantly change cell population levels. Overall, this work highlights the ability of PFASs to alter A6 cells, whether forming monolayers or differentiated into dome structures, and the potential of PFOS and PFOA to induce cell death. PMID:27078751

  8. Adsorption of Lysine on Na-Montmorillonite and Competition with Ca(2+): A Combined XRD and ATR-FTIR Study.

    PubMed

    Yang, Yanli; Wang, Shengrui; Liu, Jingyang; Xu, Yisheng; Zhou, Xiaoyun

    2016-05-17

    Lysine adsorption at clay/aqueous interfaces plays an important role in the mobility, bioavailability, and degradation of amino acids in the environment. Knowledge of these interfacial interactions facilitates our full understanding of the fate and transport of amino acids. Here, X-ray diffraction (XRD) and attenuated total reflectance Fourier-transform infrared spectroscopy (ATR-FTIR) measurements were used to explore the dynamic process of lysine adsorption on montmorillonite and the competition with Ca(2+) at the molecular level. Density functional theory (DFT) calculations were employed to determine the peak assignments of dissolved lysine in the solution phase. Three surface complexes, including dicationic, cationic, and zwitterionic structures, were observed to attach to the clay edge sites and penetrate the interlayer space. The increased surface coverage and Ca(2+) competition did not affect the interfacial lysine structures at a certain pH, whereas an elevated lysine concentration contributed to zwitterionic-type coordination at pH 10. Moreover, clay dissolution at pH 4 could be inhibited at a higher surface coverage with 5 and 10 mM lysine, whereas the inhibition effect was inconspicuous or undetected at pH 7 and 10. The presence of Ca(2+) not only could remove a part of the adsorbed lysine but also could facilitate the readsorption of dissolved Si(4+) and Al(3+) and surface protonation. Our results provide new insights into the process of lysine adsorption and its effects on montmorillonite surface sites. PMID:27118104

  9. FLUX SENSOR EVALUATIONS AT THE ATR CRITICAL FACILITY

    SciTech Connect

    Troy Unruh; Joy Rempe; David Nigg; George Imel; Jason Harris; Eric Bonebrake

    2010-11-01

    The Advanced Test Reactor (ATR) and the ATR Critical (ATRC) facilities lack real-time methods for detecting thermal neutron flux and fission reaction rates for irradiation capsules. Direct measurements of the actual power deposited into a test are now possible without resorting to complicated correction factors. In addition, it is possible to directly measure minor actinide fission reaction rates and to provide time-dependent monitoring of the fission reaction rate or fast/thermal flux during transient testing. A joint Idaho State University /Idaho National Laboratory ATR National Scientific User Facility (ATR NSUF) project was recently initiated to evaluate new real-time state-of-the-art in-pile flux detection sensors. Initially, the project is comparing the accuracy, response time, and long duration performance of French Atomic Energy Commission (CEA)-developed miniature fission chambers, specialized self-powered neutron detectors (SPNDs) by the Argentinean National Energy Commission (CNEA), specially developed commercial SPNDs, and back-to-back fission (BTB) chambers developed by Argonne National Laboratory (ANL). As discussed in this paper, specialized fixturing and software was developed by INL to facilitate these joint ISU/INL evaluations. Calculations were performed by ISU to assess the performance of and reduce uncertainties in flux detection sensors and compare data obtained from these sensors with existing integral methods employed at the ATRC. Ultimately, project results will be used to select the detector that can provide the best online regional ATRC power measurement. It is anticipated that project results may offer the potential to increase the ATRC’s current power limit and its ability to perform low-level irradiation experiments. In addition, results from this effort will provide insights about the viability of using these detectors in the ATR. Hence, this effort complements current activities to improve ATR software tools, computational protocols and in-core instrumentation under the ATR Modeling, Simulation and V&V Upgrade initiative, as well as the work to replace nuclear instrumentation under the ATR Life Extension Project (LEP) and provide support to the ATR NSUF.

  10. Airborne particulate matter (PM) filter analysis and modeling by total reflection X-ray fluorescence (TXRF) and X-ray standing wave (XSW).

    PubMed

    Borgese, L; Salmistraro, M; Gianoncelli, A; Zacco, A; Lucchini, R; Zimmerman, N; Pisani, L; Siviero, G; Depero, L E; Bontempi, E

    2012-01-30

    This work is presented as an improvement of a recently introduced method for airborne particulate matter (PM) filter analysis [1]. X-ray standing wave (XSW) and total reflection X-ray fluorescence (TXRF) were performed with a new dedicated laboratory instrumentation. The main advantage of performing both XSW and TXRF, is the possibility to distinguish the nature of the sample: if it is a small droplet dry residue, a thin film like or a bulk sample. Another advantage is related to the possibility to select the angle of total reflection to make TXRF measurements. Finally, the possibility to switch the X-ray source allows to measure with more accuracy lighter and heavier elements (with a change in X-ray anode, for example from Mo to Cu). The aim of the present study is to lay the theoretical foundation of the new proposed method for airborne PM filters quantitative analysis improving the accuracy and efficiency of quantification by means of an external standard. The theoretical model presented and discussed demonstrated that airborne PM filters can be considered as thin layers. A set of reference samples is prepared in laboratory and used to obtain a calibration curve. Our results demonstrate that the proposed method for quantitative analysis of air PM filters is affordable and reliable without the necessity to digest filters to obtain quantitative chemical analysis, and that the use of XSW improve the accuracy of TXRF analysis. PMID:22284465

  11. Airborne Particulate Matter (PM) filter analysis and modeling by Total reflection X-Ray Fluorescence (TXRF) and X-Ray Standing Wave (XSW)

    PubMed Central

    Borgese, L.; Salmistraro, M.; Gianoncelli, A; Zacco, A.; Lucchini, R.; Zimmerman, N.; Pisani, L.; Siviero, G.; Depero, L. E.; Bontempi, E.

    2011-01-01

    This work is presented as an improvement of a recently introduced method for airborne particulate matter (PM) filter analysis [1]. X-ray Standing Wave (XSW) and Total reflection X-Ray Fluorescence (TXRF) were performed with a new dedicated laboratory instrumentation. The main advantage of performing both XSW and TXRF, is the possibility to distinguish the nature of the sample: if it is a small droplet dry residue, a thin film like or a bulk sample; and to select the angle of total reflection to make TXRF measurements. Finally, the possibility to switch the X-ray source allows to measure with more accuracy lighter and heavier elements (with a a change in X-ray anode, for example from Mo to Cu). The aim of the present study is to lay the theoretical foundation of the new proposed method for airborne PM filters quantitative analysis improving the accuracy and efficiency of quantification by means of an external standard. The theoretical model presented and discussed demonstrated that airborne PM filters can be considered as thin layers. A set of reference samples is prepared in laboratory and used to obtain a calibration curve. Our results demonstrate that the proposed method for quantitative analysis of air PM filters is affordable and reliable without the necessity to digest filters to obtain quantitative chemical analysis, and that the use of XRW improve the accuracy of TXRF analysis. PMID:22284465

  12. Versatile microfluidic total internal reflection (TIR)-based devices: application to microbeads velocity measurement and single molecule detection with upright and inverted microscope.

    PubMed

    Le, Nam Cao Hoai; Yokokawa, Ryuji; Dao, Dzung Viet; Nguyen, Thien Duy; Wells, John C; Sugiyama, Susumu

    2009-01-21

    A poly(dimethylsiloxane) (PDMS) chip for Total Internal Reflection (TIR)-based imaging and detection has been developed using Si bulk micromachining and PDMS casting. In this paper, we report the applications of the chip on both inverted and upright fluorescent microscopes and confirm that two types of sample delivery platforms, PDMS microchannel and glass microchannel, can be easily integrated depending on the magnification of an objective lens needed to visualize a sample. Although any device configuration can be achievable, here we performed two experiments to demonstrate the versatility of the microfluidic TIR-based devices. The first experiment was velocity measurement of Nile red microbeads with nominal diameter of 500 nm in a pressure-driven flow. The time-sequenced fluorescent images of microbeads, illuminated by an evanescent field, were cross-correlated by a Particle Image Velocimetry (PIV) program to obtain near-wall velocity field of the microbeads at various flow rates from 500 nl/min to 3000 nl/min. We then evaluated the capabilities of the device for Single Molecule Detection (SMD) of fluorescently labeled DNA molecules from 30 bp to 48.5 kbp and confirm that DNA molecules as short as 1105 bp were detectable. Our versatile, integrated device could provide low-cost and fast accessibility to Total Internal Reflection Fluorescent Microscopy (TIRFM) on both conventional upright and inverted microscopes. It could also be a useful component in a Micro-Total Analysis System (micro-TAS) to analyze nanoparticles or biomolecules near-wall transport or motion. PMID:19107280

  13. ATR NATIONAL SCIENTIFIC USER FACILITY INSTRUMENTATION ENHANCEMENT EFFORTS

    SciTech Connect

    Joy L. Rempe; Mitchell K. Meyer

    2009-04-01

    A key component of the Advanced Test Reactor (ATR) National Scientific User Facility (NSUF) effort is to enhance instrumentation techniques available to users conducting irradiation tests in this unique facility. In particular, development of sensors capable of providing ‘real-time’ measurements of key irradiation parameters is emphasized because of their potential to offer increased fidelity data and reduced post-test examination costs. This paper describes the strategy for identifying new instrumentation needed for ATR irradiations and the program underway to develop and evaluate new sensors to address these needs. Accomplishments from this program are illustrated by describing several new sensors now available to users of the ATR NSUF. In addition, progress is reported on current research efforts to provide users improved in-pile instrumentation.

  14. Homeostatic regulation of meiotic DSB formation by ATM/ATR

    SciTech Connect

    Cooper, Tim J.; Wardell, Kayleigh; Garcia, Valerie; Neale, Matthew J.

    2014-11-15

    Ataxia–telangiectasia mutated (ATM) and RAD3-related (ATR) are widely known as being central players in the mitotic DNA damage response (DDR), mounting responses to DNA double-strand breaks (DSBs) and single-stranded DNA (ssDNA) respectively. The DDR signalling cascade couples cell cycle control to damage-sensing and repair processes in order to prevent untimely cell cycle progression while damage still persists [1]. Both ATM/ATR are, however, also emerging as essential factors in the process of meiosis; a specialised cell cycle programme responsible for the formation of haploid gametes via two sequential nuclear divisions. Central to achieving accurate meiotic chromosome segregation is the introduction of numerous DSBs spread across the genome by the evolutionarily conserved enzyme, Spo11. This review seeks to explore and address how cells utilise ATM/ATR pathways to regulate Spo11-DSB formation, establish DSB homeostasis and ensure meiosis is completed unperturbed.

  15. UV and genotoxic stress induce ATR relocalization in mouse spermatocytes.

    PubMed

    Di Siena, Sara; Campolo, Federica; Rossi, Pellegrino; Jannini, Emmanuele A; Dolci, Susanna; Pellegrini, Manuela

    2013-01-01

    During meiosis, phosphorylation of H2AX is one of the earliest cellular responses to the generation of DNA double-strand breaks (DSBs) by the SPO11 topoisomerase. ATM is the kinase which mediates the formation of phosphorylated H2AX (H2AX) meiotic foci, while ATR is the kinase which signals chromosome asynapsis at the level of the XY bivalent. To investigate the possible role of ATR also in DNA damage signalling in meiotic cells, we studied the effect of UV radiation and chemotherapy drugs on H2AX phosphorylation and ATR relocalization in mouse pachytene spermatocytes. Here, we report that UV, a single strand break DNA-damaging agent, induces ATR relocalization from the XY sex body to nuclear foci and intense H2AX phosphorylation. Other DNA damage proteins such as MDC1, NBS1 and 53BP1 showed a similar relocalization following UVA microirradiation of spermatocytes. We found that DNA damage induced by UV increased the intensity and the number of H2AX foci also in Atm null spermatocytes. Inhibition of RNA synthesis was found to induce the formation of H2AX foci, but it did not influence the DNA damage response to UV irradiation. Finally, exposure of spermatocytes to double strand break DNA-damaging agents such as cisplatin, bleomycin or etoposide also induced ATR relocalization and intense H2AX phosphorylation and led to anomalies in synaptonemal assembly. Our results demonstrate that DNA damage induced by genotoxic stress can activate ATR and influence meiotic chromatin remodelling through H2AX phosphorylation, likely as part of a response which normally ensures germ cell genomic integrity. PMID:23784839

  16. A dual beam total internal reflection fluorescence spectrometer for dynamic depth resolved measurements of biochemical liquid-solid interface binding reactions in opaque solvents

    NASA Astrophysics Data System (ADS)

    Liebmann, Lars W.; Robinson, John A.; Mann, Kenneth G.

    1991-09-01

    The initiation of many physiologically important biochemical reactions is dependent on the binding of a molecule or molecules from solution to an appropriate solid surface such as a cell membrane. The quantitative study of dynamic interactions of molecules in solution with immobilized surfaces under physiologically relevant conditions presents a significant physical problem. Traditionally these measurements have been performed by discontinuous, nonequilibrium assays that cannot accurately model in vivo reaction mechanisms. Total internal reflection fluorescence spectroscopy (TIRFS) is an analytical technique that is based on the excitation of fluorescence by means of an exponentially decaying surface energy wave called the evanescent wave. The limited ``penetration depth'' of the evanescent wave leads to excitation of fluorescent molecules at or near the surface. This phenomena makes TIRFS uniquely qualified for the dynamic fluorescence study of liquid-solid interface binding reactions. The instrument described here permits the powerful technique of TIRFS to be used by biomedical researchers in their investigation of biochemical interface reactions. The fully automated, menu driven instrument allows the real time dynamic measurement of binding of fluorescent-labeled molecules in solution at physiologically relevant concentrations to appropriate immobilized surfaces. The novel design of the total internal reflection element enables the study of binding from essentially opaque and highly scattering solutions such as whole blood. Measurements may be performed under static, stirred, or flow conditions. The presently described TIRFS instrument is capable of tracking a binding reaction with evanescent fields established by two identical reflecting light beams with different reflection angles. This instrumental feature allows the dynamic measurement not only of the primary binding event but also of fluctuations in the distance between the optical interface and the point of signal generation. Data from experiments involving fluorescently labeled molecules binding to cell monolayers as well as binding experiments performed in whole blood are shown to verify the instrument performance. Due to its extraordinary capabilities and its user friendly design, the developed TIRFS instrument opens up a large number of relevant but previously unmeasurable experimental systems for investigation.

  17. Analyzing effects of range resolution on MSC HRR ATR performance

    NASA Astrophysics Data System (ADS)

    McWhorter, Todd; Gross, David C.; Hawley, Robert W.; Welsh, Byron M.

    2000-08-01

    This paper is an initial exploration into the effects of range resolution on Automatic Target Recognition (ATR) algorithms based on High Range Resolution (HRR) signatures. The theoretical performance of a two-class, forced-decision classifier is used to quantify the effects of radar resolution on ATR performance. The classifier employed in this study is a forced-decision instantiation of the matched subspace classifier (MSC) developed under the DARPA TRUMPETS program. The paper also examines effects of range resolution on the separability of individual HRR profiles. This work is supported by DARPA/SPO under the MSTAR Enhancements (HBTI) program and in cooperation with AFRL/SNAA.

  18. ATR spectra on boundary with mixture containing organic substances

    NASA Astrophysics Data System (ADS)

    Schelokov, R. V.; Yatsishen, V. V.

    2005-02-01

    The problem of not destroying diagnostics and dosing of radiation at laser therapy is one of important in medicine. Therefore the purpose of our work is development of method ATR for diagnostics and researches in biomedicine. In this work as objects of consideration were: a mixture of nicotine with water, a mixture of an ascorbic acid with water and surface lesions of an eye cornea by a herpes virus. Results of our consideration are the ATR spectra defined at different concentration of organic substances and virions.

  19. Investigation of aged Asian dust particles by the combined use of quantitative ED-EPMA and ATR-FTIR imaging

    NASA Astrophysics Data System (ADS)

    Song, Y.-C.; Eom, H.-J.; Jung, H.-J.; Malek, M. A.; Kim, H. K.; Geng, H.; Ro, C.-U.

    2013-03-01

    In our previous works, it was demonstrated that the combined use of quantitative energy-dispersive electron probe X-ray microanalysis (ED-EPMA), which is also known as low-Z particle EPMA, and attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR) imaging has great potential for a detailed characterization of individual aerosol particles. In this study, extensively chemically modified (aged) individual Asian dust particles collected during an Asian dust storm event on 11 November 2002 in Korea were characterized by the combined use of low-Z particle EPMA and ATR-FTIR imaging. Overall, 109 individual particles were classified into four particle types based on their morphology, elemental concentrations, and molecular species and/or functional groups of individual particles available from the two analytical techniques: Ca-containing (38%), NaNO3-containing (30%), silicate (22%), and miscellaneous particles (10%). Among the 41 Ca-containing particles, 10, 8, and 14 particles contained nitrate, sulfate, and both, respectively, whereas only two particles contained unreacted CaCO3. Airborne amorphous calcium carbonate (ACC) particles were observed in this Asian dust sample for the first time, where their IR peaks for the insufficient symmetric environment of CO32- ions of ACC were clearly differentiated from those of crystalline CaCO3. This paper also reports the first inland field observation of CaCl2 particles probably converted from CaCO3 through the reaction with HCl(g). HCl(g) was likely released from the reaction of sea salt with NOx/HNO3, as all 33 particles of marine origin contained NaNO3 (no genuine sea salt particle was encountered). Some silicate particles with minor amounts of calcium were observed to be mixed with nitrate, sulfate, and water. Among 24 silicate particles, 10 particles are mixed with water, the presence of which could facilitate atmospheric heterogeneous reactions of silicate particles including swelling minerals, such as montmorillonite and vermiculite, and nonswelling ones, such as feldspar and quartz. This paper provides detailed information on the physicochemical characteristics of these aged individual Asia dust particles through the combined use of the two single-particle analytical techniques, and using this analytical methodology it is clearly shown that internal mixing states of the aged particles are highly complicated.

  20. Determination of trace elements in pharmaceutical substances by graphite furnace atomic absorption spectrometry and total reflection X-ray fluorescence after flow injection ion-exchange preconcentration

    NASA Astrophysics Data System (ADS)

    Kelkó-Lévai, Á.; Varga, I.; Zih-Perényi, K.; Lásztity, A.

    1999-05-01

    Flow injection iminodiacetic acid ethyl cellulose (IDAEC) microcolumn preconcentration and graphite furnace atomic absorption spectrometry determination of trace metals (Cd, Co, Ni, Pb) were carried out without decomposition of the drug matrix. The two forms of chromium Cr(III) and Cr(VI) were separated using IDAEC and anion exchanger diethylaminoethyl (DE)-cellulose, respectively. The detection limits of trace elements in pharmaceutical substances (sugars, sorbitol, mannitol, paracetamol, amidopyrine, chloral hydrate) after a 10-fold preconcentration in 1-5% m/v solution of pharmaceuticals were in the 0.3-29 ng g -1 range. The measured concentration of trace elements in substances investigated was below 100 ng g -1. The spike recovery was close to 100%. The capability of total reflection X-ray fluorescence technique for the determination of trace elements in pharmaceuticals with and without preconcentation was explored.

  1. Imaging exocytosis of single glucagon-like peptide-1 containing granules in a murine enteroendocrine cell line with total internal reflection fluorescent microscopy

    SciTech Connect

    Ohara-Imaizumi, Mica; Aoyagi, Kyota; Akimoto, Yoshihiro; Nakamichi, Yoko; Nishiwaki, Chiyono; Kawakami, Hayato; Nagamatsu, Shinya

    2009-12-04

    To analyze the exocytosis of glucagon-like peptide-1 (GLP-1) granules, we imaged the motion of GLP-1 granules labeled with enhanced yellow fluorescent protein (Venus) fused to human growth hormone (hGH-Venus) in an enteroendocrine cell line, STC-1 cells, by total internal reflection fluorescent (TIRF) microscopy. We found glucose stimulation caused biphasic GLP-1 granule exocytosis: during the first phase, fusion events occurred from two types of granules (previously docked granules and newcomers), and thereafter continuous fusion was observed mostly from newcomers during the second phase. Closely similar to the insulin granule fusion from pancreatic {beta} cells, the regulated biphasic exocytosis from two types of granules may be a common mechanism in glucose-evoked hormone release from endocrine cells.

  2. Use of total reflection X-ray fluorescence (TXRF) for the evaluation of heavy metal poisoning due to the improper use of a traditional ayurvedic drug.

    PubMed

    Borgese, L; Zacco, A; Bontempi, E; Pellegatta, M; Vigna, L; Patrini, L; Riboldi, L; Rubino, F M; Depero, L E

    2010-09-01

    An Indian patient referred to Clinica del Lavoro 'L.Devoto' of Milano showed clinical signs of heavy metal poisoning, possibly related to a sustained 6-month use of approx. 3 g/day of a traditional preparation (a whitish powder with a 'mineral' appearance) to treat urological problems. To confirm the causal relationship between the disease and the use of such product, metal testing was performed on the patient's hair and the ayurvedic remedy samples by total reflection X-ray fluorescence (TXRF). For TXRF analysis 1-cm cut of the patient's hair was directly deposited onto the quartz glass sample carrier, then 10 microl of nitric acid 65% were added and dried in air. TXRF showed high versatility, rapid and simultaneous element detection, and short analysis time, thus supporting a wider use in emergency medicine and in forensic analyses. PMID:20304577

  3. Determination of metals by total reflection X-ray fluorescence and evaluation of toxicity of a river impacted by coal mining in the south of Brazil.

    PubMed

    Lattuada, R M; Menezes, C T B; Pavei, P T; Peralba, M C R; Dos Santos, J H Z

    2009-04-30

    Metal (Fe, Mn, Zn, Ni, Cd, and Pb) concentrations in the region of Criciuma (Brazil), a region impacted by coal mining, were determined in water and sediments using total reflection X-ray fluorescence (TXRF) spectroscopy. Samples were collected from the Mãe Luzia River (south Brazil) at five different stations, from the source down to the river mouth (Ararangua estuary). Water and sediment toxicity were also evaluated using bioassays with Daphnia magna as the bioindicator. The metal present in the highest concentrations both in water (1.3-11 mg L(-1)) and in sediments (34-142 mg L(-1)) was iron. Results suggest an influence of coal mining on the aquatic receptors, showing a clear relationship between metal content (mostly Fe) and ecotoxicity. PMID:18692306

  4. Determination of trace elements in Syrian medicinal plants and their infusions by energy dispersive X-ray fluorescence and total reflection X-ray fluorescence spectrometry

    NASA Astrophysics Data System (ADS)

    Khuder, A.; Sawan, M. Kh.; Karjou, J.; Razouk, A. K.

    2009-07-01

    X-ray fluorescence (XRF) and total-reflection X-ray fluorescence (TXRF) techniques suited well for a multi-element determination of K, Ca, Mn, Fe, Cu, Zn, Rb, and Sr in some Syrian medicinal plant species. The accuracy and the precision of both techniques were verified by analyzing the Standard Reference Materials (SRM) peach-1547 and apple leaves-1515. A good agreement between the measured concentrations of the previously mentioned elements and the certified values were obtained with errors less than 10.7% for TXRF and 15.8% for XRF. The determination of Br was acceptable only by XRF with an error less than 24%. Furthermore, the XRF method showed a very good applicability for the determination of K, Ca, Mn, Fe, Cu, Zn, Rb, Sr, and Br in infusions of different Syrian medicinal plant species, namely anise ( Anisum vulgare), licorice root ( Glycyrrhiza glabra), and white wormwood ( Artemisia herba-alba).

  5. Unit Title: Imaging the Insertion of Superecliptic pHluorin Labeled Dopamine D2 Receptor Using Total Internal Reflection Fluorescence Microscopy

    PubMed Central

    Daly, Kathryn M.; Li, Yun; Lin, Da-Ting

    2015-01-01

    A better understanding of mechanisms governing receptor insertion to the plasma membrane (PM) requires an experimental approach with excellent spatial and temporal resolutions. Here we present a strategy that enables dynamic visualization of insertion events for dopamine D2 receptors into the PM. This approach includes tagging a pH-sensitive GFP, superecliptic pHluorin, to the extracellular domain of the receptor. By imaging pHluorin-tagged receptors under total internal reflection fluorescence microscopy (TIRFM), we were able to directly visualize individual receptor insertion events into the PM in cultured neurons. This novel imaging approach can be applied to both secreted proteins and many membrane proteins with an extracellular domain labeled with superecliptic pHluorin, and will ultimately allow for detailed dissections of the key mechanisms governing secretion of soluble proteins or the insertion of different membrane proteins to the PM. PMID:25559003

  6. Quantification of modifiers in advanced materials based on zinc oxide by total reflection X-ray fluorescence and inductively coupled plasma mass spectrometry

    NASA Astrophysics Data System (ADS)

    Filatova, Daria G.; Alov, Nikolai V.; Vorobyeva, Natalia A.; Rumyantseva, Marina N.; Sharanov, Pavel Yu.; Seregina, Irina F.; Gaskov, Alexander M.

    2016-04-01

    A novel approach to quantification of Ga and Zn modifiers in advanced materials based on zinc oxide is presented. The approach includes a combination of total reflection X-ray fluorescence (TXRF) and inductively coupled plasma mass spectrometry (ICP-MS) for determination and validation of the results. It is suggested to use aqueous standards for the direct determination of elements in powder samples by TXRF with a relative standard deviation no more than sr = 0.11. The accuracy of these results was proved by ICP-MS after the sample decomposition, sr(In) = 0.05, sr(Ga) = 0.06 and sr(Zn) = 0.06. It was established that there is a possibility to determine indium above 300 ppb on the background of K-M3 line of argon.

  7. Proof-of-concept demonstration of a total internal reflection based module for fluorescence and absorbance detection using a 3D-printed syringe pump

    NASA Astrophysics Data System (ADS)

    Verschooten, Tom; Ottevaere, Heidi; Vervaeke, Michael; Van Erps, Jürgen; Thienpont, Hugo

    2014-05-01

    In this paper we demonstrate the proof-of-concept of an optofluidic module capable of simultaneous laser-induced fluorescence (LIF) and absorbance (ABS) detection based on total internal reflection (TIR) optics. We discuss the design of the optofluidic detection module, its fabrication, and the setup used for the proof-of-concept. The injection of sample under test is done using two 3D printed syringe pumps, managing accurate injection and repeatable sample propagation through the detector module. We discuss the process of development behind these pumps and review their technical specifications. With this demonstrator setup we find that the limits of detection for the ABS and LIF detection of coumarin 480 are 500 nM and 100 nM respectively.

  8. In situ ATR-FTIR studies on MgCl2-diisobutyl phthalate interactions in thin film Ziegler-Natta catalysts.

    PubMed

    Cheruvathur, Ajin V; Langner, Ernie H G; Niemantsverdriet, J W Hans; Thüne, Peter C

    2012-02-01

    To study the surface structure of MgCl(2) support and its interaction with other active components in Ziegler-Natta catalyst, such as electron donors, we prepared a thin film analogue for Ziegler-Natta ethylene polymerization catalyst support by spin-coating a solution of MgCl(2) in ethanol, optionally containing a diester internal donor (diisobutyl-ortho-phthalate, DIBP) on a flat Si crystal surface. The donor content of these films was quantified by applying attenuated total internal reflection-Fourier transform infrared spectroscopy (ATR-FTIR) and X-ray photoelectron spectroscopy (XPS). Changes in the interaction of DIBP with MgCl(2) at various temperatures were monitored by in situ ATR-FTIR. Upon increasing the temperature, a shift in the (C═O) band toward lower wavenumbers was observed together with the depletion of (O-H) stretching band due to the desorption of residual ethanol. We assign this shift to gradual redistribution of adsorbed DIBP from adsorption sites on the MgCl(2) (104) surface toward the more acidic MgCl(2) (110) surface. The morphologies of MgCl(2) and MgCl(2)/DIBP films were studied by transmission electron microscopy (TEM) revealing a preferential orientation of ClMgCl layers (001) parallel to the lateral film dimensions. This orientation becomes more pronounced upon annealing. In the absence of donor, the MgCl(2) grow in to large crystals aligned in large domains upon annealing. Both crystal growth and alignment is impeded by the presence of donor. PMID:22216939

  9. Proposal of AAA-battery-size one-shot ATR Fourier spectroscopic imager for on-site analysis: Simultaneous measurement of multi-components with high accuracy

    NASA Astrophysics Data System (ADS)

    Hosono, Satsuki; Qi, Wei; Sato, Shun; Suzuki, Yo; Fujiwara, Masaru; Hiramatsu, Hiroyuki; Suzuki, Satoru; Abeygunawardhana, P. K. W.; Wada, Kenji; Nishiyama, Akira; Ishimaru, Ichiro

    2015-03-01

    For simultaneous measurement of multi-components on-site like factories, the ultra-compact (diameter: 9[mm], length: 45[mm], weight: 200[g]) one-shot ATR (Attenuated Total Reflection) Fourier spectroscopic imager was proposed. Because the proposed one-shot Fourier spectroscopic imaging is based on spatial-phase-shift interferometer, interferograms could be obtained with simple optical configurations. We introduced the transmission-type relativeinclined phase-shifter, that was constructed with a cuboid prism and a wedge prism, onto the optical Fourier transform plane of infinity corrected optical systems. And also, small light-sources and cameras in the mid-infrared light region, whose size are several millimeter on a side, are essential components for the ultra-compact spectroscopic configuration. We selected the Graphite light source (light source area: 1.7×1.7[mm], maker: Hawkeye technologies) whose radiation factor was high. Fortunately, in these days we could apply the cost-effective 2-dimensional light receiving device for smartphone (e.g. product name: LEPTON, maker: FLIR, price: around 400USD). In the case of alcoholic drinks factory, conventionally workers measure glucose and ethanol concentrations by bringing liquid solution back to laboratories every day. The high portable spectroscopy will make it possible to measure multi-components simultaneously on manufacturing scene. But we found experimentally that absorption spectrum of glucose and water and ethanol were overlapped each other in near infrared light region. But for mid-infrared light region, we could distinguish specific absorption peaks of glucose (@10.5[μm]) and ethanol (@11.5[μm]) independently from water absorption. We obtained standard curve between absorption (@9.6[μm]) and ethanol concentration with high correlation coefficient 0.98 successfully by ATR imaging-type 2-dimensional Fourier spectroscopy (wavelength resolution: 0.057[μm]) with the graphite light source (maker: Hawkeye technologies, type: IR-75).

  10. Adsorption of Organic Matter at Mineral/Water Interfaces: 7. ATR-FTIR and Quantum Chemical Study of Lactate Interactions with Hematite Nanoparticles

    SciTech Connect

    Ha, Juyoung; Yoon, Tae Hyun; Wang, Yingge; Musgrave, Charles B.; Brown, Jr., Gordon E.

    2008-12-04

    The interaction of the l-lactate ion (l-CH{sub 3}CH(OH)COO{sup -}, lact{sup -1}) with hematite ({alpha}-Fe{sub 2}O{sub 3}) nanoparticles (average diameter 11 nm) in the presence of bulk water at pH 5 and 25 C was examined using a combination of (1) macroscopic uptake measurements, (2) in situ attenuated total reflectance-Fourier transform infrared (ATR-FTIR) spectroscopy, and (3) density functional theory modeling at the B3LYP/6-31+G* level. Uptake measurements indicate that increasing [lact{sup -1}]{sub (aq)} results in an increase in lact{sup -1} uptake and a concomitant increase in Fe(III) release as a result of the dissolution of the hematite nanoparticles. The ATR-FTIR spectra of aqueous lact{sup -1} and lact{sup -1} adsorbed onto hematite nanoparticles at coverages ranging from 0.52 to 5.21 {mu}mol/m{sup 2} showed significant differences in peak positions and shapes of carboxyl group stretches. On the basis of Gaussian fits of the spectra, we conclude that lact{sup -1} is present as both outer-sphere and inner-sphere complexes on the hematite nanoparticles. No significant dependence of the extent of lact{sup -1} adsorption on background electrolyte concentration was found, suggesting that the dominant adsorption mode for lact{sup -1} is inner sphere under these conditions. On the basis of quantum chemical modeling, we suggest that inner-sphere complexes of lact{sup -1} adsorbed on hematite nanoparticles occur dominantly as monodentate, mononuclear complexes with the hydroxyl functional group pointing away from the Fe(III) center.

  11. A setup for synchrotron-radiation-induced total reflection X-ray fluorescence and X-ray absorption near-edge structure recently commissioned at BESSY II BAMline.

    PubMed

    Fittschen, U; Guilherme, A; Böttger, S; Rosenberg, D; Menzel, M; Jansen, W; Busker, M; Gotlib, Z P; Radtke, M; Riesemeier, H; Wobrauschek, P; Streli, C

    2016-05-01

    An automatic sample changer chamber for total reflection X-ray fluorescence (TXRF) and X-ray absorption near-edge structure (XANES) analysis in TXRF geometry was successfully set up at the BAMline at BESSY II. TXRF and TXRF-XANES are valuable tools for elemental determination and speciation, especially where sample amounts are limited (<1 mg) and concentrations are low (ng ml(-1) to µg ml(-1)). TXRF requires a well defined geometry regarding the reflecting surface of a sample carrier and the synchrotron beam. The newly installed chamber allows for reliable sample positioning, remote sample changing and evacuation of the fluorescence beam path. The chamber was successfully used showing accurate determination of elemental amounts in the certified reference material NIST water 1640. Low limits of detection of less than 100 fg absolute (10 pg ml(-1)) for Ni were found. TXRF-XANES on different Re species was applied. An unknown species of Re was found to be Re in the +7 oxidation state. PMID:27140163

  12. Total reflection X-ray fluorescence and energy-dispersive X-ray fluorescence analysis of runoff water and vegetation from abandoned mining of Pb Zn ores

    NASA Astrophysics Data System (ADS)

    Marques, A. F.; Queralt, I.; Carvalho, M. L.; Bordalo, M.

    2003-12-01

    The present work reports on the heavy metal content: Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Cd and Pb in running waters and vegetation around abandoned mining areas. Two species of mosses ( Dicranum sp. and Pleurocarpus sp.) and three different species of wild grass ( Bromus sp., Rumex sp. and Pseudoavena sp.) growing on the surrounding areas of old lead-zinc mines (Aran Valley, Pyrenees, NE Spain) have been analyzed. Both water and vegetation were collected in two different sampling places: (a) near the mine gallery water outlets and (b) on the landfill close to the abandoned mineral concentration factories. For the heavy metal content determination, two different techniques were used: total reflection X-ray fluorescence for water analysis and energy-dispersive X-ray fluorescence for vegetation study. Surface waters around mine outlets exhibit anomalous content of Co, Ni, Zn, Cd. Stream waters running on mining landfills exhibit higher Cu, Zn, Cd and Pb than those of the waters at the mine gallery outlets. The results allow us to assess the extent of the environmental impact of the mining activities on the water quality. The intake of these elements by vegetation was related with the sampling place, reflecting the metal water content and the substrate chemistry. Accumulation of metals in mosses is higher than those exhibited in wild grasses. Furthermore, different levels of accumulation were found in different wild grass. Rumex sp. presented the lowest metal concentrations, while Pseudoavena sp. reported the highest metal content.

  13. Biomonitoring of environmental pollution using growth tree rings of Tipuana tipu: Quantification by synchrotron radiation total reflection X-ray fluorescence

    NASA Astrophysics Data System (ADS)

    Geraldo, S. M.; Canteras, F. B.; Moreira, S.

    2014-02-01

    Currently, many studies use the bioindicators to qualitatively and/or quantitatively measure pollution. The analyses of tree growth rings represent one such bioindicator as changes in the environment are often recorded as impressions in the wood. The main objective of the present study is to examine the growth rings of Tipuana tipu - a member of the Leguminosae family that is native to Argentina and Bolivia and was introduced in Brazil as an ornamental plant - for potentially toxic elements. T. tipu is one of the most common trees in the urban landscape of Sao Paulo city and would provide an accurate reflection of environment changes. Tree ring samples previously dated using Synchrotron Radiation Total Reflection X-ray Fluorescence were collected from strategic locations in Sao Paulo. These locations include Piracicaba (SP) that has little access and small flow traffic and the campus of the University of São Paulo. Some trace elements present concentrations higher than considered as normal in some periods. In São Paulo city, samples collected from the campus of University of São Paulo (Butantã), showed the highest toxicity, with concentrations above the tolerable limit for the elements: Cr, Cu, and Pb. For the samples collected in Piracicaba city, one sample presented highest concentrations for the majority of the elements when compared to the other four samples collected at the same place, exceeding the toxicity limits for: Cr, Ni, Cu, and Pb.

  14. Structure determination of the rutile-TiO2(110)-(1 × 2) surface using total-reflection high-energy positron diffraction (TRHEPD).

    PubMed

    Mochizuki, I; Ariga, H; Fukaya, Y; Wada, K; Maekawa, M; Kawasuso, A; Shidara, T; Asakura, K; Hyodo, T

    2016-03-01

    The exact structure of the rutile-TiO2(110)-(1 × 2) surface, which had been under debate over the past 30 years, was investigated using the newly developed technique of total-reflection high-energy positron diffraction (TRHEPD), which is a positron counterpart of reflection high-energy electron diffraction (RHEED). The rocking-curves for the 00-spot obtained from the experimental diffraction patterns were compared to the curves for various models calculated with a full-dynamical theory. It was found that the rocking-curves matched those for a surface consisting of a Ti2O3 configuration, originally suggested by Onishi and Iwasawa [H. Onishi and Y. Iwasawa, Surf. Sci., 1994, 313, L783], but with a further modification of atomic positions close to the ones proposed by Wang et al. [Q. Wang, A. R. Oganov, Q. Zhu and X. F. Zhou, Phys. Rev. Lett., 2014, 113, 266101]. This result demonstrates that TRHEPD can distinguish between the existence and absence of the oxygen atoms on the topmost surface, and between the Ti atoms residing in positions at the interstitial-vertical sites and those at interstitial-horizontal sites. PMID:26884096

  15. Analysis of nutrition-relevant trace elements in human blood and serum by means of total reflection X-ray fluorescence (TXRF) spectroscopy

    NASA Astrophysics Data System (ADS)

    Stosnach, Hagen; Mages, Margarete

    2009-04-01

    In clinical service laboratories, one of the most common analytical tasks with regard to inorganic traces is the determination of the nutrition-relevant elements Fe, Cu, Zn, and Se. Because of the high numbers of samples and the commercial character of these analyses, a time-consuming sample preparation must be avoided. In this presentation, the results of total reflection X-ray fluorescence measurements with a low-power system and different sample preparation procedures are compared with those derived from analysis with common methods like Atomic Absorption Spectroscopy (AAS) and Inductively Coupled Plasma Mass Spectroscopy (ICP-MS). The results of these investigations indicate that the optimal total reflection X-ray fluorescence analysis of the nutrition-relevant elements Fe, Cu, Zn, and Se can be performed by preparing whole blood and serum samples after dilution with ultrapure water and transferring 10 μl of internally standardized sample to an unsiliconized quartz glass sample carrier with subsequent drying in a laboratory oven. Suitable measurement time was found to be 600 s. The enhanced sample preparation by means of microwave or open digestion, in parts combined with cold plasma ashing, led to an improvement of detection limits by a factor of 2 for serum samples while for whole blood samples an improvement was only observed for samples prepared by means of microwave digestion. As the matrix elements P, S, Cl, and for whole blood Fe have a major influence on the detection limits, most probably a further enhancement of analytical quality requires the removal of the organic matrix. However, for the routine analysis of the nutrition-relevant elements, the dilution preparation was found to be sufficient.

  16. Preliminary vitrinite and bitumen reflectance, total organic carbon, and pyrolysis data for samples from Upper and Lower Cretaceous strata, Maverick Basin, south Texas

    USGS Publications Warehouse

    Hackley, Paul C.; Dennen, Kristin O.; Gesserman, Rachel M.; Ridgley, Jennie L.

    2009-01-01

    The Lower Cretaceous Pearsall Formation, a regionally occurring limestone and shale interval of 500-600-ft maximum thickness (Rose, 1986), is being evaluated as part of an ongoing U.S. Geological Survey (USGS) assessment of undiscovered hydrocarbon resources in onshore Lower Cretaceous strata of the northern Gulf of Mexico. The purpose of this report is to release preliminary vitrinite and bitumen reflectance, total organic carbon, and pyrolysis data for Pearsall Formation, Glen Rose Formation, Hosston Formation, Austin Group, and Eagle Ford Group samples from the Maverick Basin in south Texas in order to aid in the characterization of these strata in this area. The preliminary nature of this report and the data contained herein reflect that the assessment and characterization of these samples is a work currently in progress. Pearsall Formation subdivisions are, in ascending stratigraphic order, the Pine Island Shale, James Limestone, and Bexar Shale Members (Loucks, 2002). The Lower Cretaceous Glen Rose Formation is also part of the USGS Lower Cretaceous assessment and produces oil in the Maverick Basin (Loucks and Kerans, 2003). The Hosston Formation was assessed by the USGS for undiscovered oil and gas resources in 2006 (Dyman and Condon, 2006), but not in south Texas. The Upper Cretaceous Austin Group is being assessed as part of the USGS assessment of undiscovered hydrocarbon resources in the Upper Cretaceous strata of the northern Gulf of Mexico and, along with the Upper Cretaceous Eagle Ford Group, is considered to be an important source rock in the Smackover-Austin-Eagleford Total Petroleum System (Condon and Dyman, 2006). Both the Austin Group and the Eagle Ford Group are present in the Maverick Basin in south Texas (Rose, 1986).

  17. The ATR barrier to replication-born DNA damage

    PubMed Central

    López-Contreras, Andrés J.; Fernandez-Capetillo, Oscar

    2013-01-01

    Replication comes with a price. The molecular gymnastics that occur on DNA during its duplication frequently derive to a wide spectrum of abnormalities which are still far from understood. These are brought together under the unifying term “replicative stress” (RS) which likely stands for large and unprotected regions of single-stranded DNA (ssDNA). In addition to RS, recombinogenic stretches of ssDNA are also formed at resected DNA double strand breaks (DSB). Both situations converge on a ssDNA intermediate, which is the triggering signal for a damage situation. The cellular response in both cases is coordinated by a phosphorylation-based signaling cascade that starts with the activation of the ATR (ATM and Rad3-related) kinase. Given that ATR is essential for replicating cells, understanding the consequences of a defective ATR response for a mammalian organism has been limited until recent years. We here discuss on the topic and review the findings that connect ATR to ageing and cancer. PMID:21036674

  18. ATR inhibition preferentially targets homologous recombination-deficient tumor cells.

    PubMed

    Krajewska, M; Fehrmann, R S N; Schoonen, P M; Labib, S; de Vries, E G E; Franke, L; van Vugt, M A T M

    2015-06-01

    Homologous recombination (HR) is required for faithful repair of double-strand DNA breaks. Defects in HR repair cause severe genomic instability and challenge cellular viability. Paradoxically, various cancers are HR defective and have apparently acquired characteristics to survive genomic instability. We aimed to identify these characteristics to uncover therapeutic targets for HR-deficient cancers. Cytogenetic analysis of 1143 ovarian cancers showed that the degree of genomic instability was correlated to amplification of replication checkpoint genes ataxia telangiectasia and Rad3-related kinase (ATR) and CHEK1. To test whether genomic instability leads to increased reliance on replication checkpoint signaling, we inactivated Rad51 to model HR-related genomic instability. Rad51 inactivation caused defective HR repair and induced aberrant replication dynamics. Notably, inhibition of Rad51 led to increased ATR/checkpoint kinase-1 (Chk1)-mediated replication stress signaling. Importantly, inhibition of ATR or Chk1 preferentially killed HR-deficient cancer cells. Combined, our data show that defective HR caused by Rad51 inhibition results in differential sensitivity for ATR and Chk1 inhibitors, implicating replication checkpoint kinases as potential drug targets for HR-defective cancers. PMID:25174396

  19. USE OF SILICON CARBIDE MONITORS IN ATR IRRADIATION TESTING

    SciTech Connect

    K. L. Davis; B. Chase; T. Unruh; D. Knudson; J. L. Rempe

    2012-07-01

    In April 2007, the Department of Energy (DOE) designated the Advanced Test Reactor (ATR) a National Scientific User Facility (NSUF) to advance US leadership in nuclear science and technology. By attracting new users from universities, laboratories, and industry, the ATR will support basic and applied nuclear research and development and help address the nation's energy security needs. In support of this new program, the Idaho National Laboratory (INL) has developed in-house capabilities to fabricate, test, and qualify new and enhanced temperature sensors for irradiation testing. Although most efforts emphasize sensors capable of providing real-time data, selected tasks have been completed to enhance sensors provided in irradiation locations where instrumentation leads cannot be included, such as drop-in capsule and Hydraulic Shuttle Irradiation System (HSIS) or 'rabbit' locations. For example, silicon carbide (SiC) monitors are now available to detect peak irradiation temperatures between 200°C and 800°C. Using a resistance measurement approach, specialized equipment installed at INL's High Temperature Test Laboratory (HTTL) and specialized procedures were developed to ensure that accurate peak irradiation temperature measurements are inferred from SiC monitors irradiated at the ATR. Comparison examinations were completed by INL to demonstrate this capability, and several programs currently rely on SiC monitors for peak temperature detection. This paper discusses the use of SiC monitors at the ATR, the process used to evaluate them at the HTTL, and presents representative measurements taken using SiC monitors.

  20. WWOX modulates the ATR-mediated DNA damage checkpoint response

    PubMed Central

    Abu-Odeh, Mohammad; Hereema, Nyla A.; Aqeilan, Rami I.

    2016-01-01

    For many decades genomic instability is considered one of the hallmarks of cancer. Role of the tumor suppressor WWOX (WW domain-containing oxidoreductase) in DNA damage response upon double strand breaks has been recently revealed. Here we demonstrate unforeseen functions for WWOX upon DNA single strand breaks (SSBs) checkpoint activation. We found that WWOX levels are induced following SSBs and accumulate in the nucleus. WWOX deficiency is associated with reduced activation of ataxia telangiectasia and Rad3-related protein (ATR) checkpoint proteins and increased chromosomal breaks. At the molecular level, we show that upon SSBs WWOX is modified at lysine 274 by ubiquitination mediated by the ubiquitin E3 ligase ITCH and interacts with ataxia telangiectasia-mutated (ATM). Interestingly, ATM inhibition was associated with reduced activation of ATR checkpoint proteins suggesting that WWOX manipulation of ATR checkpoint proteins is ATM-dependent. Taken together, the present findings indicate that WWOX plays a key role in ATR checkpoint activation, while its absence might facilitate genomic instability. PMID:26675548

  1. 30 CFR 75.209 - Automated Temporary Roof Support (ATRS) systems.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... 30 Mineral Resources 1 2012-07-01 2012-07-01 false Automated Temporary Roof Support (ATRS) systems... Automated Temporary Roof Support (ATRS) systems. (a) Except in anthracite mines and as specified in paragraphs (b) and (c) of this section, an ATRS system shall be used with roof bolting machines...

  2. 30 CFR 75.209 - Automated Temporary Roof Support (ATRS) systems.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... 30 Mineral Resources 1 2013-07-01 2013-07-01 false Automated Temporary Roof Support (ATRS) systems... Automated Temporary Roof Support (ATRS) systems. (a) Except in anthracite mines and as specified in paragraphs (b) and (c) of this section, an ATRS system shall be used with roof bolting machines...

  3. 30 CFR 75.209 - Automated Temporary Roof Support (ATRS) systems.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... 30 Mineral Resources 1 2010-07-01 2010-07-01 false Automated Temporary Roof Support (ATRS) systems... Automated Temporary Roof Support (ATRS) systems. (a) Except in anthracite mines and as specified in paragraphs (b) and (c) of this section, an ATRS system shall be used with roof bolting machines...

  4. 30 CFR 75.209 - Automated Temporary Roof Support (ATRS) systems.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... 30 Mineral Resources 1 2011-07-01 2011-07-01 false Automated Temporary Roof Support (ATRS) systems... Automated Temporary Roof Support (ATRS) systems. (a) Except in anthracite mines and as specified in paragraphs (b) and (c) of this section, an ATRS system shall be used with roof bolting machines...

  5. 30 CFR 75.209 - Automated Temporary Roof Support (ATRS) systems.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... 30 Mineral Resources 1 2014-07-01 2014-07-01 false Automated Temporary Roof Support (ATRS) systems... Automated Temporary Roof Support (ATRS) systems. (a) Except in anthracite mines and as specified in paragraphs (b) and (c) of this section, an ATRS system shall be used with roof bolting machines...

  6. 78 FR 70892 - Airworthiness Directives; ATR-GIE Avions de Transport Régional Airplanes

    Federal Register 2010, 2011, 2012, 2013, 2014

    2013-11-27

    ...; ] DEPARTMENT OF TRANSPORTATION Federal Aviation Administration 14 CFR Part 39 RIN 2120-AA64 Airworthiness Directives; ATR--GIE Avions de Transport R gional Airplanes AGENCY: Federal Aviation Administration (FAA... directive (AD) 2009-18- 18, which applies to certain ATR--GIE Avions de Transport R gional Model ATR42...

  7. Validation of HELIOS for ATR Core Follow Analyses

    SciTech Connect

    Bays, Samuel E.; Swain, Emily T.; Crawford, Douglas S.; Nigg, David W.

    2015-03-01

    This work summarizes the validation analyses for the HELIOS code to support core design and safety assurance calculations of the Advanced Test Reactor (ATR). Past and current core safety assurance is performed by the PDQ-7 diffusion code; a state of the art reactor physics simulation tool from the nuclear industry’s earlier days. Over the past twenty years, improvements in computational speed have enabled the use of modern neutron transport methodologies to replace the role of diffusion theory for simulation of complex systems, such as the ATR. More exact methodologies have enabled a paradigm-shift away from highly tuned codes that force compliance with a bounding safety envelope, and towards codes regularly validated against routine measurements. To validate HELIOS, the 16 ATR operational cycles from late-2009 to present were modeled. The computed power distribution was compared against data collected by the ATR’s on-line power surveillance system. It was found that the ATR’s lobe-powers could be determined with ±10% accuracy. Also, the ATR’s cold startup shim configuration for each of these 16 cycles was estimated and compared against the reported critical position from the reactor log-book. HELIOS successfully predicted criticality within the tolerance set by the ATR startup procedure for 13 out of the 16 cycles. This is compared to 12 times for PDQ (without empirical adjustment). These findings, as well as other insights discussed in this report, suggest that HELIOS is highly suited for replacing PDQ for core safety assurance of the ATR. Furthermore, a modern verification and validation framework has been established that allows reactor and fuel performance data to be computed with a known degree of accuracy and stated uncertainty.

  8. Integrate knowledge acquisition with target recognition through closed-loop ATR

    NASA Astrophysics Data System (ADS)

    Yu, Ssu-Hsin; McLaughlin, Pat; Zatezalo, Aleksandar; Hsiao, Kai-yuh; Boskovic, Jovan

    2015-05-01

    Automatic Target Recognition (ATR) algorithm performance is highly dependent on the sensing conditions under which the input data is collected. Open-loop fly-bys often produce poor results due to less than ideal measurement conditions. In addition, ATR algorithms must be extremely complicated to handle the diverse range of inputs with a resulting reduction in overall performance and increase in complexity. Our approach, closed-loop ATR (CL-ATR), focuses on improving the quality of information input to the ATR algorithms by optimizing motion, sensor settings and team (vehicle-vehicle-human) collaboration to dramatically improve classification accuracy. By managing the data collection guided by predicted ATR performance gain, we increase the information content of the data and thus dramatically improve ATR performance with existing ATR algorithms. CL-ATR has two major functions; first, an ATR utility function, which represents the performance sensitivity of ATR produced classification labels as a function of parameters that correlate to vehicle/sensor states. This utility function is developed off-line and is often available from the original ATR study as a confusion matrix, or it can be derived through simulation without direct access to the inner working of the ATR algorithm. The utility function is inserted into our CLATR framework to autonomously control the vehicle/sensor. Second, an on-board planner maps the utility function into vehicle position and sensor collection plans. Because we only require the utility function on-board, we can activate any ATR algorithm onto a unmanned aerial vehicle (UAV) platform no matter how complex. This pairing of ATR performance profiles with vehicle/sensor controls creates a unique and powerful active perception behavior.

  9. Application of total-reflection X-ray fluorescence spectrometry and high-performance liquid chromatography for the chemical characterization of xylem saps of nickel contaminated cucumber plants

    NASA Astrophysics Data System (ADS)

    Mihucz, Victor G.; Tatár, Eniko; Varga, Anita; Záray, Gyula; Cseh, Edit

    2001-11-01

    Total-reflection X-ray fluorescence (TXRF) spectrometry, reversed-phase (RP) and size-exclusion (SE) high-performance liquid chromatography (HPLC) methods were applied for the characterization of low-volume xylem sap of control and nickel contaminated cucumber plants growing in hydroponics containing urea as the sole nitrogen source. In these saps collected for 1 h, Ca, K, Fe, Mn, Ni, Zn, as well as malic, citric and fumaric acids were determined. The SEC measurements showed that macromolecules were not detectable in the samples. Nickel contamination had minimum impact on the organic acid transport, however, the transport of Zn, K and Fe was reduced by 50, 22 and 11%, respectively. This observation supports the results of our earlier experiments when nitrate ions were used as the sole nitrogen form. At the same time, the fresh root weight and the volume of the collected xylem sap increased by 36 and 85%, respectively. Therefore, nickel addition seemed to decrease the urea toxicity of the plants. By pooling the eluting fractions of the SEC column, which were 10-fold concentrated by freeze-drying, the series of the resulted samples were analyzed by the TXRF spectrometry and RP-HPLC. The three organic acids could be identified in only one of the fractions, which contained Fe and, in the case of the contaminated plants, Ni in detectable concentration. However, considerable parts of these two elements and Mn, as well as practically the total amounts of Cu may be transported by unidentified organic compounds in the xylem.

  10. The SUMO (Small Ubiquitin-like Modifier) Ligase PIAS3 Primes ATR for Checkpoint Activation.

    PubMed

    Wu, Ching-Shyi; Zou, Lee

    2016-01-01

    The maintenance of genomic stability relies on the concerted action of DNA repair and DNA damage signaling pathways. The PIAS (protein inhibitor of activated STAT) family of SUMO (small ubiquitin-like modifier) ligases has been implicated in DNA repair, but whether it plays a role in DNA damage signaling is still unclear. Here, we show that the PIAS3 SUMO ligase is important for activation of the ATR (ataxia telangiectasia and Rad3 related)-regulated DNA damage signaling pathway. PIAS3 is the only member of the PIAS family that is indispensable for ATR activation. In response to different types of DNA damage and replication stress, PIAS3 plays multiple roles in ATR activation. In cells treated with camptothecin (CPT), PIAS3 contributes to formation of DNA double-stranded breaks. In UV (ultraviolet light)- or HU (hydroxyurea)-treated cells, PIAS3 is required for efficient ATR autophosphorylation, one of the earliest events during ATR activation. Although PIAS3 is dispensable for ATRIP (ATR-interacting protein) SUMOylation and the ATR-ATRIP interaction, it is required for maintaining the basal kinase activity of ATR prior to DNA damage. In the absence of PIAS3, ATR fails to display normal kinase activity after DNA damage, which accompanies with reduced phosphorylation of ATR substrates. Together, these results suggest that PIAS3 primes ATR for checkpoint activation by sustaining its basal kinase activity, revealing a new function of the PIAS family in DNA damage signaling. PMID:26565033

  11. ATR localizes to the photoreceptor connecting cilium and deficiency leads to severe photoreceptor degeneration in mice.

    PubMed

    Valdés-Sánchez, Lourdes; De la Cerda, Berta; Diaz-Corrales, Francisco J; Massalini, Simone; Chakarova, Christina F; Wright, Alan F; Bhattacharya, Shomi S

    2013-04-15

    Ataxia-telangiectasia and Rad3 (ATR), a sensor of DNA damage, is associated with the regulation and control of cell division. ATR deficit is known to cause Seckel syndrome, characterized by severe proportionate short stature and microcephaly. We used a mouse model for Seckel disease to study the effect of ATR deficit on retinal development and function and we have found a new role for ATR, which is critical for the postnatal development of the photoreceptor (PR) layer in mouse retina. The structural and functional characterization of the ATR(+/s) mouse retinas displayed a specific, severe and early degeneration of rod and cone cells resembling some characteristics of human retinal degenerations. A new localization of ATR in the cilia of PRs and the fact that mutant mice have shorter cilia suggests that the PR degeneration here described results from a ciliary defect. PMID:23297361

  12. Monitoring of the environmental pollution by trace element analysis in tree-rings using synchrotron radiation total reflection X-ray fluorescence

    NASA Astrophysics Data System (ADS)

    de Vives, Ana Elisa Sirito; Moreira, Silvana; Brienza, Sandra Maria Boscolo; Medeiros, Jean Gabriel Silva; Filho, Mário Tomazello; Zucchi, Orghêda Luíza Araújo Domingues; Filho, Virgílio Franco do Nascimento

    2006-11-01

    This paper aims to study the environmental pollution in the tree development, in order to evaluate its use as bioindicator in urban and country sides. The sample collection was carried out in Piracicaba city, São Paulo State, which presents high level of environmental contamination in water, soil and air, due to industrial activities, vehicles combustion, sugar-cane leaves burning in the harvesting, etc. The species Caesalpinia peltophoroides ("Sibipiruna") was selected because it is widely used in urban forestation. Synchrotron Radiation Total Reflection X-ray Fluorescence technique (SR-TXRF) was employed to identify and quantify the elements and metals of nutritional and toxicological importance in the wood samples. The analysis was performed in the Brazilian Synchrotron Light Source Laboratory, using a white beam for excitation and a Si(Li) detector for X-ray detection. In several samples, P, K, Ca, Ti, Fe, Sr, Ba and Pb were quantified. The K/Ca, K/P and Pb/Ca ratios were found to decrease towards the bark.

  13. Mechanism of formation of humus coatings on mineral surfaces 2. Attenuated total reflectance spectra of hydrophobic and hydrophilic fractions of organic acids from compost leachate on alumina

    USGS Publications Warehouse

    Wershaw, R. L.; Llaguno, E.C.; Leenheer, J.A.; Sperline, R.P.; Song, Y.

    1996-01-01

    Hydrophobic and hydrophilic fractions were isolated from a compost leachate. The adsorption isotherms of both fractions on alumina were measured by attenuated total reflectance infrared spectroscopy. The shapes of the adsorption isotherms of the two fractions were different. The isotherms for the hydrophilic fraction showed little change in surface excess with increasing solution concentration above 4 mg L-1. The isotherms for the hydrophobic fraction, on the other hand, displayed a marked increase in surface excess with increasing solution concentration. This increase is evidence for the formation of aggregates (admicelles or hemimicelles) on the alumina surface. Linear dichroism calculations indicated that more of the carboxylate groups in the adsorbed hydrophobic molecules than in the absorbed hydrophilic fraction were free to rotate. The hindered rotation of the carboxylate groups in the adsorbed hydrophilic-fraction molecules probably indicates that these groups are bound to surface aluminum ions by a bidentate mechanism in which the two oxygen atoms of a single carboxylate group bind to separate aluminum ions.

  14. A simple method for the multi-elemental analysis of organic fertilizer by slurry sampling and total reflection X-ray fluorescence.

    PubMed

    Resende, Luciene V; Nascentes, Clésia C

    2016-01-15

    A simple and fast method for the multi-elemental determination of 18 inorganic constituents (P, S, Cl, K, Ca, Ti, Cr, V, Mn, Fe, Ni, Cu, Zn, Br, Rb, Sr, Ba and Pb) in organic fertilizers employing slurry sampling and total reflection X-ray fluorescence (TXRF) is presented. A 2(3) factorial design with a central point was employed to optimize the slurry sampling procedure. The internal standard and instrumental conditions were optimized by univariate studies. The selectivity of the method to determining Se, As, Pb, Cr, Ni and Cd was assessed. The accuracy was evaluated by the analysis of four standard reference materials (SRM). The recoveries varied from 72% to 114%. For most of the elements, good agreement was achieved between the certified value and the value measured in the SRM. The relative standard deviation (RSD %) ranged from 0.5% to 14%. The evaluated method was applied to the determination of analytes in the press cake of palm, castor, curcas, sunflower, fodder turnip, white lupin, rapeseed and pequi, and their potential to be used as organic fertilizer was evaluated in accordance with Brazilian legislation. PMID:26592637

  15. Near-surface density of ion-implanted Si studied by Rutherford backscattering and total-reflection x-ray fluorescence

    SciTech Connect

    Klockenkaemper, R.; Becker, M.; Bohlen, A. von; Becker, H.W.; Krzyzanowska, H.; Palmetshofer, L.

    2005-08-01

    The implantation of ions in solids is of high technical relevance. The different effects within the solid target caused by the ion bombardment can be investigated by depth profiling of near-surface layers. As and Co ions were implanted in Si wafers: As ions with a fluence of 1x10{sup 17}/cm{sup 2} and an energy of 100 keV and Co ions with 1x10{sup 16}/cm{sup 2} at 25 keV. Subsequently depth profiling was carried out by Rutherford backscattering spectrometry as well as by total-reflection x-ray fluorescence analysis which was combined with differential weighing and interferometry after repeated large-surface sputter etching. Over and above the amorphization of the Si crystal, two other essential effects were observed: (i) a swelling or expansion of the original Si crystal in the near-surface region, in particular in the case of the As implantation, and (ii) a shrinking or compression of the Si crystal for deeper sublayers especially distinct for the Co implantation. On the other hand, a high surface enrichment of implanted ions was found for the As implantation while only a low surface concentration was detected for the Co implantation.

  16. Whole-Cell Scan using Automatic Variable-Angle and Variable-Illumination-Depth Pseudo—Total Internal Reflection Fluorescence Microscopy

    SciTech Connect

    Sun, Wei; Xu, Aoshuang; Marchuk, Kyle; Wang, Gufeng; Fang, Ning

    2011-08-01

    An automatic calibration and angle-scanning prism-type total internal reflection fluorescence microscope (TIRFM) was modified to function in both TIRFM and pseudo-TIRFM modes. When the incident angle of the excitation laser beam was controlled to be larger than the critical angle, the instrument served as a variable-angle TIRFM. A homemade computer program automatically calibrates the laser illumination spot in the sample to overlap with the center of the microscope's field of view. Then, by measuring the fluorescence intensities at different incident angles, the z-positions of fluorescent nanospheres close to the cell basolateral membrane can be extracted. When the incident angle is reduced to be in the subcritical range, the instrument works as a pseudo-TIRFM. The whole cell body from bottom to top can be imaged in a vertical scan process. Furthermore, the illumination field depth in the pseudo-TIRFM can be controlled by changing the incident angle or the horizontal position of the laser spot.

  17. Analysis of some chosen elements of cerebrospinal fluid and serum in amyotrophic lateral sclerosis patients by total reflection X-ray fluorescence

    NASA Astrophysics Data System (ADS)

    Ostachowicz, B.; Lankosz, M.; Tomik, B.; Adamek, D.; Wobrauschek, P.; Streli, C.; Kregsamer, P.

    2006-11-01

    Trace elements play an important role in the human central nervous system. Significant variations of the concentration of trace elements in body fluids may occur in neurodegenerative diseases. In the present work an investigation of the elemental composition of the serum, and the cerebrospinal fluid in amyotrophic lateral sclerosis patients and a control group was performed. For the analysis of the body fluids Total reflection X-ray Fluorescence (TXRF) spectrometry was used. The samples were taken during routine diagnostic procedures. Na, Mg, Cl, K, Ca, Cu, Zn, and Br were determined in both fluids. In order to validate the results of analysis a serum standard reference material was measured. A t-test was applied to check if the mean concentrations of the elements are different for ALS and the control group. For the serum samples higher values for Br were found in the ALS group, for the cerebrospinal fluid lower values of Na, Mg and Zn as well as higher Ca values were found in the ALS group compared to the control group.

  18. Characterization by Total Reflection X-ray Fluorescence Spectrometry of filtered water into the cave under the Sun Pyramid in Teotihuacan City

    NASA Astrophysics Data System (ADS)

    Martinez, T.; Zarazua, G.; Avila-Perez, P.; Juarez, F.; Cabrera, L.; Martinez, G.

    2008-12-01

    Teotihuacan (50 km north-east Mexico City) was the most important ancient city in Mesoamerica and it flourished 200-750 AC. It is situated in the central part of the Valley of Teotihuacan, in Central México. This study was carried out in the 102 m-long cave under the largest single construction, the massive Sun Pyramid, being located on the east side of the "Avenue of the Dead", in the northern half-part of the city. The study shows the results of Total Reflection X-ray Fluorescence Spectrometry analysis and other techniques of a water sample obtained from the inside of the cave. The inside temperature ranged between 19 and 22 °C; relative humidity was between 98 and 99.3%; water-dropping velocity (water de-sorption capability) was 13.5 μL min - 1 . Water samples from wells around the site were analyzed too. Metal concentration in all of the water samples matches the characteristics of the sampling site, well's depth, soil and minerals.

  19. Development and validation of an environmentally friendly attenuated total reflectance in the mid-infrared region method for the determination of ethanol content in used engine lubrication oil.

    PubMed

    Hatanaka, Rafael Rodrigues; Sequinel, Rodrigo; Gualtieri, Carlos Eduardo; Tercini, Antônio Carlos Bergamaschi; Flumignan, Danilo Luiz; de Oliveira, José Eduardo

    2013-05-15

    Lubricating oils are crucial in the operation of automotive engines because they both reduce friction between moving parts and protect against corrosion. However, the performance of lubricant oil may be affected by contaminants, such as gasoline, diesel, ethanol, water and ethylene glycol. Although there are many standard methods and studies related to the quantification of contaminants in lubricant oil, such as gasoline and diesel oil, to the best of our knowledge, no methods have been reported for the quantification of ethanol in used Otto cycle engine lubrication oils. Therefore, this work aimed at the development and validation of a routine method based on partial least-squares multivariate analysis combined with attenuated total reflectance in the mid-infrared region to quantify ethanol content in used lubrication oil. The method was validated based on its figures of merit (using the net analyte signal) as follows: limit of detection (0.049%), limit of quantification (0.16%), accuracy (root mean square error of prediction=0.089% w/w), repeatability (0.05% w/w), fit (R(2)=0.9997), mean selectivity (0.047), sensitivity (0.011), inverse analytical sensitivity (0.016% w/w(-1)) and signal-to-noise ratio (max: 812.4 and min: 200.9). The results show that the proposed method can be routinely implemented for the quality control of lubricant oils. PMID:23618159

  20. Total internal reflection plasmonic scattering-based fluorescence-free nanoimmunosensor probe for ultra-sensitive detection of cancer antigen 125.

    PubMed

    Chakkarapani, Suresh Kumar; Zhang, Peng; Ahn, Sujin; Kang, Seong Ho

    2016-07-15

    Highly sensitive detection of cancer antigen 125 (CA125) on nanoarray chips was carried out by means of total internal reflection (TIR) microscopy based on fluorescent labeling (i.e., TIR fluorescence microscopy; TIRFM) and fluorescent-free labeling (TIR scattering microscopy; TIRSM). TIR plasmonic scattering of nanoparticles (NPs) as a fluorescence-free immunosensor probe potentially superior to fluorescent probes was applied to quantify CA125 on a nanoarray chip. NP-labeled CA125 (NP-CA125) was immunoreacted on chips, and the TIR scattering illumination of NP-CA125 allowed quantitative TIRSM measurement of wavelength-dependent plasmonic scattering detection of CA125. In addition, Alexafluor 488-labeled CA125 was immunoreacted on the same chips for comparison of detection sensitivity. TIRSM showed less photobleaching and higher photostability and detection sensitivity than TIRFM, as well as a lower limit of detection (LOD), 0.0018U/mL. This LOD was ~144 times lower than that of previously reported detection methods. These results demonstrated that the wavelength-dependent TIR plasmon NPs can be used as an enhanced nanoimmunosensor probe, providing ultra-sensitive fluorescence-free biomolecule detection to enable earliest-stage disease diagnosis. PMID:26913504