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Sample records for fused silica capillary

  1. Capillary electrophoresis in a fused-silica capillary with surface roughness gradient.

    Science.gov (United States)

    Horká, Marie; Šlais, Karel; Karásek, Pavel; Růžička, Filip; Šalplachta, Jiří; Šesták, Jozef; Kahle, Vladislav; Roth, Michal

    2016-10-01

    The electro-osmotic flow, a significant factor in capillary electrophoretic separations, is very sensitive to small changes in structure and surface roughness of the inner surface of fused silica capillary. Besides a number of negative effects, the electro-osmotic flow can also have a positive effect on the separation. An example could be fused silica capillaries with homogenous surface roughness along their entire separation length as produced by etching with supercritical water. Different strains of methicillin-resistant and methicillin-susceptible Staphylococcus aureus were separated on that type of capillaries. In the present study, fused-silica capillaries with a gradient of surface roughness were prepared and their basic behavior was studied in capillary zone electrophoresis with UV-visible detection. First the influence of the electro-osmotic flow on the peak shape of a marker of electro-osmotic flow, thiourea, has been discussed. An antifungal agent, hydrophobic amphotericin B, and a protein marker, albumin, have been used as model analytes. A significant narrowing of the detected zones of the examined analytes was achieved in supercritical-water-treated capillaries as compared to the electrophoretic separation in smooth capillaries. Minimum detectable amounts of 5 ng/mL amphotericin B and 5 μg/mL albumin were reached with this method.

  2. A new method for synthesizing fluid inclusions in fused silica capillaries containing organic and inorganic material

    Science.gov (United States)

    Chou, I.-Ming; Song, Y.; Burruss, R.C.

    2008-01-01

    Considerable advances in our understanding of physicochemical properties of geological fluids and their roles in many geological processes have been achieved by the use of synthetic fluid inclusions. We have developed a new method to synthesize fluid inclusions containing organic and inorganic material in fused silica capillary tubing. We have used both round (0.3 mm OD and 0.05 or 0.1 mm ID) and square cross-section tubing (0.3 ?? 0.3 mm with 0.05 ?? 0.05 mm or 0.1 ?? 0.1 mm cavities). For microthermometric measurements in a USGS-type heating-cooling stage, sample capsules must be less than 25 mm in length. The square-sectioned capsules have the advantage of providing images without optical distortion. However, the maximum internal pressure (P; about 100 MPa at 22 ??C) and temperature (T; about 500 ??C) maintained by the square-sectioned capsules are less than those held by the round-sectioned capsules (about 300 MPa at room T, and T up to 650 ??C). The fused silica capsules can be applied to a wide range of problems of interest in fluid inclusion and hydrothermal research, such as creating standards for the calibration of thermocouples in heating-cooling stages and frequency shifts in Raman spectrometers. The fused silica capsules can also be used as containers for hydrothermal reactions, especially for organic samples, including individual hydrocarbons, crude oils, and gases, such as cracking of C18H38 between 350 and 400 ??C, isotopic exchanges between C18H38 and D2O and between C19D40 and H2O at similar temperatures. Results of these types of studies provide information on the kinetics of oil cracking and the changes of oil composition under thermal stress. When compared with synthesis of fluid inclusions formed by healing fractures in quartz or other minerals or by overgrowth of quartz at elevated P-T conditions, the new fused-silica method has the following advantages: (1) it is simple; (2) fluid inclusions without the presence of water can be formed; (3

  3. Comparison of three modifications of fused-silica capillaries and untreated capillaries for protein profiling of maize extracts by capillary electrophoresis.

    Science.gov (United States)

    Pobozy, Ewa; Sentkowska, Aleksandra; Piskor, Anna

    2014-09-01

    In this work, capillary electrophoresis was applied to protein profiling of fractionated extracts of maize. A comparative study on the application of uncoated fused-silica capillaries and capillaries modified with hydroxypropylmethylcellulose, ω-iodoalkylammonium salt and a commercially available neutral capillary covalently coated with polyacrylamide is presented. The coating stability, background electrolyte composition, and separation efficiency were investigated. It was found that for zeins separation, the most stable and efficient was the capillary coated with polyacrylamide. Finally, the usefulness of these methods was studied for the differentiation of zein fraction in transgenic and nontransgenic maize. Zeins extracted from maize standards containing 0 and 5% m/m genetic modification were successfully separated, but slight differences were observed in terms of the zein content. Albumin and globulin fractions were analyzed with the use of unmodified fused-silica capillary with borate buffer pH 9 and the capillary coated with polyacrylamide with phosphate buffer pH 3. In the albumin fraction, additional peaks were found in genetically modified samples.

  4. Hydrolysis of polycarbonate in sub-critical water in fused silica capillary reactor with in situ Raman spectroscopy

    Science.gov (United States)

    Pan, Z.; Chou, I.-Ming; Burruss, R.C.

    2009-01-01

    The advantages of using fused silica capillary reactor (FSCR) instead of conventional autoclave for studying chemical reactions at elevated pressure and temperature conditions were demonstrated in this study, including the allowance for visual observation under a microscope and in situ Raman spectroscopic characterization of polycarbonate and coexisting phases during hydrolysis in subcritical water. ?? 2009 The Royal Society of Chemistry.

  5. Separation of iron-free and iron-saturated forms of transferrin and lactoferrin via capillary electrophoresis performed in fused-silica and neutral capillaries.

    Science.gov (United States)

    Nowak, Paweł; Śpiewak, Klaudyna; Brindell, Małgorzata; Woźniakiewicz, Michał; Stochel, Grażyna; Kościelniak, Paweł

    2013-12-20

    A capillary electrophoresis-based method for the cost-effective and high efficient separation of iron-free and iron-saturated forms of two members of transferrin family: transferrin and lactoferrin has been developed. The proposed qualitative method relying on the SDS application allowed us to separate iron-free and iron-saturated forms of these proteins, as well as human serum albumin, used as an internal standard. Owing to the distinct migration times under established conditions, the combination of transferrin and lactoferrin assays within a single analytical procedure was feasible. The performance of the method using a fused-silica capillary has been compared with the results obtained using the same method but performed with the use of a neutral capillary of the same dimensions. Neutral capillary has been used as an alternative, since the comparable resolution has been achieved with a concomitant reduction of the electroosmotic flow. Despite of this fact, the migration of analytes occurred with similar velocity but in opposite order, due to the reverse polarity application. A quantitative method employing fused-silica capillary for iron saturation study has been also developed, to evaluate the iron saturation in commercial preparations of lactoferrin.

  6. Determination of diffusion coefficients of hydrogen in fused silica between 296 and 523 K by Raman spectroscopy and application of fused silica capillaries in studying redox reactions

    Science.gov (United States)

    Shang, L.; Chou, I.-Ming; Lu, W.; Burruss, R.C.; Zhang, Y.

    2009-01-01

    Diffusion coefficients (D) of hydrogen in fused silica capillaries (FSC) were determined between 296 and 523 K by Raman spectroscopy using CO2 as an internal standard. FSC capsules (3.25 ?? 10-4 m OD, 9.9 ?? 10-5 m ID, and ???0.01 m long) containing CO2 and H2 were prepared and the initial relative concentrations of hydrogen in these capsules were derived from the Raman peak-height ratios between H2 (near 587 cm-1) and CO2 (near 1387 cm-1). The sample capsules were then heated at a fixed temperature (T) at one atmosphere to let H2 diffuse out of the capsule, and the changes of hydrogen concentration were monitored by Raman spectroscopy after quench. This process was repeated using different heating durations at 296 (room T), 323, 375, 430, 473, and 523 K; the same sample capsule was used repeatedly at each temperature. The values of D (in m2 s-1) in FSC were obtained by fitting the observed changes of hydrogen concentration in the FSC capsule to an equation based on Fick's law. Our D values are in good agreement with the more recent of the two previously reported experimental data sets, and both can be represented by: ln D = - (16.471 ?? 0.035) - frac(44589 ?? 139, RT) (R2 = 0.99991) where R is the gas constant (8.3145 J/mol K), T in Kelvin, and errors at 1?? level. The slope corresponds to an activation energy of 44.59 ?? 0.14 kJ/mol. The D in FSC determined at 296 K is about an order of magnitude higher than that in platinum at 723 K, indicating that FSC is a suitable membrane for hydrogen at temperature between 673 K and room temperature, and has a great potential for studying redox reactions at these temperatures, especially for systems containing organic material and/or sulphur. ?? 2009 Elsevier Ltd.

  7. Pepsin immobilized in dextran-modified fused-silica capillaries for on-line protein digestion and peptide mapping

    Energy Technology Data Exchange (ETDEWEB)

    Stigter, E.C.A. [Division of Biomedical Analysis, Department of Pharmaceutical Sciences, Faculty of Science, Utrecht University, Sorbonnelaan 16, 3584 CA Utrecht (Netherlands)], E-mail: e.c.a.stigter@uu.nl; Jong, G.J. de; Bennekom, W.P. van [Division of Biomedical Analysis, Department of Pharmaceutical Sciences, Faculty of Science, Utrecht University, Sorbonnelaan 16, 3584 CA Utrecht (Netherlands)

    2008-07-07

    On-line digestion of proteins under acidic conditions was studied using micro-reactors consisting of dextran-modified fused-silica capillaries with covalently immobilized pepsin. The proteins used in this study differed in molecular weight, isoelectric point and sample composition. The injected protein samples were completely digested in 3 min and the digest was analyzed with micro-high performance liquid chromatography (HPLC) and tandem mass spectrometry (MS/MS). The different proteins present in the samples could be identified with a Mascot database search on the basis of auto-MS/MS data. It proved also to be possible to digest and analyze protein mixtures with a sequence coverage of 55% and 97% for the haemoglobin {beta}- and {alpha}-chain, respectively, and 35-55% for the various casein variants. Protease auto-digestion, sample carry-over and loss of signal due to adsorption of the injected proteins were not observed. The backpressure of the reactor is low which makes coupling to systems such as Surface Plasmon Resonance biosensors, which do not tolerate too high pressure, possible. The reactor was stable for at least 40 days when used continuously.

  8. Automated coating procedures to produce poly(ethylene glycol) brushes in fused-silica capillaries

    DEFF Research Database (Denmark)

    Poulsen, Nicklas N.; Østergaard, Jesper; Petersen, Nickolaj J.

    2017-01-01

    . Flexible and reliable approaches for preventing unwanted protein adsorption in separation science are thus in high demand. We therefore present new coating approaches based on an automated in-capillary surface initiated atom transfer radical polymerization process (covalent coating) as well...... as by electrostatically adsorbing a pre-synthesized polymer leading to functionalized molecular brushes. The electroosmotic flow was measured following each step of the covalent coating procedure providing a detailed characterization and quality control. Both approaches resulted in good fouling resistance against...... the four model proteins cytochrome c, myoglobin, ovalbumin and human serum albumin in the pH range 3.4-8.4. Further, even samples containing 10% v/v plasma derived from human blood did not show signs of adsorbing to the coated capillaries. The covalent as well as the electrostatically adsorbed coating were...

  9. Electrophoretic behavior of charge regulated zwitter ionic buffers in covalently and dynamically coated fused silica capillaries

    Directory of Open Access Journals (Sweden)

    Medhat A. Al-Ghobashy

    2014-06-01

    Full Text Available In this work, the electrophoretic behavior of zwitterionic buffers is investigated in the absence of electroosmotic flow (EOF. Electro mobilization of capillary contents is noted when zwitterionic buffers are employed as the background electrolyte at a pH where the buffering moiety carries a net charge. The bulk flow of capillary contents was demonstrated via monitoring the migration of a neutral marker as well as a free and micellar negatively charged marker and SDS–protein complexes. This electrolyte-driven mobilization (EDM was investigated in detail using 4-(2-hydroxyethylpiprazine-1-ethanesulfonic acid (HEPES buffer over a wide pH range (pH 4.0–8.0. Results confirmed that at a pH where HEPES molecules carry a net negative charge, a bulk flow toward the anode is observed. This was attributed to the migration of HEPES ions toward the anode along with their hydration shells. The relatively large difference in size and solvation number between the ionic buffering moiety and its counter-migrating ions (Na+ or H+ resulted in such a net movement. Results indicated that at constant voltage, plotting the measured current versus buffer pH can be used for determination of the isoelectric point of the zwitterionic buffering moiety. Furthermore, this novel mobilization modality was demonstrated using five different HEPES analogs over pH range 5.0–8.0. More in depth investigations are required in order to explore the applicability of EDM in coated capillaries of different wall chemistries and dimensions.

  10. Analysis of polycyclic aromatic hydrocarbons I. Determination by gas chromatography with glass and fused silica capillary columns; Analisis de Hidrocarburos aromaticos policiclicos. I. Determinacion por cromatografia de gases con columnas capilares de vidrio de silice fundida

    Energy Technology Data Exchange (ETDEWEB)

    Perez, M. M.; Gonzalez, D.

    1987-07-01

    A study of the analysis by gas chromatography of aromatic polycyclic hydrocarbons is presented. The separation has been carried out by glass and fused silica capillary column. The limitations and the advantages of the procedure are discussed in terms of separation efficiency, sensitivity and precision. (Author) 17 refs.

  11. Raman spectroscopic measurements of CO2 density: Experimental calibration with high-pressure optical cell (HPOC) and fused silica capillary capsule (FSCC) with application to fluid inclusion observations

    Science.gov (United States)

    Wang, X.; Chou, I.-Ming; Hu, W.; Burruss, R.C.; Sun, Q.; Song, Y.

    2011-01-01

    Raman spectroscopy is a powerful method for the determination of CO2 densities in fluid inclusions, especially for those with small size and/or low fluid density. The relationship between CO2 Fermi diad split (??, cm-1) and CO2 density (??, g/cm3) has been documented by several previous studies. However, significant discrepancies exist among these studies mainly because of inconsistent calibration procedures and lack of measurements for CO2 fluids having densities between 0.21 and 0.75g/cm3, where liquid and vapor phases coexist near room temperature.In this study, a high-pressure optical cell and fused silica capillary capsules were used to prepare pure CO2 samples with densities between 0.0472 and 1.0060g/cm3. The measured CO2 Fermi diad splits were calibrated with two well established Raman bands of benzonitrile at 1192.6 and 1598.9cm-1. The relationship between the CO2 Fermi diad split and density can be represented by: ??=47513.64243-1374.824414????+13.25586152????2-0.04258891551????3 (r2=0.99835, ??=0.0253g/cm3), and this relationship was tested by synthetic fluid inclusions and natural CO2-rich fluid inclusions. The effects of temperature and the presence of H2O and CH4 on this relationship were also examined. ?? 2011 Elsevier Ltd.

  12. Fused silica capillaries with two segments of different internal diameters and inner surface roughnesses prepared by etching with supercritical water and used for volume coupling electrophoresis.

    Science.gov (United States)

    Horká, Marie; Karásek, Pavel; Roth, Michal; Šlais, Karel

    2017-02-22

    In this work, single-piece fused silica capillaries with two different internal diameter segments featuring different inner surface roughness were prepared by new etching technology with supercritical water and used for volume coupling electrophoresis. The concept of separation and online pre-concentration of analytes in high conductivity matrix is based on the online large-volume sample pre-concentration by the combination of transient isotachophoretic stacking and sweeping of charged proteins in micellar electrokinetic chromatography using non-ionogenic surfactant. The modified surface roughness step helped to the significant narrowing of the zones of examined analytes. The sweeping and separating steps were accomplished simultaneously by the use of phosphate buffer (pH 7) containing ethanol, non-ionogenic surfactant Brij 35, and polyethylene glycol (PEG 10000) after sample injection. Sample solution of a large volume (maximum 3.7 μL) dissolved in physiological saline solution was injected into the wider end of capillary with inlet inner diameter from 150, 185 or 218 μm. The calibration plots were linear (R(2) ∼ 0.9993) over a 0.060-1 μg/mL range for the proteins used, albumin and cytochrome c. The peak area RSDs from at least 20 independent measuremens were below 3.2%. This online pre-concentration technique produced a more than 196-fold increase in sensitivity, and it can be applied for detection of, e.g. the presence of albumin in urine (0.060 μg/mL).

  13. Hybrid integrated PDMS microfluidics with a silica capillary.

    Science.gov (United States)

    Dimov, Ivan K; Riaz, Asif; Ducrée, Jens; Lee, Luke P

    2010-06-07

    To harness the properties of both PDMS and silica, we have demonstrated hybrid integrated PDMS microfluidic systems with fused silica capillaries. The hybrid integrated PDMS microfluidics and silica capillary (iPSC) modules exhibit a novel architecture and method for leakage free CE sample injection merely requiring a single high voltage source and one pair of electrodes. The use of the iPSC device is based on a modular approach which allows the capillary to be reused extensively whilst replacing the attached fluidic module for different experiments. Integrating fused silica capillaries with PDMS microfluidic modules allows the direct application of a wide variety of well established conventional CE protocols for separations of complex analytes. Furthermore it bears the potential for facile coupling to standard electro-spray ionization mass spectrometry (ESI-MS), letting users focus on the sample analysis rather than the development of new separation protocols. The fabrication of the iPSC module consists of a simple and quick three-step method that submerges a fused silica capillary in PDMS prepolymer. After cross linking the prepolymer and punching the inlets, the iPSC module layer can be mounted onto a microfluidic device for CE separation.

  14. Fused silica windows for solar receiver applications

    Science.gov (United States)

    Hertel, Johannes; Uhlig, Ralf; Söhn, Matthias; Schenk, Christian; Helsch, Gundula; Bornhöft, Hansjörg

    2016-05-01

    A comprehensive study of optical and mechanical properties of quartz glass (fused silica) with regard to application in high temperature solar receivers is presented. The dependence of rupture strength on different surface conditions as well as high temperature is analyzed, focussing particularly on damage by devitrification and sandblasting. The influence of typical types of contamination in combination with thermal cycling on the optical properties of fused silica is determined. Cleaning methods are compared regarding effectiveness on contamination-induced degradation for samples with and without antireflective coating. The FEM-aided design of different types of receiver windows and their support structure is presented. A large-scale production process has been developed for producing fused silica dome shaped windows (pressurized window) up to a diameter of 816 mm. Prototypes were successfully pressure-tested in a test bench and certified according to the European Pressure Vessel Directive.

  15. Gel electrophoresis in a polyvinylalcohol coated fused silica capillary for purity assessment of modified and secondary-structured oligo- and polyribonucleotides.

    Science.gov (United States)

    Barciszewska, Martyna; Sucha, Agnieszka; Bałabańska, Sandra; Chmielewski, Marcin K

    2016-01-18

    Application of a polyvinylalcohol-coated (PVA-coated) capillary in capillary gel electrophoresis (CGE) enables the selective separation of oligoribonucleotides and their modifications at high resolution. Quality assessment of shorter oligomers of small interfering RNA (siRNA) is of key importance for ribonucleic acid (RNA) technology which is increasingly being applied in medical applications. CGE is a technique of choice for calculation of chemically synthesized RNAs and their modifications which are frequently obtained as a mixture including shorter oligoribonucleotides. The use of CGE with a PVA-coated capillary to analyze siRNA mixtures presents an alternative to conventionally employed techniques. Here, we present study on identification of the length and purity of RNA mixture ingredients by using PVA-coated capillaries. Also, we demonstrate the use of PVA-coated capillaries to identify and separate phosphorylated siRNAs and secondary structures (e.g. siRNA duplexes).

  16. Electrostatic Discharge Properties of Fused Silica Coatings

    Science.gov (United States)

    Andersen, Allen; Sim, Charles; Dennison, J. R.

    2012-10-01

    The electric field value at which electrostatic discharge (ESD) occurs was studied for thin coatings of fused silica (highly disordered SiO2/SiOx) on conductive substrates, such as those encountered as optical coatings and in Si microfabrication. The electrostatic breakdown field was determined using an increasing voltage, while monitoring the leakage current. A simple parallel-plate capacitor geometry was used, under medium vacuum and at temperatures down to ˜150 K using a liquid N2 reservoir. The breakdown field, pre-breakdown arcing and I-V curves for fused silica samples are compared for ˜60 nm and ˜80 μm thick, room and low temperature, and untreated and irradiated samples. Unlike typical I-V results for polymeric insulators, the thin film silica samples did not exhibit pre-breakdown arcing, displayed transitional resistivity after initial breakdown, and in many cases showed evidence of a second discontinuity in the I-V curves. This diversity of observed discharge phenomena is discussed in terms of breakdown modes and defect generation on a microscopic scale.

  17. Quartz/fused silica chip carriers

    Science.gov (United States)

    1992-01-01

    The primary objective of this research and development effort was to develop monolithic microwave integrated circuit (MMIC) packaging which will operate efficiently at millimeter-wave frequencies. The packages incorporated fused silica as the substrate material which was selected due to its favorable electrical properties and potential performance improvement over more conventional materials for Ka-band operation. The first step towards meeting this objective is to develop a package that meets standard mechanical and thermal requirements using fused silica and to be compatible with semiconductor devices operating up to at least 44 GHz. The second step is to modify the package design and add multilayer and multicavity capacity to allow for application specific integrated circuits (ASIC's) to control multiple phase shifters. The final step is to adapt the package design to a phased array module with integral radiating elements. The first task was a continuation of the SBIR Phase 1 work. Phase 1 identified fused silica as a viable substrate material by demonstrating various plating, machining, and adhesion properties. In Phase 2 Task 1, a package was designed and fabricated to validate these findings. Task 2 was to take the next step in packaging and fabricate a multilayer, multichip module (MCM). This package is the predecessor to the phased array module and demonstrates the ability to via fill, circuit print, laminate, and to form vertical interconnects. The final task was to build a phased array module. The radiating elements were to be incorporated into the package instead of connecting to it with wire or ribbon bonds.

  18. Laser Damage Precursors in Fused Silica

    Energy Technology Data Exchange (ETDEWEB)

    Miller, P; Suratwala, T; Bude, J; Laurence, T A; Shen, N; Steele, W A; Feit, M; Menapace, J; Wong, L

    2009-11-11

    There is a longstanding, and largely unexplained, correlation between the laser damage susceptibility of optical components and both the surface quality of the optics, and the presence of near surface fractures in an optic. In the present work, a combination of acid leaching, acid etching, and confocal time resolved photoluminescence (CTP) microscopy has been used to study laser damage initiation at indentation sites. The combination of localized polishing and variations in indentation loads allows one to isolate and characterize the laser damage susceptibility of densified, plastically flowed and fractured fused silica. The present results suggest that: (1) laser damage initiation and growth are strongly correlated with fracture surfaces, while densified and plastically flowed material is relatively benign, and (2) fracture events result in the formation of an electronically defective rich surface layer which promotes energy transfer from the optical beam to the glass matrix.

  19. Fused silica challenges in sensitive space applications

    Science.gov (United States)

    Criddle, Josephine; Nürnberg, Frank; Sawyer, Robert; Bauer, Peter; Langner, Andreas; Schötz, Gerhard

    2016-07-01

    Space bound as well as earthbound spectroscopy of extra-terrestrial objects finds its challenge in light sources with low intensities. High transmission for every optical element along the light path requires optical materials with outstanding performance to enable the measurement of even a one-photon event. Using the Lunar Laser Ranging Project and the LIGO and VIRGO Gravitational Wave Detectors as examples, the influence of the optical properties of fused silica will be described. The Visible and Infrared Surveillance Telescope for Astronomy (VISTA) points out the material behavior in the NIR regime, where the chemical composition of optical materials changes the performance. Special fibers are often used in combination with optical elements as light guides to the spectroscopic application. In an extended spectral range between 350 and 2,200 nm Heraeus developed STU fiber preforms dedicated for broad band spectroscopy in astronomy. STU fibers in the broad spectral range as well as SSU fibers for UV transmission (180 - 400 nm) show also high gamma radiation resistance which allows space applications.

  20. Quantification of residual stress from photonic signatures of fused silica

    Science.gov (United States)

    Cramer, K. Elliott; Hayward, Maurice; Yost, William T.

    2014-02-01

    A commercially available grey-field polariscope (GFP) instrument for photoelastic examination is used to assess impact damage inflicted upon the outer-most pane of Space Shuttle windows made from fused silica. A method and apparatus for calibration of the stress-optic coefficient using four-point bending is discussed. The results are validated on known material (acrylic) and are found to agree with literature values to within 6%. The calibration procedure is then applied to fused-silica specimens and the stress-optic coefficient is determined to be 2.43 ± 0.54 × 10-12 Pa-1. Fused silica specimens containing impacts artificially made at NASA's Hypervelocity Impact Technology Facility (HIT-F), to simulate damage typical during space flight, are examined. The damage sites are cored from fused silica window carcasses and examined with the GFP. The calibrated GFP measurements of residual stress patterns surrounding the damage sites are presented.

  1. Effects of Vacuum of Fused Silica UV Damage

    Institute of Scientific and Technical Information of China (English)

    XU Shi-Zhen; LV Hai-Bing; YUAN Xiao-Dong; HUANG Jin; JIANG Xiao-Dong; WANG Hai-Jun; ZU Xiao-Tao; ZHENG Wan-Guo

    2008-01-01

    Damage points induced by 355 nm laser irradiation increase more quickly on the surface of fused silica in vacuum of about 10-3Pa than in atmospheric air at the same fluence.The larger concentration of point defects in vacuum is confirmed by photoluminescence intensity.X-ray photoelectron spectroscopy and infrared absorption indicate the formation of sub-stoichiometric sillca on the surface.The degradation mechanism of fused silica in vacuum is discussed.

  2. Global equation of state for a glassy material: Fused silica

    Energy Technology Data Exchange (ETDEWEB)

    Boettger, J.C.

    1994-09-01

    A new SESAME equation of state (EOS) for fused silica has been generated using the computer program GRIZZLY and will be added to the SESAME library as material number 7387. This new EOS provides better agreement with experimental data than was achieved by all previous SESAME EOSs for fused silica. Material number 7387 also constitutes the most realistic SESAME-type EOS generated for any glassy material thus far.

  3. Modified monolithic silica capillary for preconcentration of catecholamines

    Institute of Scientific and Technical Information of China (English)

    Wei Chang; Tusyo-shi Komazu

    2009-01-01

    Preconcentration of catecholamines by the modified monolithic silica in the capillary was investigated in this study. In order to achieve a microchip-based method for determining catecholamines in the saliva, the monolithic silica was fabricated in the capillary and the monolithic silica was chemically modified by on-column reaction with phenylboronate. Different modified methods were compared. The concentration conditions were optimized. This study indicates the applicability of the modified monolithic silica capillary when it was used to concentrate catecholamines.

  4. Quantification of Residual Stress from Photonic Signatures of Fused Silica

    Science.gov (United States)

    Cramer, K. Elliott; Hayward, Maurice; Yost, William E.

    2013-01-01

    A commercially available grey-field polariscope (GFP) instrument for photoelastic examination is used to assess impact damage inflicted upon the outer-most pane of Space Shuttle windows made from fused silica. A method and apparatus for calibration of the stress-optic coefficient using four-point bending is discussed. The results are validated on known material (acrylic) and are found to agree with literature values to within 6%. The calibration procedure is then applied to fused-silica specimens and the stress-optic coefficient is determined to be 2.43 +/- 0.54 x 10(exp -12)/Pa. Fused silica specimens containing impacts artificially made at NASA's Hypervelocity Impact Technology Facility (HIT-F), to simulate damage typical during space flight, are examined. The damage sites are cored from fused silica window carcasses and examined with the GFP. The calibrated GFP measurements of residual stress patterns surrounding the damage sites are presented. Keywords: Glass, fused silica, photoelasticity, residual stress

  5. Photopolymerization of acrylamide as a new functionalization way of silica monoliths for hydrophilic interaction chromatography and coated silica capillaries for capillary electrophoresis.

    Science.gov (United States)

    El-Debs, R; Marechal, A; Dugas, V; Demesmay, C

    2014-01-24

    A simple, rapid and localizable photochemical process for the preparation of hydrophilic coated capillary and silica-based monolithic capillary columns is described. The process involves the free radical polymerization of acrylamide monomers onto acrylate pre-activated silica surface triggered by UV photoinitiation. The experimental conditions (monomer content, time of irradiation) were optimized on silica monolithic columns by monitoring the evolution of the chromatographic properties (retention, permeability, efficiency) in HILIC mode using a set of nucleosides as test solutes. Compared to thermal polymerization process, the photoinitiation allows the preparation of highly retentive and efficient HILIC monolithic columns in less than 10min of irradiation. This process was then successfully applied to the surface coating of fused silica capillary walls. In addition to its relative high stability and ability to reduce the electroosmotic flow, this polyacrylamide coating is localizable. Benefits of this localizable photochemical process are highlighted through the conception of an in-line integrated bimodal microseparation tool combining a SPE preconcentration step on a photografted silica monolith and an electrokinetic separation step in a polyacrylamide photopolymerized capillary section. Two neuropeptides are used as model solutes to illustrate the suitability of this approach.

  6. 一种新型人工“流体包裹体”:融合二氧化硅毛细管技术%A new synthetic "fluid inclusion": The technique of optical fused silica capillary

    Institute of Scientific and Technical Information of China (English)

    倪培; 丁俊英; I-Ming Chou; Jean Dubessy

    2011-01-01

    利用融合二氧化硅毛细管技术制作了纯H2O体系、纯CO2体系、H2O-NaCl体系和H2O-CO2体系的人工包裹体样品,并对样品进行了显微测温和激光拉曼光谱测试工作。实验结果显示毛细管样品中的流体成分具有代表性,而且常规的流体包裹体显微测温和显微激光拉曼光谱分析技术完全适于毛细管样品的测试。对样品的显微测温和拉曼光谱研究结果表明毛细管样品能够作为标样,标定流体包裹体显微测温过程中的流体相变以及流体包裹体拉曼光谱,而且能够发展和建立拉曼光谱分析流体包裹体成分的方法。此次工作表明,融合二氧化硅毛细管技术为流体包裹体研究提供了一种新的手段,在包裹体研究领域有着广阔的应用前景。%Synthetic fluid inclusions in the systems of pure H2O,of pure CO2,of H2O-NaCl and of H2O-CO2 were made using the technique of optical fused silica capillary.Those capillary samples were analyzed by micro-thermometry and micro-spectroscopy.The experiment shows that the fluids in silica capillary are the representative of loading fluids,and the micro-thermometry and micro-spectroscopy,the two common approaches for measuring the fluid inclusion,are suitable to be applied to the analysis of capillary samples.The micro-thermometric and micro-spectroscopic results reveal that the technique of silica capillary gives us a better means to understand the phase equilibria during the progress of micro-thermometry and to characterize the spectra of inclusion fluids and to develop the methods of analyzing the fluid inclusion.This study demonstrates that the technique of optical fused silica capillary provides a new means for the study of fluid inclusion,which may be widely applied to the fluid inclusion study.

  7. Modified monolithic silica capillary for preconcentration of catecholamines

    Institute of Scientific and Technical Information of China (English)

    2009-01-01

    Preconcentration of catecholamines by the modified monolithic silica in the capillary was investigated in this study. In order to achieve a microchip-based method for determining catecholamines in the saliva,the monolithic silica was fabricated in the capillary and the monolithic silica was chemically modified by on-column reaction with phenylboronate. Different modified methods were compared. The concentration conditions were optimized. This study indicates the applicability of the modified monolithic sili...

  8. Fused silica suspension for the VIRGO optics: status and perspectives

    CERN Document Server

    Amico, P; Carbone, L; Gammaitoni, L; Punturo, M; Travasso, F; Vocca, H

    2002-01-01

    Thermal noise in mirror suspension wires is the main limitation of low-frequency sensitivity of interferometric gravitational wave detectors. In order to minimize the pendulum thermal noise, a monolithic design, using a low dissipation material, is proposed for VIRGO. High mechanical Qs and high breaking strengths have been obtained for monolithic fused silica fibres. A low-dissipation and high-strength bonding technique using potassium silicate bonding is proposed.

  9. Nanodrilling of fused silica using nanosecond laser radiation

    Energy Technology Data Exchange (ETDEWEB)

    Lorenz, P., E-mail: pierre.lorenz@iom-leipzig.de; Zajadacz, J.; Bayer, L.; Ehrhardt, M.; Zimmer, K.

    2015-10-01

    Graphical abstract: - Highlights: • Low-fluence irradiation of 10 nm Mo on SiO{sub 2} results in the formation of Mo droplets. • High-fluence irradiation of droplets results in the formation of holes in the SiO{sub 2}. • The process allows the formation of randomly distributed and periodic holes. • The randomly distributed hole density ρ{sub h} depends on the fluence (ρ{sub h} ≤ 1.3 μm{sup −2}). • The interaction of the laser beam with Mo/SiO{sub 2} was simulated by FEM. - Abstract: The fast laser drilling of dielectric surfaces with hole diameters in the sub-μm range and a high aspect ratio is a challenge for laser methods. In this study, a novel laser structuring method for the production of randomly and periodically distributed holes in a fused silica surface will be presented using a self-assembling process. A fused silica surface was covered with a 10 nm thick magnetron-sputtered molybdenum film. The metal film was irradiated by a KrF excimer laser (wavelength λ = 248 nm, pulse duration Δt{sub p} = 25 ns) with low laser fluences (Φ < 1 J/cm{sup 2}) and the laser-induced heating resulting in a melting of the metal film and finally in a self-assembled formation of randomly distributed metal droplets due to the surface tension of the metal liquid phase using a top hat beam profile. Furthermore, the usage of a periodically modulated laser beam profile allows the fabrication of periodically distributed droplet pattern. The multi-pulse irradiation of the laser-generated metal droplets with higher laser fluences results in a stepwise evaporation of the metal and in a partial evaporation of the fused silica near the metal droplets. Finally, the laser-induced stepwise evaporation process results in a formation of cone-like holes in the fused silica surface where the resultant holes are dependent on the size of the generated metal droplets and on the laser parameters. The “drilling” process allows the fabrication of holes with a depth up to 1

  10. Optimized condition for etching fused-silica phase gratings with inductively coupled plasma technology.

    Science.gov (United States)

    Wang, Shunquan; Zhou, Changhe; Ru, Huayi; Zhang, Yanyan

    2005-07-20

    Polymer deposition is a serious problem associated with the etching of fused silica by use of inductively coupled plasma (ICP) technology, and it usually prevents further etching. We report an optimized etching condition under which no polymer deposition will occur for etching fused silica with ICP technology. Under the optimized etching condition, surfaces of the fabricated fused silica gratings are smooth and clean. Etch rate of fused silica is relatively high, and it demonstrates a linear relation between etched depth and working time. Results of the diffraction of gratings fabricated under the optimized etching condition match theoretical results well.

  11. Threats to ICF reactor materials: computational simulations of radiation damage induced topological changes in fused silica

    CERN Document Server

    Kubota, A; Stolken, J; Sadigh, B; Reyes, S; Rubia, T D; Latkowski, J F

    2003-01-01

    We have performed molecular dynamics simulations of radiation damage in fused silica. In this study, we discuss the role of successive cascade overlap on the saturation and self-healing of oxygen vacancy defects in the amorphous fused silica network. Furthermore, we present findings on the topological changes in fused silica due to repeated energetic recoil atoms. These topological network modifications consistent with experimental Raman spectroscopic observation on neutron and ion irradiated fused silica are indicators of permanent densification that has also been observed experimentally.

  12. Thermal annealing of laser damage precursors on fused silica surfaces

    Energy Technology Data Exchange (ETDEWEB)

    Shen, N; Miller, P E; Bude, J D; Laurence, T A; Suratwala, T I; Steele, W A; Feit, M D; Wang, L L

    2012-03-19

    Previous studies have identified two significant precursors of laser damage on fused silica surfaces at fluenes below {approx} 35 J/cm{sup 2}, photoactive impurities in the polishing layer and surface fractures. In the present work, isothermal heating is studied as a means of remediating the highly absorptive, defect structure associated with surface fractures. A series of Vickers indentations were applied to silica surfaces at loads between 0.5N and 10N creating fracture networks between {approx} 10{micro}m and {approx} 50{micro}m in diameter. The indentations were characterized prior to and following thermal annealing under various times and temperature conditions using confocal time-resolved photo-luminescence (CTP) imaging, and R/1 optical damage testing with 3ns, 355nm laser pulses. Significant improvements in the damage thresholds, together with corresponding reductions in CTP intensity, were observed at temperatures well below the glass transition temperature (T{sub g}). For example, the damage threshold on 05.N indentations which typically initiates at fluences <8 J/cm{sup 2} could be improved >35 J/cm{sup 2} through the use of a {approx} 750 C thermal treatment. Larger fracture networks required longer or higher temperature treatment to achieve similar results. At an annealing temperature > 1100 C, optical microscopy indicates morphological changes in some of the fracture structure of indentations, although remnants of the original fracture and significant deformation was still observed after thermal annealing. This study demonstrates the potential of using isothermal annealing as a means of improving the laser damage resistance of fused silica optical components. Similarly, it provides a means of further understanding the physics associated with optical damage and related mitigation processes.

  13. Laser smoothing of sub-micron grooves in hydroxyl-rich fused silica

    Energy Technology Data Exchange (ETDEWEB)

    Shen, N; Matthews, M J; Fair, J E; Britten, J A; Nguyen, H T; Cooke, D; Elhadj, S; Yang, S T

    2009-10-30

    Nano- to micrometer-sized surface defects on UV-grade fused silica surfaces are known to be effectively smoothed through the use of high-temperature localized CO{sub 2} laser heating, thereby enhancing optical properties. However, the details of the mass transport and the effect of hydroxyl content on the laser smoothing of defective silica at submicron length scales is still not completely understood. In this study, we examine the morphological evolution of sub-micron, dry-etched periodic surface structures on type II and type III SiO{sub 2} substrates under 10.6 {micro}m CO{sub 2} laser irradiation using atomic force microscopy (AFM). In-situ thermal imaging was used to map the transient temperature field across the heated region, allowing assessment of the T-dependent mass transport mechanisms under different laser-heating conditions. Computational fluid dynamics simulations correlated well with experimental results, and showed that for large effective capillary numbers (N{sub c} > 2), surface diffusion is negligible and smoothing is dictated by capillary action, despite the relatively small spatial scales studied here. Extracted viscosity values over 1700-2000K were higher than the predicted bulk values, but were consistent with the surface depletion of OH groups, which was confirmed using confocal Raman microscopy.

  14. Note: Discharging fused silica test masses with ionized nitrogen

    Science.gov (United States)

    Ugolini, D.; Funk, Q.; Amen, T.

    2011-04-01

    We have developed a technique for discharging fused silica test masses in a gravitational-wave interferometer with nitrogen ionized by an electron beam. The electrons are produced from a heated filament by thermionic emission in a low-pressure region to avoid contamination and burnout. Some electrons then pass through a small aperture and ionize nitrogen in a higher-pressure region, and this ionized gas is pumped across the test mass surface, neutralizing both polarities of charge. The discharge rate varies exponentially with charge density and filament current, quadratically with filament potential, and has an optimal working pressure of ˜8 mT. Adapting the technique to larger test mass chambers is also discussed.

  15. Fabrication of microchannels in fused silica using femtosecond Bessel beams

    Energy Technology Data Exchange (ETDEWEB)

    Yashunin, D. A., E-mail: yashuninda@yandex.ru [Institute of Applied Physics of the Russian Academy of Sciences, 46 Ulyanov Str., Nizhny Novgorod 603950 (Russian Federation); Nizhny Novgorod State Technical University, 24 Minin St., Nizhny Novgorod 603950 (Russian Federation); Malkov, Yu. A. [Institute of Applied Physics of the Russian Academy of Sciences, 46 Ulyanov Str., Nizhny Novgorod 603950 (Russian Federation); Mochalov, L. A.; Stepanov, A. N. [Institute of Applied Physics of the Russian Academy of Sciences, 46 Ulyanov Str., Nizhny Novgorod 603950 (Russian Federation); Nizhny Novgorod State Technical University, 24 Minin St., Nizhny Novgorod 603950 (Russian Federation); Lobachevsky State University of Nizhny Novgorod, 23 Gagarin Ave., Nizhny Novgorod 603950 (Russian Federation)

    2015-09-07

    Extended birefringent waveguiding microchannels up to 15 mm long were created inside fused silica by single-pulse irradiation with femtosecond Bessel beams. The birefringent refractive index change of 2–4 × 10{sup −4} is attributed to residual mechanical stress. The microchannels were chemically etched in KOH solution to produce 15 mm long microcapillaries with smooth walls and a high aspect ratio of 1:250. Bessel beams provide higher speed of material processing compared to conventional multipulse femtosecond laser micromachining techniques and permit simple control of the optical axis direction of the birefringent waveguides, which is important for practical applications [Corrielli et al., “Rotated waveplates in integrated waveguide optics,” Nat. Commun. 5, 4249 (2014)].

  16. Characterization of the polishing induced contamination of fused silica optics

    Science.gov (United States)

    Pfiffer, Mathilde; Longuet, Jean-Louis; Labrugère, Christine; Fargin, Evelyne; Bousquet, Bruno; Dussauze, Marc; Lambert, Sébastien; Cormont, Philippe; Néauport, Jérôme

    2016-12-01

    Secondary Ion Mass Spectroscopy (SIMS), Electron Probe Micro Analysis (EPMA) and X-Ray Photoelectron Spectroscopy (XPS) were used to analyze the polishing induced contamination layer at the fused silica optics surface. Samples were prepared using an MRF polishing machine and cerium-based slurry. The cerium and iron penetration and concentration were measured in the surface out of defects. Cerium is embedded at the surface in a 60 nm layer and concentrated at 1200 ppmw in this layer while iron concentration falls down at 30 nm. Spatial distribution and homogeneity of the pollution were also studied in scratches and bevel using SIMS and EPMA techniques. An overconcentration was observed in the chamfer and we saw evidence that surface defects such as scratches are specific places that hold the pollutants. A wet etching was able to completely remove the contamination in the scratch.

  17. Surface initiated polymerization of a cationic monomer on inner surfaces of silica capillaries: analyte separation by capillary electrophoresis versus polyelectrolyte behavior.

    Science.gov (United States)

    Witos, Joanna; Karesoja, Mikko; Karjalainen, Erno; Tenhu, Heikki; Riekkola, Marja-Liisa

    2013-03-01

    [2-(Methacryloyl)oxyethyl]trimethylammonium chloride was successfully polymerized by surface-initiated atom transfer radical polymerization method on the inner surface of fused-silica capillaries resulting in a covalently bound poly([2-(methacryloyl)oxyethyl]trimethylammonium chloride) coating. The coated capillaries provided in capillary electrophoresis an excellent run-to-run repeatability, capillary-to-capillary and day-to-day reproducibility. The capillaries worked reliably over 1 month with EOF repeatability below 0.5%. The positively charged coated capillaries were successfully applied to the capillary electrophoretic separation of three standard proteins and five β-blockers with the separation efficiencies ranging from 132,000 to 303,000 plates/m, and from 82,000 to 189,000 plates/m, respectively. In addition, challenging high- and low-density lipoprotein particles could be separated. The hydrodynamic sizes of free polymer chains in buffers used in the capillary electrophoretic experiments were measured for the characterization of the coatings.

  18. Indirect slumping of D263 glass on Fused Silica mould

    Science.gov (United States)

    Proserpio, Laura; Wen, Mingwu; Breunig, Elias; Burwitz, Vadim; Friedrich, Peter; Madarasz, Emanuel

    2016-07-01

    The Slumped Glass Optic (SGO) group of the Max Planck Institute for Extraterrestrial physics (MPE) is studying the indirect slumping technology for its application to X-ray telescope manufacturing. Several aspects of the technology have been analyzed in the past. During the last months, we concentrated our activities on the slumping of Schott D263 glass on a precise machined Fused Silica mould: The concave mould was produced by the Italian company Media Lario Technologies with the parabola and hyperbola side of the typical Wolter I design in one single piece. Its shape quality was estimated by optical metrology to be around 6 arcsec Half Energy Width (HEW) in double reflection. The application of an anti-sticking Boron Nitride layer was necessary to avoid the adhesion of the glass on the mould during the forming process at high temperatures. The mould has been used for the slumping of seven mirror segments 200 mm long, 100 mm wide, and with thickness of 200 μm or 400 μm. The influence of the holding time at maximum temperature was explored in this first run of tests. The current results of the activities are described in the paper and plans for further investigations are outlined.

  19. The compaction of fused silica resulting from ion implantation

    Energy Technology Data Exchange (ETDEWEB)

    Johnson, C.M.; Ridgway, M.C. [Australian National Univ., Canberra, ACT (Australia); Leech, P.L. [Telstra Research Laboratories, Clayton, Victoria (Australia)

    1996-12-31

    Ion implantation of fused silica results in compaction and consequently an increase in refractive index. This method of modifying the near-surface region has been shown as a potential means for fabricating single mode channel waveguides. This study has measured the compaction of the implanted regions for Si implantations as a function of dose (2x10{sup 12} - 6x10{sup l6} ions/cm{sup 2}), energy (1-9 MeV) and post-implantation annealing temperature (200-900 degree C). For a given energy, a dose-dependence of the step height (depth of compacted region) is observed for doses less than {approx}10{sup 15} ions/cm{sup 2}. At higher doses the step height saturates. For a given dose, a linear trend is evident for the step height as a function of energy suggesting that the major mechanism for this compaction is electronic stopping. As the annealing temperature increases, the step height gradually decreases from {approx}0.1-0.2 {mu} to -10-20% of the original value. From the annealing data, it is possible to extract an activation energy of 0.08 eV associated with the thermal removal of the compacted region. 4 refs., 4 figs.

  20. Mitigation of organic laser damage precursors from chemical processing of fused silica.

    Science.gov (United States)

    Baxamusa, S; Miller, P E; Wong, L; Steele, R; Shen, N; Bude, J

    2014-12-01

    Increases in the laser damage threshold of fused silica have been driven by the successive elimination of near-surface damage precursors such as polishing residue, fractures, and inorganic salts. In this work, we show that trace impurities in ultrapure water used to process fused silica optics may be responsible for the formation of carbonaceous deposits. We use surrogate materials to show that organic compounds precipitated onto fused silica surfaces form discrete damage precursors. Following a standard etching process, solvent-free oxidative decomposition using oxygen plasma or high-temperature thermal treatments in air reduced the total density of damage precursors to as low as inorganic compounds are more likely to cause damage when they are tightly adhered to a surface, which may explain why high-temperature thermal treatments have been historically unsuccessful at removing extrinsic damage precursors from fused silica.

  1. Effects of humidity on the interaction between a fused silica test mass and an electrostatic drive

    Energy Technology Data Exchange (ETDEWEB)

    Koptsov, D.V., E-mail: kopcov@physics.msu.ru; Prokhorov, L.G.; Mitrofanov, V.P.

    2015-10-23

    Interaction of a fused silica test mass with electric field of an electrostatic drive with interdigitated electrodes and influence of ambient air humidity on this interaction are investigated. The key element of the experimental setup is the fused silica torsional oscillator. Time dependent increase of the torque acting on the oscillator's plate after application of DC voltage to the drive is demonstrated. The torque relaxation is presumably caused by the redistribution of electric charges on the fused silica plate. The numerical model has been developed to compute the time evolution of the plate's surface charge distribution and the corresponding torque. - Highlights: • Interaction between a fused silica plate and an electrostatic drive was investigated. • The interaction force is time and relative humidity dependent. • Numerical model of the interaction was developed. • Charge redistribution is shown to be the cause of the interaction force evolution.

  2. Search for stress dependence in the internal friction of fused silica

    Energy Technology Data Exchange (ETDEWEB)

    Willems, Phil; Lamb, Corinne; Heptonstall, Alastair; Hough, Jim

    2003-12-01

    The quality factor (Q) of the vertical bounce mode of a fused silica fiber pendulum is measured at high and low stresses. The internal friction of fused silica fibers is found to be independent of stress from 12.8 to 213 MPa at a level of 1.6x10{sup -8}. Comparison with Q's of fiber bending modes is consistent with losses concentrated in the surface of the fiber.

  3. Search for stress dependence in the internal friction of fused silica

    Science.gov (United States)

    Willems, Phil; Lamb, Corinne; Heptonstall, Alastair; Hough, Jim

    2003-12-01

    The quality factor ( Q) of the vertical bounce mode of a fused silica fiber pendulum is measured at high and low stresses. The internal friction of fused silica fibers is found to be independent of stress from 12.8 to 213 MPa at a level of 1.6×10 -8. Comparison with Q's of fiber bending modes is consistent with losses concentrated in the surface of the fiber.

  4. Effect of Sintering Temperature on the Properties of Fused Silica Ceramics Prepared by Gelcasting

    Science.gov (United States)

    Wan, Wei; Huang, Chun-e.; Yang, Jian; Zeng, Jinzhen; Qiu, Tai

    2014-07-01

    Fused silica ceramics were fabricated by gelcasting, by use of a low-toxicity N' N-dimethylacrylamide gel system, and had excellent properties compared with those obtained by use of the low-toxicity 2-hydroxyethyl methacrylate and toxic acrylamide systems. The effect of sintering temperature on the microstructure, mechanical and dielectric properties, and thermal shock resistance of the fused silica ceramics was investigated. The results showed that sintering temperature has a critical effect. Use of an appropriate sintering temperature will promote densification and improve the strength, thermal shock resistance, and dielectric properties of fused silica ceramics. However, excessively high sintering temperature will greatly facilitate crystallization of amorphous silica and result in more cristobalite in the sample, which will cause deterioration of these properties. Fused silica ceramics sintered at 1275°C have the maximum flexural strength, as high as 81.32 MPa, but, simultaneously, a high coefficient of linear expansion (2.56 × 10-6/K at 800°C) and dramatically reduced residual flexural strength after thermal shock (600°C). Fused silica ceramics sintered at 1250°C have excellent properties, relatively high and similar flexural strength before (67.43 MPa) and after thermal shock (65.45 MPa), a dielectric constant of 3.34, and the lowest dielectric loss of 1.20 × 10-3 (at 1 MHz).

  5. Photothermal microscopic studies of surface and subsurface defects on fused silica at 355nm

    Science.gov (United States)

    Chen, Jian; Dong, Jingtao; Zhang, Qi; Wu, Zhouling

    2014-10-01

    It is believed that surface and subsurface defects formed during standard grinding and polishing processes are mainly responsible for laser induced damage in fused silica. The correlation between the laser damage susceptibility and absorption property of these defects has not been totally understood. In this paper, we present the characterization of surface and subsurface defects of fused silica by measuring their absorption properties based on a photothermal technique at 355 nm. The photothermal microscopic imaging reveals that the surface/subsurface absorption defects in fused silica can be identified. In addition, a 3D photothermal imaging of a laser damage site on the silica is also obtained. Our results demonstrate that photothermal microscopy is a powerful tool for defect characterization of optical materials for high power laser applications.

  6. Densification and Devitrification of Fused Silica Induced by Ballistic Impact: A Computational Investigation

    Directory of Open Access Journals (Sweden)

    Mica Grujicic

    2015-01-01

    Full Text Available A molecular-level computational investigation is carried out to determine the dynamic response and material topology changes of fused silica subjected to ballistic impact by a hard projectile. The analysis was focused on the investigation of specific aspects of the dynamic response and of the topological changes such as the deformation of highly sheared and densified regions, and the conversion of amorphous fused silica to SiO2 crystalline polymorphs (in particular, α-quartz and stishovite. The topological changes in question were determined by carrying out a postprocessing atom-coordination procedure. This procedure suggested the formation of stishovite (and perhaps α-quartz within fused silica during ballistic impact. To rationalize the findings obtained, the all-atom molecular-level computational analysis is complemented by a series of quantum-mechanics density functional theory (DFT computations. The latter computations enable determination of the relative potential energies of the fused silica, α-quartz and stishovite, under ambient pressure (i.e., under their natural densities as well as under imposed (as high as 50 GPa pressures (i.e., under higher densities and shear strains. In addition, the transition states associated with various fused-silica devitrification processes were identified. The results obtained are found to be in good agreement with their respective experimental counterparts.

  7. On the mechanical quality factors of cryogenic test masses from fused silica and crystalline quartz

    CERN Document Server

    Schroeter, Anja; Schnabel, Roman; Reid, Stuart; Martin, Iain; Rowan, Sheila; Schwarz, Christian; Koettig, Torsten; Neubert, Ralf; Thürk, Matthias; Vodel, Wolfgang; Tünnermann, Andreas; Danzmann, Karsten; Seidel, Paul

    2007-01-01

    Current interferometric gravitational wave detectors (IGWDs) are operated at room temperature with test masses made from fused silica. Fused silica shows very low absorption at the laser wavelength of 1064 nm. It is also well suited to realize low thermal noise floors in the detector signal band since it offers low mechanical loss, i. e. high quality factors (Q factors) at room temperature. However, for a further reduction of thermal noise, cooling the test masses to cryogenic temperatures may prove an interesting technique. Here we compare the results of Q factor measurements at cryogenic temperatures of acoustic eigenmodes of test masses from fused silica and its crystalline counterpart. Our results show that the mechanical loss of fused silica increases with lower temperature and reaches a maximum at 30 K for frequencies of slightly above 10 kHz. The losses of crystalline quartz generally show lower values and even fall below the room temperature values of fused silica below 10 K. Our results show that in ...

  8. Nanosecond laser nanostructuring of fused silica surfaces assisted by a chromium triangle template

    Science.gov (United States)

    Lorenz, P.; Grüner, C.; Frost, F.; Ehrhardt, M.; Zimmer, K.

    2017-10-01

    The well-reproducible, fast and cost-effective nanostructuring is a big challenge for laser methods. The laser nanostructuring of fused silica assisted by chromium nanotriangles was studied using a KrF excimer laser (λ = 248 nm, Δtp = 25 ns, top hat beam profile). Therefore, a fused silica substrate was covered with periodically ordered polystyrene (PS) spheres with a diameter of 1.59 μm. Subsequently, this system was covered with 30 nm chromium by electron beam evaporation. Afterwards the PS spheres were removed and the bare and resultant periodic Cr triangles were irradiated. The laser irradiation with high laser fluences resulted in a removal of the chromium and in localized modifications of the fused silica like a localized ablation of the fused silica. The resultant structures were studied by scanning electron (SEM) and atomic force microscopy (AFM) as well as the surface composition was analysed by energy-dispersive X-ray spectroscopy (EDX). The laser process allows the production of well-defined periodic hole structures into the fused silica surface where the resultant surface structure depends on the laser parameters. The multi-pulse irradiation of the Cr/SiO2 sample with moderate laser fluences (Φ ∼ 650 mJ/cm2) allows the fabrication of periodic pyramidal-like structures (depth Δz = 130 nm).

  9. Applying Fused Silica and Other Transparent Window Materials in Aerospace Applications

    Science.gov (United States)

    Salem, Jon

    2017-01-01

    A variety of transparent ceramics, such as AlONs and spinels, that were developed for military applications hold promise as spacecraft windows. Window materials in spacecraft such as the Space Shuttle must meet many requirements such as maintaining cabin pressure, sustaining thermal shock, and tolerating damage from hyper-velocity impact while providing superior optical characteristics. The workhorse transparent material for space missions from Apollo to the International Space Station has been fused silica due in part to its low density, low coefficient of expansion and optical quality. Despite its successful use, fused silica exhibits lower fracture toughness and impact resistance as compared to newer materials. Can these newer transparent ceramics lighten spacecraft window systems and might they be useful for applications such as phone screens? This presentation will compare recent optical ceramics to fused silica and demonstrate how weight can be saved.

  10. Laser-Induced Damage Growth on Larger-Aperture Fused Silica Optical Components at 351 nm

    Institute of Scientific and Technical Information of China (English)

    HUANG Wan-Qing; ZHANG Xiao-Min; HAN Wei; WANG Fang; XIANG Yong; LI Fu-Quan; FENG Bin; JING Feng; WEI Xiao-Feng; ZHENG Wan-Guo

    2009-01-01

    Laser-induced damage is a key lifetime limiter for optics in high-power laser facility. Damage initiation and growth under 351 nm high-fluence laser irradiation are observed on larger-aperture fused silica optics. The input surface of one fused silica component is damaged most severely and an explanation is presented. Obscurations and the area of a scratch on it are found to grow exponentially with the shot number. The area of damage site grows linearly. Micrographs of damage sites support the micro-explosion damage model which could be used to qualitatively explain the phenomena.

  11. Development of a Process Model for CO(2) Laser Mitigation of Damage Growth in Fused Silica

    Energy Technology Data Exchange (ETDEWEB)

    Feit, M D; Rubenchik, A M; Boley, C; Rotter, M D

    2003-11-01

    A numerical model of CO{sub 2} laser mitigation of damage growth in fused silica has been constructed that accounts for laser energy absorption, heat conduction, radiation transport, evaporation of fused silica and thermally induced stresses. This model will be used to understand scaling issues and effects of pulse and beam shapes on material removal, temperatures reached and stresses generated. Initial calculations show good agreement of simulated and measured material removal. The model has also been applied to LG-770 glass as a prototype red blocker material.

  12. Structural Modifications in Fused Silica Due to Laser Damage Induced Shock Compression

    Energy Technology Data Exchange (ETDEWEB)

    Kubota, A; Davila, L; Caturla, M J; Stolken, J S; Sadigh, B; Quong, A; Rubenchik, A; Feit, M D

    2001-12-05

    High power laser pulses can produce damage in high quality fused silica optics that can lead to its eventual obscuration and failure. Current models suggest the initiation of a plasma detonation due to absorbing initiators and defects, leading to the formation of shock waves. Recent experiments have found a densified layer at the bottom of damage sites, as evidence of the laser-damage model. We have studied the propagation of shock waves through fused silica using molecular dynamics. These simulations show drastic modifications in the structure and topology of the network, in agreement with experimental observations.

  13. Simulation of Light Intensification Induced by Defects of Polished Fused Silica

    Institute of Scientific and Technical Information of China (English)

    WANG Feng-Rui; LIU Hong-Jie; HUANG Jin; ZHOU Xin-Da; JIANG Xiao-Dong; WU Wei-Dong; ZHENG Wan-Guo; JU Xin

    2011-01-01

    Light intensity distribution in the vicinity of inclusions and etched cracks in polished fused silica at wavelength scale are simulated by using the finite-difference time-domain algorithm. Light intensity enhancement factor as functions of diameter and refractive index of inclusions are investigated, more than 10 times that of incident beam is obtained in the simulation. We model the etched crack in close proximity to a real structure, which is characterized by AFM. We find that the peak light intensity of the crack is a function of its cross sectional breadth depth ratio, providing good hints for the effective processing of fused silica samples to improve the damage threshold.

  14. Rapidly removing grinding damage layer on fused silica by inductively coupled plasma processing

    Science.gov (United States)

    Chen, Heng; Zhou, Lin; Xie, Xuhui; Shi, Baolu; Xiong, Haobin

    2016-10-01

    During the conventional optical shaping process of fused silica, lapping is generally used to remove grinding damage layer. But this process is of low efficiency, it cannot meet the demand of large aperture optical components. Therefore, Inductively Coupled Plasma Processing (ICPP) was proposed to remove grinding damage layer instead of lapping. ICPP is a non-contact, deterministic figuring technology performed at atmospheric pressure. The process benefits from its ability to simultaneously remove sub-surface damage (SSD) while imparting the desired figure to the surface with high material remove rate. The removing damage capability of ICPP has preliminarily been confirmed on medium size optical surfaces made of fused silica, meanwhile serious edge warping was found. This paper focused on edge effect and a technique has been designed to compensate for these difficulties. Then it was demonstrated on a large aperture fused silica mirror (Long320mm×Wide370mm×High50mm), the removal depth was 30.2μm and removal rate got 6.6mm3/min. The results indicate that ICPP can rapidly remove damage layer on the fused silica induced by the previous grinding process and edge effect is effective controlled.

  15. Wear and mechanical properties of nano-silica-fused whisker composites.

    Science.gov (United States)

    Xu, H H K; Quinn, J B; Giuseppetti, A A

    2004-12-01

    Resin composites must be improved if they are to overcome the high failure rates in large stress-bearing posterior restorations. This study aimed to improve wear resistance via nano-silica-fused whiskers. It was hypothesized that nano-silica-fused whiskers would significantly improve composite mechanical properties and wear resistance. Nano-silicas were fused onto whiskers and incorporated into a resin at mass fractions of 0%-74%. Fracture toughness (mean +/- SD; n = 6) was 2.92 +/- 0.14 MPa.m(1/2) for whisker composite with 74% fillers, higher than 1.13 +/- 0.19 MPa.m(1/2) for a prosthetic control, and 0.95 +/- 0.11 MPa.m(1/2) for an inlay/onlay control (Tukey's at 0.95). A whisker composite with 74% fillers had a wear depth of 77.7 +/- 6.9 mum, less than 118.0 +/- 23.8 microm of an inlay/onlay control, and 172.5 +/- 15.4 microm of a prosthetic control (p hardness, modulus, strength, and toughness, with R = 0.95-0.97. Novel nano-silica-fused whisker composites possessed high toughness and wear resistance with smooth worn surfaces, and may be useful in large stress-bearing restorations.

  16. Bulk damage and absorption in fused silica due to high-power laser applications

    Science.gov (United States)

    Nürnberg, F.; Kühn, B.; Langner, A.; Altwein, M.; Schötz, G.; Takke, R.; Thomas, S.; Vydra, J.

    2015-11-01

    Laser fusion projects are heading for IR optics with high broadband transmission, high shock and temperature resistance, long laser durability, and best purity. For this application, fused silica is an excellent choice. The energy density threshold on IR laser optics is mainly influenced by the purity and homogeneity of the fused silica. The absorption behavior regarding the hydroxyl content was studied for various synthetic fused silica grades. The main absorption influenced by OH vibrational excitation leads to different IR attenuations for OH-rich and low-OH fused silica. Industrial laser systems aim for the maximum energy extraction possible. Heraeus Quarzglas developed an Yb-doped fused silica fiber to support this growing market. But the performance of laser welding and cutting systems is fundamentally limited by beam quality and stability of focus. Since absorption in the optical components of optical systems has a detrimental effect on the laser focus shift, the beam energy loss and the resulting heating has to be minimized both in the bulk materials and at the coated surfaces. In collaboration with a laser research institute, an optical finisher and end users, photo thermal absorption measurements on coated samples of different fused silica grades were performed to investigate the influence of basic material properties on the absorption level. High purity, synthetic fused silica is as well the material of choice for optical components designed for DUV applications (wavelength range 160 nm - 260 nm). For higher light intensities, e.g. provided by Excimer lasers, UV photons may generate defect centers that effect the optical properties during usage, resulting in an aging of the optical components (UV radiation damage). Powerful Excimer lasers require optical materials that can withstand photon energy close to the band gap and the high intensity of the short pulse length. The UV transmission loss is restricted to the DUV wavelength range below 300 nm and

  17. Ionoluminescence of fused silica under swift ion irradiation

    Energy Technology Data Exchange (ETDEWEB)

    Saavedra, R. [Fusion Materials Research Unit, National Fusion Laboratory, CIEMAT, Av Complutense, 40, 28040 Madrid (Spain); Jiménez-Rey, D. [Fusion Materials Research Unit, National Fusion Laboratory, CIEMAT, Av Complutense, 40, 28040 Madrid (Spain); Centre for Micro Analysis of Materials, Universidad Autónoma de Madrid, Cantoblanco, 28049 Madrid (Spain); Martin, P.; Vila, R. [Fusion Materials Research Unit, National Fusion Laboratory, CIEMAT, Av Complutense, 40, 28040 Madrid (Spain)

    2016-09-01

    Highlights: • Irradiation with He{sup +} ions (lowest stopping power) shows highest luminescence. • Silica with highest OH content presents the lowest blue luminescence. • Electronic excitation was the predominant process of energy transfer. • Surface cracks were observed in Si or O irradiated samples at low fluence. • Blue IL maximum for O and Si irradiated samples is related to structural changes. - Abstract: Ion beam induced luminescence spectra have been in-situ recorded during He{sup +} (2.5 MeV), O{sup 4+} (13.5 MeV) and Si{sup 4+} (24.4 MeV) irradiations for three vitreous silica grades with different OH content (KU1, KS-4V and Infrasil 301). Remarkable changes in the ionoluminescence spectra of the three silica grades were observed for low ion fluences. He{sup +} irradiated samples exhibited higher luminescence than equivalent ones irradiated with heavier O{sup 4+} and Si{sup 4+} ions. KU1 samples with the highest OH content showed the lowest blue luminescence. Blue luminescence maximum during ion irradiations with O{sup 4+} and Si{sup 4+} ions is correlated with structural changes.

  18. Evolution of Oxygen Deficiency Center on Fused Silica Surface Irradiated by Ultraviolet Laser and Posttreatment

    Directory of Open Access Journals (Sweden)

    Hai-Bing Lü

    2014-01-01

    Full Text Available Evolution of oxygen deficiency centers (ODCs on a fused silica surface irradiated using a 355 nm ultraviolet (UV laser beam in both vacuum and atmospheric conditions was quantitatively studied using photoluminescence and X-ray photoelectron spectroscopy. When the fusedsilica surface was exposed to the UV laser in vacuum, the laser damage threshold was decreased whereas the concentration of the ODCs was increased. For the fuse silica operated under the high power lasers, creation of ODCs on their surface resulted from the UV laser irradiation, and this is more severe in a high vacuum. The laser fluence and/or laser intensity have significant effects on the increase of the ODCs concentration. The ODCs can be effectively repaired using postoxygen plasma treatment and UV laser irradiation in an excessive oxygen environment. Results also demonstrated that the “gain” and “loss” of oxygen at the silica surface is a reversible and dynamic process.

  19. Advanced Mitigation Process (AMP) for Improving Laser Damage Threshold of Fused Silica Optics

    Science.gov (United States)

    Ye, Xin; Huang, Jin; Liu, Hongjie; Geng, Feng; Sun, Laixi; Jiang, Xiaodong; Wu, Weidong; Qiao, Liang; Zu, Xiaotao; Zheng, Wanguo

    2016-08-01

    The laser damage precursors in subsurface of fused silica (e.g. photosensitive impurities, scratches and redeposited silica compounds) were mitigated by mineral acid leaching and HF etching with multi-frequency ultrasonic agitation, respectively. The comparison of scratches morphology after static etching and high-frequency ultrasonic agitation etching was devoted in our case. And comparison of laser induce damage resistance of scratched and non-scratched fused silica surfaces after HF etching with high-frequency ultrasonic agitation were also investigated in this study. The global laser induce damage resistance was increased significantly after the laser damage precursors were mitigated in this case. The redeposition of reaction produce was avoided by involving multi-frequency ultrasonic and chemical leaching process. These methods made the increase of laser damage threshold more stable. In addition, there is no scratch related damage initiations found on the samples which were treated by Advanced Mitigation Process.

  20. One step physically adsorbed coating of silica capillary with excellent stability for the separation of basic proteins by capillary zone electrophoresis.

    Science.gov (United States)

    Guo, Xiao-Feng; Guo, Xiao-Mei; Wang, Hong; Zhang, Hua-Shan

    2015-11-01

    The coating of capillary inner surface is considered to be an effective approach to suppress the adsorption of proteins on capillary inner surface in CE. However, most of coating materials reported are water-soluble, which may dissolve in BGE during the procedure of electrophoresis. In this study, a novel strategy for selection of physically coating materials has been illustrated to get coating layer with excellent stability using materials having poor solubility in commonly used solvents. Taking natural chitin as example (not hydrolyzed water soluble chitosan), a simple one step coating method using chitin solution in hexafluoroisopropanol was adopted within only 21 min with good coating reproducibility (RSDs of EOF for within-batch coated capillaries of 1.55% and between-batch coated capillaries of 2.31%), and a separation of four basic proteins on a chitin coated capillary was performed to evaluate the coating efficacy. Using chitin coating, the adsorption of proteins on capillary inner surface was successfully suppressed with reversed and stable EOF, and four basic proteins including lysozyme, cytochrome c, ribonuclease A and α-chymotrypsinogen A were baseline separated within 16 min with satisfied separation efficiency using 20 mM pH 2.0 H3PO4-Na2HPO4 as back ground electrolyte and 20 kV as separation voltage. What is more important, the chitin coating layer could be stable for more than two months during this study, which demonstrates that chitin is an ideal material for preparing semi-permanent coating on bare fused silica capillary inner wall and has hopeful potential in routine separation of proteins with CE.

  1. Thermal transport in CO2 laser irradiated fused silica: In situ measurements and analysis

    Science.gov (United States)

    Yang, Steven T.; Matthews, Manyalibo J.; Elhadj, Selim; Draggoo, Vaughn G.; Bisson, Scott E.

    2009-11-01

    In situ spatial and temporal temperature measurements of pristine fused silica surfaces heated with a 10.6 μm CO2 laser were obtained using an infrared radiation thermometer based on a mercury cadmium telluride camera. Laser spot sizes ranged from 250 to 1000 μm diameter with peak axial irradiance levels of 0.13-16 kW/cm2. For temperatures below 2800 K, the measured steady-state surface temperature is observed to rise linearly with both increasing beam size and incident laser irradiance. The effective thermal conductivity estimated over this range was approximately 2 W/m-K, in good agreement with classical calculations based on phonon heat capacities. Similarly, time-dependent temperature measurements up to 2000 K yielded thermal diffusivity values which were close to reported values of 7×10-7 m2/s. Above ˜2800 K, the fused silica surface temperature asymptotically approaches 3100 K as laser power is further increased, consistent with the onset of evaporative heat losses near the silica boiling point. These results show that in the laser heating regime studied here, the T3 temperature dependent thermal conductivity due to radiation transport can be neglected, but at temperatures above 2800 K heat transport due to evaporation must also be considered. The thermal transport in fused silica up to 2800 K, over a range of conditions, can then be adequately described by a linear diffusive heat equation assuming constant thermal properties.

  2. Particle damage sources for fused silica optics and their mitigation on high energy laser systems.

    Science.gov (United States)

    Bude, J; Carr, C W; Miller, P E; Parham, T; Whitman, P; Monticelli, M; Raman, R; Cross, D; Welday, B; Ravizza, F; Suratwala, T; Davis, J; Fischer, M; Hawley, R; Lee, H; Matthews, M; Norton, M; Nostrand, M; VanBlarcom, D; Sommer, S

    2017-05-15

    High energy laser systems are ultimately limited by laser-induced damage to their critical components. This is especially true of damage to critical fused silica optics, which grows rapidly upon exposure to additional laser pulses. Much progress has been made in eliminating damage precursors in as-processed fused silica optics (the advanced mitigation process, AMP3), and very high damage resistance has been demonstrated in laboratory studies. However, the full potential of these improvements has not yet been realized in actual laser systems. In this work, we explore the importance of additional damage sources-in particular, particle contamination-for fused silica optics fielded in a high-performance laser environment, the National Ignition Facility (NIF) laser system. We demonstrate that the most dangerous sources of particle contamination in a system-level environment are laser-driven particle sources. In the specific case of the NIF laser, we have identified the two important particle sources which account for nearly all the damage observed on AMP3 optics during full laser operation and present mitigations for these particle sources. Finally, with the elimination of these laser-driven particle sources, we demonstrate essentially damage free operation of AMP3 fused silica for ten large optics (a total of 12,000 cm(2) of beam area) for shots from 8.6 J/cm(2) to 9.5 J/cm(2) of 351 nm light (3 ns Gaussian pulse shapes). Potentially many other pulsed high energy laser systems have similar particle sources, and given the insight provided by this study, their identification and elimination should be possible. The mitigations demonstrated here are currently being employed for all large UV silica optics on the National Ignition Facility.

  3. Fiber fuse light-induced continuous breakdown of silica glass optical fiber

    CERN Document Server

    Todoroki, Shin-ichi

    2014-01-01

    This book describes the fiber fuse phenomenon that causes a serious problem for the present optical communication systems. High-power light often brings about catastrophic damage to optical devices. Silica glass optical fibers with ultralow transmission loss are not the exception. A fiber fuse appears in a heated region of the fiber cable delivering a few watts of light and runs toward the light source destroying its core region. Understanding this phenomenon is a necessary first step in the development of future optical communication systems. This book provides supplementary videos and photog

  4. The size prediction of potential inclusions embedded in the sub-surface of fused silica by damage morphology

    Directory of Open Access Journals (Sweden)

    Gao Xiang

    2017-04-01

    Full Text Available A model for predicting the size ranges of different potential inclusions initiating damage on the surface of fused silica has been presented. This accounts for the heating of nanometric inclusions whose absorptivity is described based on Mie Theory. The depth profile of impurities has been measured by ICP-OES. By the measured temporal pulse profile on the surface of fused silica, the temperature and thermal stress has been calculated. Furthermore, considering the limit conditions of temperature and thermal stress strength for different damage morphologies, the size range of potential inclusions for fused silica is discussed.

  5. UV-induced modification of fused silica: Insights from ReaxFF-based molecular dynamics simulations

    Science.gov (United States)

    Tian, Ye; Du, Jincheng; Zu, Xiaotao; Han, Wei; Yuan, Xiaodong; Zheng, Wanguo

    2016-09-01

    Atomic structural modification and defect processes of fused silica resulting from UV-laser irradiation are studied by a combination of molecular dynamics (MD) simulations and the Reactive Force Field (ReaxFF). Bond state transitions by laser excitation are modeled as the result of localized recoils during energy deposition. Computations of pair distribution functions and bond angle distributions of the irradiated structure reveal that fused silica undergoes significant changes in terms of Si-O, Si-Si pair distances and Si-O-Si bond angles, which are attributed to the formation of silicon and oxygen coordination defects. It is found that nonbridging oxygen is responsible for the decreased Si-O bond length, while laser-induced five-coordinated silicon leads to small Si-O-Si bond angles in 2-membered rings.

  6. Viscosity of fused silica and thermal noise from the standard linear solid model

    Science.gov (United States)

    Kondratiev, N. M.; Gorodetsky, M. L.

    2016-10-01

    The fluctuation-dissipation theorem states that each source of dissipation yields corresponding fluctuations. The most obvious source of dissipation in liquids is viscosity—internal friction between layers of matter. However, this property also exists in solid materials in a glass state, i.e., an amorphous substance that cannot become a crystal due to high viscosity. Fused silica is a low-loss glass material used in many interferometric applications demanding high stability, such as Fabry-Perot etalons and gravitational-wave detector mirrors and suspensions. Very high viscosity (from 1 017 to 1 040 Pa s in the literature) can be the source of additional noise and can influence the performance of such devices. We show that fused silica may be described with the standard linear solid model of viscoelastisity and present a method to estimate this type of noise.

  7. Microwave interrogated large core fused silica fiber Michelson interferometer for strain sensing.

    Science.gov (United States)

    Hua, Liwei; Song, Yang; Huang, Jie; Lan, Xinwei; Li, Yanjun; Xiao, Hai

    2015-08-20

    A Michelson-type large core optical fiber sensor has been developed, which is designed based on the optical carrier-based microwave interferometry technique, and fabricated by using two pieces of 200-μm diameter fused silica core fiber as two arms of the Michelson interferometer. The interference fringe pattern caused by the optical path difference of the two arms is interrogated in the microwave domain, where the fringe visibility of 40 dB has easily been obtained. The strain sensing at both room temperature and high temperatures has been demonstrated by using such a sensor. Experimental results show that this sensor has a linear response to the applied strain, and also has relatively low temperature-strain cross talk. The dopant-free quality of the fused silica fiber provides high possibility for the sensor to have promising strain sensing performance in a high temperature environment.

  8. Birefringence and residual stress induced by CO2 laser mitigation of damage growth in fused silica

    Science.gov (United States)

    Gallais, L.; Cormont, P.; Rullier, J. L.

    2009-10-01

    We investigate the residual stress field created near mitigated sites and its influence on the efficiency on the CO2 laser mitigation of damage growth process. A numerical model of CO2 laser interaction with fused silica is developed that take into account laser energy absorption, heat transfer, thermally-induced stress and birefringence. Specific photoelastic methods are developed to characterize the residual stress near mitigated sites in fused silica samples. The stress distribution and quantitative values of stress levels are obtained for sites treated with the CO2 laser in various conditions of energy deposition (beam size, pulse duration, incident power). The results obtained also show that the presence of birefringence/residual stress around the mitigated sites has a critical effect on their laser damage resistance.

  9. Studies on transmitted beam modulation effect from laser induced damage on fused silica optics.

    Science.gov (United States)

    Zheng, Yi; Ma, Ping; Li, Haibo; Liu, Zhichao; Chen, Songlin

    2013-07-15

    UV laser induced damage (LID) on exit surface of fused silica could cause modulation effect to transmitted beam and further influence downstream propagation properties. This paper presents our experimental and analytical studies on this topic. In experiment, a series of measurement instruments are applied, including beam profiler, interferometer, microscope, and optical coherent tomography (OCT). Creating and characterizing of LID on fused silica sample have been implemented. Morphological features are studied based on their particular modulation effects on transmitted beam. In theoretical investigation, analytical modeling and numerical simulation are performed. Modulation effects from amplitude, phase, and size factors are analyzed respectively. Furthermore, we have novelly designed a simplified polygon model to simulate actual damage site with multiform modulation features, and the simulation results demonstrate that the modeling is usable and representative.

  10. Resonance Fluorescence of Fused Silica by the Depopulation of the Ground State

    Directory of Open Access Journals (Sweden)

    Fuat Bayrakceken

    2012-01-01

    Full Text Available Spectroscopically pure fused silica has been used in many applications ranging from optoelectronics and optical fibers to laser flash spectroscopy. Although ultraviolet light irradiated optical absorption spectra and coherence fluorescence of silicon dioxide have been studied in the past, we present discrete absorption and resonance coherent fluorescence line of silicon dioxide which were recorded photographically at 288.2 nm. This discrete fluorescence is observed at room temperature using high photon flux (1024 photon/pulse excitation spectroscopy.

  11. Form control in atmospheric pressure plasma processing of ground fused silica

    Science.gov (United States)

    Li, Duo; Wang, Bo; Xin, Qiang; Jin, Huiliang; Wang, Jun; Dong, Wenxia

    2014-08-01

    Atmospheric Pressure Plasma Processing (APPP) using inductively coupled plasma has demonstrated that it can achieve comparable removal rate on the optical surface of fused silica under the atmosphere pressure and has the advantage of inducing no sub-surface damage for its non-contact and chemical etching mechanism. APPP technology is a cost effective way, compared with traditional mechanical polishing, magnetorheological finishing and ion beam figuring. Thus, due to these advantages, this technology is being tested to fabricate large aperture optics of fused silica to help shorten the polishing time in optics fabrication chain. Now our group proposes to use inductively coupled plasma processing technology to fabricate ground surface of fused silica directly after the grinding stage. In this paper, form control method and several processing parameters are investigated to evaluate the removal efficiency and the surface quality, including the robustness of removal function, velocity control mode and tool path strategy. However, because of the high heat flux of inductively coupled plasma, the removal depth with time can be non-linear and the ground surface evolvement will be affected. The heat polishing phenomenon is founded. The value of surface roughness is reduced greatly, which is very helpful to reduce the time of follow-up mechanical polishing. Finally, conformal and deterministic polishing experiments are analyzed and discussed. The form error is less 3%, before and after the APPP, when 10μm depth of uniform removal is achieved on a 60×60mm ground fused silica. Also, a basin feature is fabricated to demonstrate the figuring capability and stability. Thus, APPP is a promising technology in processing the large aperture optics.

  12. Measurement of initial absorption of fused silica at 193nm using laser induced deflection technique (LID)

    Science.gov (United States)

    Schönfeld, Dörte; Klett, Ursula; Mühlig, Christian; Thomas, Stephan

    2008-01-01

    The ongoing development in microlithography towards further miniaturization of structures creates a strong demand for lens material with nearly ideal optical properties. Beside the highly demanding requirements on homogeneity and stress induced birefringence (SIB), low absorption is a key factor. Even a small absorption is associated with a temperature increase and results in thermally induced local variations of refractive index and SIB. This could affect the achievable resolution of the lithographic process. The total absorption of the material is composed of initial absorption and of absorption induced during irradiation. Thus, the optimization of both improves the lifetime of the material. In principal, it is possible to measure transmission and scattering with a suitable spectrometer assembly and calculate absorption from them. However, owing to the influence of sample surfaces and errors of measurement, these methods usually do not provide satisfactory results for highly light-transmissive fused silica. Therefore, it is most desirable to find a technique that is capable of directly measuring absorption coefficients in the range of (1...10)•10 -4 cm -1 (base 10) directly. We report our first results for fused silica achieved with the LID technique. Besides a fused silica grade designed for 193 nm applications, grades with higher absorption at 193 nm were measured to test the LID technique. A special focus was set on the possibility of measuring initial absorption without the influence of degradation effects.

  13. Pattern transfer on fused silica samples using sub-aperture reactive ion beam etching

    Energy Technology Data Exchange (ETDEWEB)

    Miessler, Andre; Arnold, Thomas [Leibniz-Institut fuer Oberflaechenmodifizierung (IOM), Permoserstrasse 15, D-04318 Leipzig (Germany)

    2012-07-01

    In comparison to sole Ar ion beam sputtering Reactive Ion Beam Etching (RIBE) reveals the main advantage of increasing the selectivity for different kind of materials due to chemical contributions during the material removal. Therefore RIBE is qualified to be an excellent candidate for pattern transfer applications. The goal of the present study is to apply a sub-aperture reactive ion beam for pattern transfer on large fused silica samples. Concerning this matter, the etching behavior in the ion beam periphery plays a decisive role. Using a Kaufman-typed ion source with NF{sub 3} as reactive gas, XPS measurements of the modified surface exposes impurities like Ni, Fe and Cr, which belongs to chemically eroded material of the plasma pot and a layer formation of silicon nitride, handicaps the etching process mainly in the beam periphery where the sputtering contribution decrease. These side effects influence the pattern transfer of trench structures, produced in AZ MIR 701 photoresist by lithography on a 2'' fused silica plate, by changing the selectivity due to modified chemical reactions of the resist layer. Concerning this we investigate a RF-Ion source for sub aperture reactive ion beam applications and finally we examine the pattern transfer on large fused silica plates using NF{sub 3}-sub-aperture RIBE.

  14. Single-Molecule Imaging of DNAs with Sticky Ends at Water/Fused Silica Interface

    Energy Technology Data Exchange (ETDEWEB)

    Isailovic, Slavica [Iowa State Univ., Ames, IA (United States)

    2005-01-01

    Total internal reflection fluorescence microscopy (TIRFM) was used to study intermolecular interactions of DNAs with unpaired (sticky) ends of different lengths at water/fused silica interface at the single-molecule level. Evanescent field residence time, linear velocity and adsorption/desorption frequency were measured in a microchannel for individual DNA molecules from T7, Lambda, and PSP3 phages at various pH values. The longest residence times and the highest adsorption/desorption frequencies at the constant flow at pH 5.5 were found for PSP3 DNA, followed by lower values for Lambda DNA, and the lowest values for T7 DNA. Since T7, Lambda, and PSP3 DNA molecules contain none, twelve and nineteen unpaired bases, respectively, it was concluded that the affinity of DNAs for the surface increases with the length of the sticky ends. This confirms that hydrophobic and hydrogen-bonding interactions between sticky ends and fused-silica surface are driving forces for DNA adsorption at the fused-silica surface. Described single-molecule methodology and results therein can be valuable for investigation of interactions in liquid chromatography, as well as for design of DNA hybridization sensors and drug delivery systems.

  15. Optical properties in the Cu-fused silica system irradiated with swift heavy ions

    Energy Technology Data Exchange (ETDEWEB)

    Gupta, Ranjana C. [Department of Physics, University of Mumbai, Vidyanagari, Santacruz East, Mumbai 400 098 (India); Kothari, D.C. [Department of Physics, University of Mumbai, Vidyanagari, Santacruz East, Mumbai 400 098 (India)]. E-mail: kothari@mu.ac.in; Choudhari, R.J. [Nuclear Science Centre, P.O. Box 10502, Aruna Asaf Ali Marg, New Delhi 110 067 (India); Kumar, Ravi [Nuclear Science Centre, P.O. Box 10502, Aruna Asaf Ali Marg, New Delhi 110 067 (India); Sahoo, P.K. [II. Physikalisches Institut, Universitaet Goettingen, Friedrich-Hund-Platz 1, D-37077 Goettingen (Germany); Lieb, K.P. [II. Physikalisches Institut, Universitaet Goettingen, Friedrich-Hund-Platz 1, D-37077 Goettingen (Germany); Klaumuenzer, S. [Hahn-Meitner Institut, Glienicker Str. 100, D-14109 Berlin (Germany)

    2006-04-15

    Swift heavy ions are used to study the effects of electronic energy loss on Cu cluster formation in fused silica after post-irradiation annealing. Fused silica substrates covered with 10 nm thin Cu-films were irradiated using beams of either 120 MeV Ag{sup 9+} ions or 350 MeV Au{sup 26+} ions at fluences ranging from 2 x 10{sup 13} to 1 x 10{sup 14} cm{sup -2}. After irradiation, the samples were annealed for 30 min in argon, at temperatures of 773-1200 K and characterized by UV-VIS absorption spectroscopy. The swift ion irradiations created E' and B{sub 2} defects in silica, which were partially eliminated during annealing. In addition, Cu cluster formation in silica was observed after annealing. Irradiation fluences exceeding 4 x 10{sup 13} cm{sup -2} and annealing temperatures above 1100 K are more effective in forming larger nanoclusters.

  16. Surface roughening of ground fused silica processed by atmospheric inductively coupled plasma

    Energy Technology Data Exchange (ETDEWEB)

    Xin, Qiang; Li, Na; Wang, Jun; Wang, Bo, E-mail: bradywang@hit.edu.cn; Li, Guo; Ding, Fei; Jin, Huiliang

    2015-06-30

    Highlights: • The morphology evolution of ground fused silica, processed by atmospheric plasma, was investigated experimentally. • The roughness development results from opening and coalescing of the plasma-etched cracks. • The shapes of grain-like etched pits are the results of the adjacent cracks coalescing with one another. • The descent of the pits density is due to some smaller etched pits that are swallowed up by larger pits. • Leading role in surface smoothing is laterally etching away the side walls of the intersecting pits. - Abstract: Subsurface damage (SSD) is a defect that is inevitably induced during mechanical processes, such as grinding and polishing. This defect dramatically reduces the mechanical strength and the laser damage thresholds of optical elements. Compared with traditional mechanical machining, atmospheric pressure plasma processing (APPP) is a relatively novel technology that induces almost no SSD during the processing of silica-based optical materials. In this paper, a form of APPP, inductively coupled plasma (ICP), is used to process fused silica substrates with fluorocarbon precursor under atmospheric pressure. The surface morphology evolution of ICP-processed substrates was observed and characterized by confocal laser scanning microscope (CLSM), field emission scanning electron microscope (SEM), and atomic force microscopy (AFM). The results show that the roughness evolves with the etching depth, and the roughness evolution is a single-peaked curve. This curve results from the opening and the coalescing of surface cracks and fractures. The coalescence procedure of these microstructures was simulated with two common etched pits on a polished fused silica surface. Understanding the roughness evolution of plasma-processed surface might be helpful in optimizing the optical fabrication chain that contains APPP.

  17. Thermal transport in CO2 laser irradiated fused silica: in situ measurements and analysis

    Energy Technology Data Exchange (ETDEWEB)

    Yang, S T; Matthews, M J; Elhadj, S; Draggoo, V G; Bisson, S E

    2009-07-07

    In situ spatial and temporal temperature measurements of pristine fused silica surfaces heated with a 10.6 {micro}m CO{sub 2} laser were obtained using an infrared radiation thermometer based on a Mercury Cadmium Telluride (MCT) camera. Laser spot sizes ranged from 250 {micro}m to 1000 {micro}m diameter with peak axial irradiance levels of 0.13 to 16 kW/cm{sup 2}. For temperatures below 2800K, the measured steady-state surface temperature is observed to rise linearly with both increasing beam size and incident laser irradiance. The effective thermal conductivity estimated over this range was approximately 2W/mK, in good agreement with classical calculations based on phonon heat capacities. Similarly, time-dependent temperature measurements up to 2000K yielded thermal diffusivity values which were close to reported values of 7 x 10{sup -7} m{sup 2}/s. Above {approx}2800K, the fused silica surface temperature asymptotically approaches 3100K as laser power is further increased, consistent with the onset of evaporative heat losses near the silica boiling point. These results show that in the laser heating regime studied here, the T{sup 3} temperature dependent thermal conductivity due to radiation transport can be neglected, but at temperatures above 2800K heat transport due to evaporation must be considered. The thermal transport in fused silica up to 2800K, over a range of conditions, can then be adequately described by a linear diffusive heat equation assuming constant thermal properties.

  18. Femtosecond laser assisted 3-dimensional freeform fabrication of metal microstructures in fused silica (Conference Presentation)

    Science.gov (United States)

    Ebrahim, Fatmah; Charvet, Raphaël.; Dénéréaz, Cyril; Mortensen, Andreas; Bellouard, Yves

    2017-03-01

    Femtosecond laser exposure of fused silica combined with chemical etching has opened up new opportunities for three-dimensional freeform processing of micro-structures that can form complex micro-devices of silica, integrating optical, mechanical and/or fluidic functionalities. Here, we demontrate an expansion of this process with an additional fabrication step that enables the integration of three-dimensional embedded metallic structures out of useful engineering metals such as silver, gold, copper as well as some of their alloys. This additional step is an adaptation of the pressure infiltration for the insertion of high conductivity, high melting point metals and alloys into topologically complex, femtosecond laser-machined cavities in fused silica. This produces truly 3-dimensional microstructures, including microcoils and needles, within the bulk of glass substrates. Combining this added capability with the existing possibilities of femtosecond laser micromachining (i.e. direct written waveguides, microchannels, resonators, etc.) opens up a host of potential applications for the contactless fabrication of highly integrated monolithic devices that include conductive element of all kind. We present preliminary results from this new fabrication process, including prototype devices that incorporate 3D electrodes with aspect ratios of 1:100 and a feature size resolution down to 2μm. We demonstrate the generation of high electric field gradients (of the order of 1013 Vm-2) in these devices due to the 3-dimensional topology of fabricated microstructures.

  19. Electrical field-induced faceting of etched features using plasma etching of fused silica

    Science.gov (United States)

    Huff, M.; Pedersen, M.

    2017-07-01

    This paper reports a previously unreported anomaly that occurs when attempting to perform deep, highly anisotropic etches into fused silica using an Inductively-Coupled Plasma (ICP) etch process. Specifically, it was observed that the top portion of the etched features exhibited a substantially different angle compared to the vertical sidewalls that would be expected in a typical highly anisotropic etch process. This anomaly has been termed as "faceting." A possible explanation of the mechanism that causes this effect and a method to eradicate it has been developed. Additionally, the method to eliminate the faceting is demonstrated. It is theorized that this faceting is a result of the interaction of the electro-potential electrical fields that surround the patterned nickel layers used as a hard mask and the electrical fields directing the high-energy ions from the plasma to the substrate surface. Based on this theory, an equation for calculating the minimum hard mask thickness required for a desired etch depth into fused silica to avoid faceting was derived. As validation, test samples were fabricated employing hard masks of thicknesses calculated based on the derived equation, and it was found that no faceting was observed on these samples, thereby demonstrating that the solution performed as predicted. Deep highly anisotropic etching of fused silica, as well as other forms of silicon dioxide, including crystalline quartz, using plasma etching, has an important application in the fabrication of several MEMS, NEMS, microelectronic, and photonic devices. Therefore, a method to eliminate faceting is an important development for the accurate control of the dimensions of deep and anisotropic etched features of these devices using ICP etch technology.

  20. Growth of laser damage in fused silica: diameter to depth ratio

    Energy Technology Data Exchange (ETDEWEB)

    Norton, M A; Adams, J J; Carr, C W; Donohue, E E; Feit, M D; Hackel, R P; Hollingsworth, W G; Jarboe, J A; Matthews, M; Rubenchik, A M; Spaeth, M L

    2007-10-29

    Growth of laser initiated damage plays a major role in determining optics lifetime in high power laser systems. Previous measurements have established that the lateral diameter grows exponentially. Knowledge of the growth of the site in the propagation direction is also important, especially so when considering techniques designed to mitigate damage growth, where it is required to reach all the subsurface damage. In this work, we present data on both the diameter and the depth of a growing exit surface damage sites in fused silica. Measured growth rates with both 351 nm illumination and with combined 351 nm and 1054 nm illumination are discussed.

  1. Initiation, Growth and Mitigation of UV Laser Induced Damage in Fused Silica

    Energy Technology Data Exchange (ETDEWEB)

    Rubenchik, A M; Feit, M D

    2001-12-21

    Laser damage of large fused silica optics initiates at imperfections. Possible initiation mechanisms are considered. We demonstrate that a model based on nanoparticle explosions is consistent with the observed initiation craters. Possible mechanisms for growth upon subsequent laser irradiation, including material modification and laser intensification, are discussed. Large aperture experiments indicate an exponential increase in damage size with number of laser shots. Physical processes associated with this growth and a qualitative explanation of self-accelerated growth is presented. Rapid growth necessitates damage growth mitigation techniques. Several possible mitigation techniques are mentioned, with special emphasis on CO{sub 2} processing. Analysis of material evaporation, crack healing, and thermally induced stress are presented.

  2. Initiation, Growth and Mitigation of UV Laser Induced Damage in Fused Silica

    Energy Technology Data Exchange (ETDEWEB)

    Rubenchik, A M; Feit, M D

    2003-06-10

    Laser damage of large fused silica optics initiates at imperfections. Possible initiation mechanisms are considered. We demonstrate that a model based on nanoparticle explosions is consistent with the observed initiation craters. Possible mechanisms for growth upon subsequent laser irradiation, including material modification and laser intensification, are discussed. Large aperture experiments indicate an exponential increase in damage size with number of laser shots. Physical processes associated with this growth and a qualitative explanation of self-accelerated growth is presented. Rapid growth necessitates damage growth mitigation techniques. Several possible mitigation techniques are mentioned, with special emphasis on CO{sub 2} processing. Analysis of material evaporation, crack healing, and thermally induced stress are presented.

  3. Evaluation of UV absorption coefficient in laser-modified fused silica

    Energy Technology Data Exchange (ETDEWEB)

    Negres, R A; Burke, M W; Sutton, S B; DeMange, P; Feit, M D; Demos, S G

    2006-08-21

    Laser-induced damage in transparent dielectrics leads to the formation of laser-modified material as a result of exposure to extreme localized temperatures and pressures. In this work, we used an infrared thermal imaging system in combination with a fluorescence microscope to map the dynamics of the local surface temperature and fluorescence intensity under cw, UV excitation of laser-modified fused silica within a damage site. Based on a thermal diffusion model, we estimate the energy deposited via linear absorption mechanisms and derive the absorption coefficient of the modified material. In addition, irreversible changes in the absorption following extended laser exposure were observed.

  4. Three-dimensional optical storage in fused silica using modulated femtosecond pulses

    Institute of Scientific and Technical Information of China (English)

    Qing Liu(刘青); Guanghua Cheng(程光华); Yishan Wang(王屹山); Zhao Cheng(程昭); Wei Zhao(赵卫); Guofu Chen(陈国夫)

    2004-01-01

    Three-dimensional bitwise optical recording with a density of 500 Gb/cm3 in fused silica using a Ti:sapphire femtosecond laser modulated by binary digits is demonstrated. Laser pulses modulation is realized by modulating two circuits of trigger pulses signal which are used to control laser pulses trapping and switching out from cavity, respectively. Bits are optically readout in both a parallel reading (phase-contrast) and a serial reading (confocal-type) methods. The method for modulating laser pulses can also be used in all of pulsed laser systems which operate in cavity-dumping configuration.

  5. Influence of Ambient Temperature on Nanosecond and Picosecond Laser-Induced Bulk Damage of Fused Silica

    Directory of Open Access Journals (Sweden)

    L. Yang

    2014-01-01

    Full Text Available The nanosecond (ns and picosecond (ps pulsed laser-induced damage behaviors of fused silica under cryogenic and room temperature have been investigated. The laser-induced damage threshold (LIDT and damage probability are used to understand the damage behavior at different ambient temperatures. The results show that the LIDTs for both ns and ps slightly increased at cryogenic temperature compared to that at room temperature. Meanwhile, the damage probability has an inverse trend; that is, the damage probability at low temperature is smaller than that at room temperature. A theoretical model based on heated crystal lattice is well consistent with the experimental results.

  6. Femtosecond laser fabrication of phase-shifted Bragg grating waveguides in fused silica.

    Science.gov (United States)

    Grenier, Jason R; Fernandes, Luís A; Aitchison, J Stewart; Marques, Paulo V S; Herman, Peter R

    2012-06-15

    Phase-shifted Bragg grating waveguides (PSBGWs) were formed in bulk fused silica glass by femtosecond laser direct writing to produce narrowband (22±3)  pm filters at 1550 nm. Tunable π and other phase shifts generated narrow passbands in controlled positions of the Bragg stopband, while the accurate placement of multiple cascaded phase-shift regions yielded a rectangular-shaped bandpass filter. A waveguide birefringence of (7.5±0.3)×10(-5) is inferred from the polarization-induced spectral shifting of the PSBGW narrowband filters.

  7. Femtosecond laser fabrication of birefringent directional couplers as polarization beam splitters in fused silica.

    Science.gov (United States)

    Fernandes, Luís A; Grenier, Jason R; Herman, Peter R; Aitchison, J Stewart; Marques, Paulo V S

    2011-06-20

    Integrated polarization beam splitters based on birefringent directional couplers are demonstrated. The devices are fabricated in bulk fused silica glass by femtosecond laser writing (300 fs, 150 nJ at 500 kHz, 522 nm). The birefringence was measured from the spectral splitting of the Bragg grating resonances associated with the vertically and horizontally polarized modes. Polarization splitting directional couplers were designed and demonstrated with 0.5 dB/cm propagation losses and -19 dB and -24 dB extinction ratios for the polarization splitting.

  8. Femtosecond diffraction dynamics of laser-induced periodic surface structures on fused silica

    Energy Technology Data Exchange (ETDEWEB)

    Hoehm, S.; Rosenfeld, A. [Max-Born-Institut fuer Nichtlineare Optik und Kurzzeitspektroskopie (MBI), Max-Born-Strasse 2A, D-12489 Berlin (Germany); Krueger, J.; Bonse, J. [BAM Bundesanstalt fuer Materialforschung und - pruefung, Unter den Eichen 87, D-12205 Berlin (Germany)

    2013-02-04

    The formation of laser-induced periodic surface structures (LIPSS) on fused silica upon irradiation with linearly polarized fs-laser pulses (50 fs pulse duration, 800 nm center wavelength) is studied experimentally using a transillumination femtosecond time-resolved (0.1 ps-1 ns) pump-probe diffraction approach. This allows to reveal the generation dynamics of near-wavelength-sized LIPSS showing a transient diffraction at specific spatial frequencies even before a corresponding permanent surface relief was observed. The results confirm that the ultrafast energy deposition to the materials surface plays a key role and triggers subsequent physical mechanisms such as carrier scattering into self-trapped excitons.

  9. Laser Mode-Dependent Size of Plasma Zones Induced by Femtosecond Laser Pulses in Fused Silica

    Institute of Scientific and Technical Information of China (English)

    TANG Shan-Chun; JIANG Hong-Bing; LIU Yi; GONG Qi-Huang

    2008-01-01

    We carry out the numerical simulations of #emtosecond laser propagation with TEM00 mode, TEM10 mode and a beam combining both the modes in fused silica. It is found that the transverse size of plasma zones induced by laser pulses with the TEM10 mode is smaller than that induced by the TEMoo mode, while the longitudinal size is almost the same, and the saturated plasma density is higher. The transverse size, the longitudinal size and the ratio of the longitudinal to transverse size, for the beam combining both the modes, all could be reduced at the same time in comparison with the TEMoo mode under the same focusing conditions.

  10. Visible supercontinuum radiation of light bullets in the femtosecond filamentation of IR pulses in fused silica

    Science.gov (United States)

    Chekalin, S. V.; Kompanets, V. O.; Dokukina, A. E.; Dormidonov, A. E.; Smetanina, E. O.; Kandidov, V. P.

    2015-05-01

    We report experimental and theoretical investigations of visible supercontinuum generation in the formation of light bullets in a filament produced by IR pulses. In the filamentation of a 1700 - 2200 nm pulse in fused silica, bright tracks are recorded resulting from the recombination glow of carriers in the laser plasma produced by a sequence of light bullets and from the scattering in silica of the visible supercontinuum generated by the light bullets. It is found that the formation of a light bullet is attended with an outburst of a certain portion of supercontinuum energy in the visible range. The energy outburst is the same for all bullets in the sequence and becomes smaller with increasing pulse wavelength.

  11. Ultraviolet laser-induced damage on fused silica substrate and its sol-gel coating.

    Science.gov (United States)

    Li, Xiaoguang; Gross, Mark; Green, Katie; Oreb, Bob; Shen, Jun

    2012-06-15

    A comparative study of the laser-induced damage thresholds (LIDTs) of fused silica substrates and their sol-gel silica coatings was carried out with 355 nm laser irradiation. Chemical etching and superpolishing were employed in different ways to improve the substrate. The laser damage tests showed that the coated substrate was no more susceptible to laser damage than the bare substrate, showing that the substrate quality was the dominant factor limiting the LIDT for UV irradiation. In addition, it was found that high value of substrate microroughness was more harmful to the LIDT of the coated than the bare substrate, and that a proper combination of etching and superpolishing can optimize the LIDT.

  12. An Improved Method of Mitigating Laser Induced Surface Damage Growth in Fused Silica Using a Rastered, Pulsed CO2 Laser

    Energy Technology Data Exchange (ETDEWEB)

    Bass, I L; Guss, G M; Nostrand, M J; Wegner, P L

    2010-10-21

    A new method of mitigating (arresting) the growth of large (>200 m diameter and depth) laser induced surface damage on fused silica has been developed that successfully addresses several issues encountered with our previously-reported large site mitigation technique. As in the previous work, a tightly-focused 10.6 {micro}m CO{sub 2} laser spot is scanned over the damage site by galvanometer steering mirrors. In contrast to the previous work, the laser is pulsed instead of CW, with the pulse length and repetition frequency chosen to allow substantial cooling between pulses. This cooling has the important effect of reducing the heat-affected zone capable of supporting thermo-capillary flow from scale lengths on the order of the overall scan pattern to scale lengths on the order of the focused laser spot, thus preventing the formation of a raised rim around the final mitigation site and its consequent down-stream intensification. Other advantages of the new method include lower residual stresses, and improved damage threshold associated with reduced amounts of redeposited material. The raster patterns can be designed to produce specific shapes of the mitigation pit including cones and pyramids. Details of the new technique and its comparison with the previous technique will be presented.

  13. Array of chemically etched fused-silica emitters for improving the sensitivity and quantitation of electrospray ionization mass spectrometry.

    Science.gov (United States)

    Kelly, Ryan T; Page, Jason S; Tang, Keqi; Smith, Richard D

    2007-06-01

    An array of emitters has been developed for increasing the sensitivity of electrospray ionization mass spectrometry (ESI-MS). The linear array consists of 19 chemically etched fused-silica capillaries arranged with 500 microm (center-to-center) spacing. The multiemitter device has a low dead volume to facilitate coupling to capillary liquid chromatography (LC) separations. The high aspect ratio of the emitters enables operation at flow rates as low as 20 nL/min/emitter, effectively extending the benefits of nanoelectrospray to higher flow rate analyses. To accommodate the larger ion current produced by the emitter array, a multicapillary inlet to the mass spectrometer was also constructed. The inlet, which matched the dimensions of the emitter array, preserved ion transmission efficiency. Standard reserpine solutions of varying concentration were electrosprayed at 1 microL/min using the multiemitter/multi-inlet combination, and the results were compared to those from a standard, single-emitter configuration. A 9-fold sensitivity enhancement was observed for the multiemitter relative to the single emitter. A bovine serum albumin tryptic digest was also analyzed, and a sensitivity increase ranging from 2.4- to 12.3-fold for the detected tryptic peptides resulted; the varying response was attributed to reduced ion suppression under the nanoESI conditions afforded by the emitter array. An equimolar mixture of leucine enkephalin and maltopentaose was studied to verify that ion suppression is indeed reduced for the multiplexed ESI (multi-ESI) array relative to a single emitter over a range of flow rates.

  14. Large-Scale Synthesis and Systematic Photoluminescence Properties of Monolayer MoS2 on Fused Silica.

    Science.gov (United States)

    Wan, Yi; Zhang, Hui; Zhang, Kun; Wang, Yilun; Sheng, Bowen; Wang, Xinqiang; Dai, Lun

    2016-07-20

    Monolayer MoS2, with fascinating mechanical, electrical, and optical properties, has generated enormous scientific curiosity and industrial interest. Controllable and scalable synthesis of monolayer MoS2 on various desired substrates has significant meaning in both basic scientific research and device application. Recent years have witnessed many advances in the direct synthesis of single-crystalline MoS2 flakes or their polycrystalline aggregates on numerous diverse substrates, such as SiO2-Si, mica, sapphire, h-BN, and SrTiO3, etc. In this work, we used the dual-temperature-zone atmospheric-pressure chemical vapor deposition method to directly synthesize large-scale monolayer MoS2 on fused silica, the most ordinary transparent insulating material in daily life. We systematically investigated the photoluminescence (PL) properties of monolayer MoS2 on fused silica and SiO2-Si substrates, which have different thermal conductivity coefficients and thermal expansion coefficients. We found that there exists a stronger strain on monolayer MoS2 grown on fused silica, and the strain becomes more obvious as temperature decreases. Moreover, the monolayer MoS2 grown on fused silica exhibits the unique trait of a fractal shape with tortuous edges and has stronger adsorbability. The monolayer MoS2 grown on fused silica may find application in sensing, energy storage, and transparent optoelectronics, etc.

  15. Damage in fused-silica spatial-filter lenses on the OMEGA laser system

    Science.gov (United States)

    Rigatti, Amy L.; Smith, Douglas J.; Schmid, Ansgar W.; Papernov, Semyon; Kelly, John H.

    1999-04-01

    Vacuum surface damage to fused-silica, spatial-filter lenses is the most prevalent laser-damage problem occurring on the OMEGA laser system. Approximately one-half of the stage C- input and output, D-input, E-input, and F-input spatial- filter lenses are currently damaged with millimeter-scale fracture sites. With the establishment of safe operational damage criteria, laser operation has not been impeded. These sol-gel-coated lenses see an average fluence of 2 to 4 J/cm2 at 1053 nm/1 ns. Sol-gel coatings on fused-silica glass have small-spot damage thresholds at least a factor of 2 higher than this peak operational fluence. It is now known that the vacuum surface of OMEGA's spatial-filter lenses are contaminated with vacuum pump oils and machine oils used in the manufacture of the tubes; however, development-phase damage tests were conducted on uncontaminated witness samples. Possible explanations for the damage include absorbing defects originating form ablated pinhole materials, contamination nucleated at surface defects on the coating, or subsurface defects from the polishing process. The damage does not correlate with hot spots in the beam, and the possibility of damage from ghost reflections has been eliminated. Experiments have been initiated to investigate the long-term benefits of ion etching to remove subsurface damage and to replace sol-gel layers by dielectric oxide coatings, which do not degrade with oil contamination.

  16. Incident laser modulation of a repaired damage site with a rim in fused silica rear subsurface

    Institute of Scientific and Technical Information of China (English)

    Li Li; Xiang Xia; Zu Xiao-Tao; Yuan Xiao-Dong; He Shao-Bo; Jiang Xiao-Dong; Zheng Wan-Guo

    2012-01-01

    Local CO2 laser treatment has proved to be an effective method to prevent the 351-nm laser-induced damage sitesin a fused silica surface from exponentially growing,which is responsible for limiting the lifetime of optics in high fluence laser systems.However,the CO2 laser induced ablation crater is often surrounded by a raised rim at the edge,which can also result in the intensification of transmitted ultraviolet light that may damage the downstream optics.In this work,the three-dimensional finite-difference time-domain method is developed to simulate the distribution of electrical field intensity in the vicinity of the CO2 laser mitigated damage site located in the exit subsurface of fused silica.The simulated results show that the repaired damage sites with raised rims cause more notable modulation to the incident laser than those without rims.Specifically,we present a theoretical model of using dimpled patterning to control the rim structure around the edge of repaired damage sites to avoid damage to downstream optics.The calculated results accord well with previous experimental results and the underlying physical mechanism is analysed in detail.

  17. Low scatter and ultra-low reflectivity measured in a fused silica window

    CERN Document Server

    Padilla, Cinthia; Muniz, Erik; Smith, Joshua R; Fritschel, Peter; Zhang, Liyuan

    2013-01-01

    We investigate the reflectivity and optical scattering characteristics at 1064\\,nm of an antireflection coated fused silica window of the type being used in the Advanced LIGO gravitational-wave detectors. Reflectivity is measured in the ultra-low range of 5-10\\,ppm (by vendor) and 14-30\\,ppm (by us). Using an angle-resolved scatterometer we measure the sample's Bidirectional Scattering Distribution Function (BSDF) and use this to estimate its transmitted and reflected scatter at roughly 20-40\\,ppm and 1\\,ppm, respectively, over the range of angles measured. We further inspect the sample's low backscatter using an imaging scatterometer, measuring an angle resolved BSDF below $10^{-6}$ sr$^{-1}$ for large angles (10$^\\circ$--80$^\\circ$ from incidence in the plane of the beam). We use the associated images to (partially) isolate scatter from different regions of the sample and find that scattering from the bulk fused silica is on par with backscatter from the antireflection coated optical surfaces. To confirm th...

  18. Downstream Intensification Effects Associated with CO2 Laser Mitigation of Fused Silica

    Energy Technology Data Exchange (ETDEWEB)

    Matthews, M J; Bass, I L; Guss, G M; Widmayer, C C; Ravizza, F L

    2007-10-29

    Mitigation of 351nm laser-induced damage sites on fused silica exit surfaces by selective CO{sub 2} treatment has been shown to effectively arrest the exponential growth responsible for limiting the lifetime of optics in high-fluence laser systems. However, the perturbation to the optical surface profile following the mitigation process introduces phase contrast to the beam, causing some amount of downstream intensification with the potential to damage downstream optics. Control of the laser treatment process and measurement of the associated phase modulation is essential to preventing downstream 'fratricide' in damage-mitigated optical systems. In this work we present measurements of the surface morphology, intensification patterns and damage associated with various CO{sub 2} mitigation treatments on fused silica surfaces. Specifically, two components of intensification pattern, one on-axis and another off-axis can lead to damage of downstream optics and are related to rims around the ablation pit left from the mitigation process. It is shown that control of the rim structure around the edge of typical mitigation sites is crucial in preventing damage to downstream optics.

  19. Effect of the repaired damage morphology of fused silica on the modulation of incident laser

    Science.gov (United States)

    Gao, X.; Jiang, Y.; Qiu, R.; Zhou, Q.; Zuo, R.; Zhou, G. R.; Yao, K.

    2017-02-01

    Local CO2 laser treatment has proved to be the most promising method to extend the life-time of fused silica. However, previous experimental data show that some raised rims are observed around the mitigated sites left from the mitigation process, which will result in hazardous light modulation to the downstream optics. In this work, the morphology features of mitigated sites on the surface of fused silica optics were analyzed in detail. According to measured morphology features, a 3D analytical model for simulating the modulation value induced by mitigated site has been developed based on the scalar diffraction theory. The diffraction patterns at a discrete distance downstream from each mitigated site are measured. The influences of geometry, laser wavelength and refractive index of substrates on the modulation by repaired damage morphology at different distances are discussed, respectively. The analytical model is usable and representative to evaluate the hazardous modulation induced by repaired damage morphology to downstream optics. Results on this research suggest that the downstream intensification can be suppressed by controlling the morphology features of mitigated sites, which provides a direction for the development and improvement of the mitigated techniques of damage optics.

  20. Micro Fluidic Channel Machining on Fused Silica Glass Using Powder Blasting

    Directory of Open Access Journals (Sweden)

    Dong-Sam Park

    2008-02-01

    Full Text Available In this study, micro fluid channels are machined on fused silica glass via powder blasting, a mechanical etching process, and the machining characteristics of the channels are experimentally evaluated. In the process, material removal is performed by the collision of micro abrasives injected by highly compressed air on to the target surface. This approach can be characterized as an integration of brittle mode machining based on micro crack propagation. Fused silica glass, a high purity synthetic amorphous silicon dioxide, is selected as a workpiece material. It has a very low thermal expansion coefficient and excellent optical qualities and exceptional transmittance over a wide spectral range, especially in the ultraviolet range. The powder blasting process parameters affecting the machined results are injection pressure, abrasive particle size and density, stand-off distance, number of nozzle scanning, and shape/size of the required patterns. In this study, the influence of the number of nozzle scanning, abrasive particle size, and pattern size on the formation of micro channels is investigated. Machined shapes and surface roughness are measured using a 3-dimensional vision profiler and the results are discussed.

  1. Investigation of surface characteristics evolution and laser damage performance of fused silica during ion-beam sputtering

    Science.gov (United States)

    Xu, Mingjin; Dai, Yifan; Zhou, Lin; Shi, Feng; Wan, Wen; Xie, Xuhui; Sui, Tingting

    2016-08-01

    Surface characteristics have great influence on the optical properties especially the laser radiation resistivity of optics. In this paper, the surface characteristics evolutions of fused silica during ion-beam sputtering and their effects on the laser damage performance were investigated. The results show that roughness change is strongly removal depth dependent and a super-smooth surface (0.25 nm RMS) can be obtained by the ion-induced smoothing effect. The concentration of metal impurities (especially Ce element) in subsurface can be effectively decreased after the removal of polishing re-deposition layer. During ion-beam sputtering process, the plastic scratches can be removed while the brittle cracks can be broadened and passivated without increase in the depth direction. Laser damage threshold of fused silica improved by 36% after ion-beam sputtering treatment. Research results have a guiding significance for ion-beam sputtering process technology of fused silica optics.

  2. Monitoring annealing via carbon dioxide laser heating of defect populations in fused silica surfaces using photoluminescence microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Raman, R N; Matthews, M J; Adams, J J; Demos, S G

    2010-02-01

    Photoluminescence (PL) microscopy and spectroscopy under 266 nm and 355 nm laser excitation are explored as a means of monitoring defect populations in laser-modified sites on the surface of fused silica and their subsequent response to heating to different temperatures via exposure to a CO{sub 2} laser beam. Laser-induced temperature changes were estimated using an analytic solution to the heat flow equation and compared to changes in the PL emission intensity. The results indicate that the defect concentrations decrease significantly with increasing CO{sub 2} laser exposure and are nearly eliminated when the peak surface temperature exceeds the softening point of fused silica ({approx}1900K), suggesting that this method might be suitable for in situ monitoring of repair of defective sites in fused silica optical components.

  3. The effect of high-pressure devitrification and densification on ballistic-penetration resistance of fused silica

    Science.gov (United States)

    Avuthu, Vasudeva Reddy

    Despite the clear benefits offered by more advanced transparent materials, (e.g. transparent ceramics offer a very attractive combination of high stiffness and high hardness levels, highly-ductile transparent polymers provide superior fragment-containing capabilities, etc.), ballistic ceramic-glass like fused-silica remains an important constituent material in a majority of transparent impact-resistant structures (e.g. windshields and windows of military vehicles, portholes in ships, ground vehicles and spacecraft) used today. Among the main reasons for the wide-scale use of glass, the following three are most frequently cited: (i) glass-structure fabrication technologies enable the production of curved, large surface-area, transparent structures with thickness approaching several inches; (ii) relatively low material and manufacturing costs; and (iii) compositional modifications, chemical strengthening, and controlled crystallization have been demonstrated to be capable of significantly improving the ballistic properties of glass. In the present work, the potential of high-pressure devitrification and densification of fused-silica as a ballistic-resistance-enhancement mechanism is investigated computationally. In the first part of the present work, all-atom molecular-level computations are carried out to infer the dynamic response and material microstructure/topology changes of fused silica subjected to ballistic impact by a nanometer-sized hard projectile. The analysis was focused on the investigation of specific aspects of the dynamic response and of the microstructural changes such as the deformation of highly sheared and densified regions, and the conversion of amorphous fused silica to SiO2 crystalline allotropic modifications (in particular, alpha-quartz and stishovite). The microstructural changes in question were determined by carrying out a post-processing atom-coordination procedure. This procedure suggested the formation of high-density stishovite (and

  4. Invited article: CO2 laser production of fused silica fibers for use in interferometric gravitational wave detector mirror suspensions.

    Science.gov (United States)

    Heptonstall, A; Barton, M A; Bell, A; Cagnoli, G; Cantley, C A; Crooks, D R M; Cumming, A; Grant, A; Hammond, G D; Harry, G M; Hough, J; Jones, R; Kelley, D; Kumar, R; Martin, I W; Robertson, N A; Rowan, S; Strain, K A; Tokmakov, K; van Veggel, M

    2011-01-01

    In 2000 the first mirror suspensions to use a quasi-monolithic final stage were installed at the GEO600 detector site outside Hannover, pioneering the use of fused silica suspension fibers in long baseline interferometric detectors to reduce suspension thermal noise. Since that time, development of the production methods of fused silica fibers has continued. We present here a review of a novel CO(2) laser-based fiber pulling machine developed for the production of fused silica suspensions for the next generation of interferometric gravitational wave detectors and for use in experiments requiring low thermal noise suspensions. We discuss tolerances, strengths, and thermal noise performance requirements for the next generation of gravitational wave detectors. Measurements made on fibers produced using this machine show a 0.8% variation in vertical stiffness and 0.05% tolerance on length, with average strengths exceeding 4 GPa, and mechanical dissipation which meets the requirements for Advanced LIGO thermal noise performance.

  5. Facile preparation of organic-silica hybrid monolith for capillary hydrophilic liquid chromatography based on "thiol-ene" click chemistry.

    Science.gov (United States)

    Chen, Ming-Luan; Zhang, Jun; Zhang, Zheng; Yuan, Bi-Feng; Yu, Qiong-Wei; Feng, Yu-Qi

    2013-04-05

    In this work, a one-step approach to facile preparation of organic-inorganic hybrid monoliths was successfully developed. After vinyl-end organic monomers and azobisisobutyronitrile (AIBN) were mixed with hydrolyzed tetramethoxysilane (TMOS) and 3-mercaptopropyltrimethoxysilane (MPTMS), the homogeneous mixture was introduced into a fused-silica capillary for simultaneous polycondensation and "thiol-ene" click reaction to form the organic-silica hybrid monoliths. By employing this strategy, two types of organic-silica hybrid monoliths with positively charged quaternary ammonium and amide groups were prepared, respectively. The functional groups were successfully introduced onto the monoliths during the sol-gel process with "thiol-ene" click reaction, which was demonstrated by ζ-potential assessment, energy dispersive X-ray spectroscopy (EDX), and Fourier transform infrared (FT-IR) spectroscopy. The porous structure of the prepared monolithic columns was examined by scanning electron microscopy (SEM), nitrogen adsorption-desorption measurement, and mercury intrusion porosimetry. These results indicate the prepared organic-silica hybrid monoliths possess homogeneous column bed, large specific surface area, good mechanical stability, and excellent permeability. The prepared monolithic columns were then applied for anion-exchange/hydrophilic interaction liquid chromatography. Different types of analytes, including benzoic acids, inorganic ions, nucleosides, and nucleotides, were well separated with high column efficiency around 80,000-130,000 plates/m. Taken together, we present a facile and universal strategy to prepare organic-silica hybrid monoliths with a variety of organic monomers using one-step approach. Copyright © 2013 Elsevier B.V. All rights reserved.

  6. Mitigation of Laser Damage Growth in Fused Silica with a Galvanometer Scanned CO2 Laser

    Energy Technology Data Exchange (ETDEWEB)

    Bass, I L; Guss, G M; Hackel, R P

    2005-10-28

    At the National Ignition Facility (NIF) at the Lawrence Livermore National Laboratory (LLNL), mitigation of laser surface damage growth on fused silica using single and multiple CO{sub 2} laser pulses has been consistently successful for damage sites whose lateral dimensions are less than 100 {micro}m, but has not been for larger sites. Cracks would often radiate outward from the damage when a CO{sub 2} pulse was applied to the larger sites. An investigation was conducted to mitigate large surface damage sites using galvanometer scanning of a tightly focused CO{sub 2} laser spot over an area encompassing the laser damage. It was thought that by initially scanning the CO{sub 2} spot outside the damage site, radiating crack propagation would be inhibited. Scan patterns were typically inward moving spirals starting at radii somewhat larger than that of the damage site. The duration of the mitigation spiral pattern was {approx}110 ms during which a total of {approx}1.3 J of energy was delivered to the sample. The CO{sub 2} laser spot had a 1/e{sup 2}-diameter of {approx}200 {micro}m. Thus, there was general heating of a large area around the damage site while rapid evaporation occurred locally at the laser spot position in the spiral. A 30 to 40 {micro}m deep crater was typically generated by this spiral with a diameter of {approx}600 {micro}m. The spiral would be repeated until there was no evidence of the original damage in microscope images. Using this technique, damage sites as large as 300 mm in size did not display new damage after mitigation when exposed to fluences exceeding 22 J/cm{sup 2} at 355 nm, 7.5 ns. It was found necessary to use a vacuum nozzle during the mitigation process to reduce the amount of re-deposited fused silica. In addition, curing spiral patterns at lower laser powers were used to presumably ''re-melt'' any re-deposited fused silica. A compact, shearing interferometer microscope was developed to permit in situ

  7. Early Regimes of Water Capillary Flow in Slit Silica Nanochannels

    DEFF Research Database (Denmark)

    Oyarzua, Elton; Walther, Jens Honore; Mejia, Andres

    2015-01-01

    Molecular dynamics simulations are conducted to investigate the initial stages of spontaneous imbibitionof water in slit silica nanochannels surrounded by air. An analysis is performed for the effects of nanoscopicconfinement, initial conditions of liquid uptake and air pressurization...

  8. Immobilization of Styrene-acrylamide Co-polymer on Either Silica Particles or Inner Surface of Silica Capillary for the Separation of D-Glucose Anomers

    Energy Technology Data Exchange (ETDEWEB)

    Ali, Faiz; Kim, Yune Sung; Cheong, Won Jo [Inha Univ., Incheon (Korea, Republic of)

    2014-02-15

    Styrene-acrylamide co-polymer was immobilized on porous partially sub-2 μm silica monolith particles and inner surface of fused silica capillary (50 μm ID and 28 cm length) to result in μLC and CEC stationary phases, respectively, for separation of anomeric D-glucose derivatives. Reversed addition-fragmentation transfer (RAFT) polymerization was incorporated to induce surface polymerization. Acrylamide was employed to incorporate amide-functionality in the stationary phase. The resultant μLC and CEC stationary phases were able to separate isomers of D-glucose derivatives with high selectivity and efficiency. The mobile phase of 75/ 25 (v/v) acetonitrile (ACN)/water with 0.1% TFA, was used for HPLC with a packed column (1 mm ID, 300 mm length). The effects of pH and ACN composition on anomeric separation of D-glucose in CEC have been examined. A mobile phase of 85/15 (v/v) ACN/30 mM sodium acetate pH 6.7 was found the optimized mobile phase for CEC. The CEC stationary phase also gave good separation of other saccharides such as maltotriose and Dextran 1500 (MW∼1500) with good separation efficiency (number of theoretical plates ∼300,000/m)

  9. Dental resin composites containing silica-fused whiskers--effects of whisker-to-silica ratio on fracture toughness and indentation properties.

    Science.gov (United States)

    Xu, Hockin H K; Quinn, Janet B; Smith, Douglas T; Antonucci, Joseph M; Schumacher, Gary E; Eichmiller, Frederick C

    2002-02-01

    Dental resin composites need to be strengthened in order to improve their performance in large stress-bearing applications such as crowns and multiple-unit restorations. Recently, silica-fused ceramic whiskers were used to reinforce dental composites, and the whisker-to-silica ratio was found to be a key microstructural parameter that determined the composite strength. The aim of this study was to further investigate the effects of whisker-to-silica ratio on the fracture toughness, elastic modulus, hardness and brittleness of the composite. Silica particles and silicon carbide whiskers were mixed at whisker:silica mass ratios of 0:1, 1:5. 1:2, 1:1, 2:1, 5:1, and 1:0. Each mixture was thermally fused, silanized and combined with a dental resin at a filler mass percentage of 60%. Fracture toughness was measured with a single-edge notched beam method. Elastic modulus and hardness were measured with a nano-indentation system. Whisker:silica ratio had significant effects on composite properties. The composite toughness (mean+/-SD; n = 9) at whisker:silica = 2:1 was (2.47+/-0.28) MPa m(1/2), significantly higher than (1.02+/-0.23) at whisker:silica = 0:1, (1.13+/-0.19) of a prosthetic composite control, and (0.95+/-0.11) of an inlay/onlay composite control (Tukey's at family confidence coefficient = 0.95). Elastic modulus increased monotonically and hardness plateaued with increasing the whisker:silica ratio. Increasing the whisker:silica ratio also decreased the composite brittleness, which became about 1/3 of that of the inlay:onlay control. Electron microscopy revealed relatively flat fracture surfaces for the controls, but much rougher ones for the whisker composites, with fracture steps and whisker pullout contributing to toughness. The whiskers appeared to be well-bonded with the matrix, probably due to the fused silica producing rough whisker surfaces. Reinforcement with silica-fused whiskers resulted in novel dental composites that possessed fracture toughness

  10. Laser Damage Growth in Fused Silica with Simultaneous 351 nm and 1053 nm irradiation

    Energy Technology Data Exchange (ETDEWEB)

    Norton, M A; Carr, A V; Carr, C W; Donohue, E E; Feit, M D; Hollingsworth, W G; Liao, Z; Negres, R A; Rubenchik, A M; Wegner, P J

    2008-10-24

    Laser-induced growth of optical damage often determines the useful lifetime of an optic in a high power laser system. We have extended our previous work on growth of laser damage in fused silica with simultaneous 351 nm and 1053 nm laser irradiation by measuring the threshold for growth with various ratios of 351 nm and 1053 nm fluence. Previously we reported that when growth occurs, the growth rate is determined by the total fluence. We now find that the threshold for growth is dependent on both the magnitude of the 351 nm fluence as well as the ratio of the 351 nm fluence to the 1053 nm fluence. Furthermore, the data suggests that under certain conditions the 1053 nm fluence does not contribute to the growth.

  11. Fabrication of 250-nm-hole arrays in glass and fused silica by UV laser ablation

    Science.gov (United States)

    Karstens, R.; Gödecke, A.; Prießner, A.; Ihlemann, J.

    2016-09-01

    Parallel nanohole drilling in glass using an ArF excimer laser (193 nm) is demonstrated. For the first time, hole arrays with 500 nm pitch and individual holes with 250 nm diameter and more than 100 nm depth are fabricated by phase mask imaging using a Schwarzschild objective. Holes in soda lime glass are drilled by direct ablation; fused silica is processed by depositing a SiOx-film on SiO2, patterning the SiOx by ablation, and finally oxidizing the remaining SiOx to SiO2. Thermally induced ordered dewetting of noble metal films deposited on such templates may be used for the fabrication of plasmonic devices.

  12. Apparatus for dimensional characterization of fused silica fibers for the suspensions of advanced gravitational wave detectors.

    Science.gov (United States)

    Cumming, A; Jones, R; Barton, M; Cagnoli, G; Cantley, C A; Crooks, D R M; Hammond, G D; Heptonstall, A; Hough, J; Rowan, S; Strain, K A

    2011-04-01

    Detection of gravitational waves from astrophysical sources remains one of the most challenging problems faced by experimental physicists. A significant limit to the sensitivity of future long-baseline interferometric gravitational wave detectors is thermal displacement noise of the test mass mirrors and their suspensions. Suspension thermal noise results from mechanical dissipation in the fused silica suspension fibers suspending the test mass mirrors and is therefore an important noise source at operating frequencies between ∼10 and 30 Hz. This dissipation occurs due to a combination of thermoelastic damping, surface and bulk losses. Its effects can be reduced by optimizing the thermoelastic and surface loss, and these parameters are a function of the cross sectional dimensions of the fiber along its length. This paper presents a new apparatus capable of high resolution measurements of the cross sectional dimensions of suspension fibers of both rectangular and circular cross section, suitable for use in advanced detector mirror suspensions.

  13. Filamentation of an annular laser beam with a vortex phase dislocation in fused silica

    Science.gov (United States)

    Vasil'ev, E. V.; Shlenov, S. A.

    2016-11-01

    The filamentation of a femtosecond laser pulse in fused silica has been numerically investigated for the case of an annular beam with a phase singularity at a wavelength of 800 {\\text{nm}}. The spatiotemporal propagation dynamics of the pulse and the transformation of its frequency-angular spectra are analysed. It is shown that a tubular structure with a radius of 3 - 4 \\unicode{956}{\\text{m}}, peak intensity of about 2.4 × 1013 {\\text{W cm}}-2, and maximum plasma density on the order of 1020 {\\text{cm}}-3 is formed in the nonlinear focus; the length of this structure significantly exceeds the waist length in the linear case. The results of the analysis are compared with the data obtained for an annular beam free of phase dislocations and for a Gaussian beam.

  14. Embedded nanogratings in bulk fused silica under non-diffractive Bessel ultrafast laser irradiation

    Science.gov (United States)

    Cheng, G.; Rudenko, A.; D'Amico, C.; Itina, T. E.; Colombier, J. P.; Stoian, R.

    2017-06-01

    We report the formation of embedded nanogratings in bulk fused silica under quasi-stationary field patterns generated by ultrashort laser pulses in nondiffractive modes. The zero-order Bessel beam consists of almost non-propagative light pulses distributed along a narrow micron-sized channel sustained over a large non-diffracting length. Upon multipulse irradiation, a regular pattern of nanoplanes is formed across the channel, spaced at approximately λ / 2 n . Applying an electromagnetic scattering model [A. Rudenko et al., Phys. Rev. B 93, 075427 (2016)], we associate the formation of nanogratings with multiple scattering from randomly distributed scattering centers created by laser light. Constructive interference between the scattered wavelets leads to periodic excitation enhancement without requiring explicit synchronism conditions. Permanent material modifications are found whenever the local carrier densities are maximized towards the critical value. Multiple periodicities are predicted, either implicitly related to the coherent electromagnetic interaction or due to periodic field depletion and photon replenishment.

  15. Infrared Femtosecond Laser Direct-Writing Digital Volume Gratings in Fused Silica

    Science.gov (United States)

    Wang, Ying; Li, Yu-Hua; Lu, Pei-Xiang

    2010-04-01

    We demonstrate that digital volume gratings can be fabricated in fused silica glass conveniently by direct femtosecond laser writing. The diffraction efficiencies of volume gratings can be essentially modulated by simply stacking and offsetting the unit structure. A series of volume gratings, which have the pitches of 5 μm and the size of 1 mm × 1 mm, have been fabricated with the writing speed of 500 μm/s, with which the processing period of each grating layer could be reduced to several minutes with a 1-kHz femtosecond laser system. Results show that the power spectrum of the diffracted waves of the volume gratings are dependent on the layer gap and layer offsetting.

  16. Nanostructuring of Fused Silica Assisted by Laser-shaped Metal Triangles Using a Nanosecond Laser

    Science.gov (United States)

    Lorenz, Pierre; Grüner, Christoph; Ehrhardt, Martin; Bayer, Lukas; Zimmer, Klaus

    Self-organized processes are of special interest for the laser-induced nanostructuring of surfaces. In this study we combined two self-organized processes: the microsphere lithography and the molten phase transformation for the nanostructuring of dielectrics. A fused silica substrate was covered with periodically ordered polystyrene (PS) spheres and the system was subsequently covered with 30 nm chromium. Afterwards the PS spheres were removed and the bare and resultant periodic Cr triangles were irradiated in two steps using a KrF excimer laser. First step: A low laser fluence treatment results in a melting and shape transformation of the triangles. Second step: A high laser fluence treatment of the pre-treated surface results in a nanostructuring of the dielectric surface (and removal of the metal). The surface topography was studied by scanning electron microscopy. Furthermore, the different steps were simulated and compared with the experimental results.

  17. Dependence of growth rate of quartz in fused silica on pressure and impurity content

    Science.gov (United States)

    Fratello, V. J.; Hays, J. F.; Turnbull, D.

    1980-01-01

    The effects of pressure, temperature, and some variations in impurity content on the growth rate u of quartz into fused silica were measured. Under all conditions the growth rate was interface controlled and increased exponentially with pressure with an activation volume averaging -21.2 cu cm/mole. The activation enthalpy for all specimens is extrapolated to a zero pressure value of 64 kcal/mole, within the experimental uncertainty. At a given stoichiometry the effect of hydroxyl content on growth rate is described entirely by a linear term C(OH) in the prefactor of the equation for the growth rate. The effect of chlorine impurity can be described similarly. Also u is increased as the ideal stoichiometry is approached from the partially reduced state.

  18. Generation of laser-induced periodic surface structures on transparent material-fused silica

    Science.gov (United States)

    Schwarz, Simon; Rung, Stefan; Hellmann, Ralf

    2016-05-01

    We report on a comparison between simulated and experimental results for the generation of laser-induced periodic surface structures with low spatial frequency on dielectrics. Using the established efficacy factor theory extended by a Drude model, we determine the required carrier density for the generation of low spatial frequency LIPSS (LSFL) and forecast their periodicity and orientation. In a subsequent calculative step, we determine the fluence of ultrashort laser pulses necessary to excite this required carrier density in due consideration of the pulse number dependent ablation threshold. The later calculation is based on a rate equation including photo- and avalanche ionization and derives appropriate process parameters for a selective generation of LSFL. Exemplarily, we apply this approach to the generation of LSFL on fused silica using a 1030 nm femtosecond laser. The experimental results for the orientation and spatial periodicity of LSFL reveal excellent agreement with the simulation.

  19. Irradiation effects of CO2 laser parameters on surface morphology of fused silica

    Institute of Scientific and Technical Information of China (English)

    Xiang Xia; Zheng Wan-Guo; Yuan Xiao-Dong; Dai Wei; Juang Yong; Li Xi-Bin; Wang Hai-Jun; Lü Hai-Bing; Zu Xiao-Tao

    2011-01-01

    To understand the surface morphology evolution of fused silica induced by 10.6-prn CO2 laser irradiation atdifferent parameters, this paper reports that optical microscopy, profilometry, and hydrophilicity tests are utilized to characterize the surface structure and roughness of the laser irradiated area. The results show that three typical surface morphologies and two typical by drophilicity test images are observed at different laser powers and pulse durations. Thecorrelations between surface temperature and surface morphology as well as hydrophilicity behaviours are presented.The different hydrophilicity behaviours are related to surface structures of the laser-induced crater and thermal diffusion area. The thermal diffusion length monotonously increases with increasing laser power and pulse duration. The crater width is almost determined by the laser beam size. The crater depth is more sensitive to the laser power and pulse duration than the crater width.

  20. Ultrafast laser induced electronic and structural modifications in bulk fused silica

    Science.gov (United States)

    Mishchik, K.; D'Amico, C.; Velpula, P. K.; Mauclair, C.; Boukenter, A.; Ouerdane, Y.; Stoian, R.

    2013-10-01

    Ultrashort laser pulses can modify the inner structure of fused silica, generating refractive index changes varying from soft positive (type I) light guiding forms to negative (type II) values with void presence and anisotropic sub-wavelength modulation. We investigate electronic and structural material changes in the type I to type II transition via coherent and incoherent secondary light emission reflecting free carrier behavior and post-irradiation material relaxation in the index change patterns. Using phase contrast microscopy, photoluminescence, and Raman spectroscopy, we determine in a space-resolved manner defect formation, redistribution and spatial segregation, and glass network reorganization paths in conditions marking the changeover between type I and type II photoinscription regimes. We first show characteristic patterns of second harmonic generation in type I and type II traces, indicating the collective involvement of free carriers and polarization memory. Second, incoherent photoemission from resonantly and non-resonantly excited defect states reveals accumulation of non-bridging oxygen hole centers (NBOHCs) in positive index domains and oxygen deficiency centers (ODCs) with O2- ions segregation in void-like regions and in the nanostructured domains, reflecting the interaction strength. Complementary Raman investigations put into evidence signatures of the different environments where photo-chemical densification (bond rearrangements) and mechanical effects can be indicated. NBOHCs setting in before visible index changes serve as precursors for subsequent compaction build-up, indicating a scenario of cold, defect-assisted densification for the soft type I irradiation regime. Additionally, we observe hydrodynamic effects and severe bond-breaking in type II zones with indications of phase transition. These observations illuminate densification paths in fused silica in low power irradiation regimes, and equally in energetic ranges, characterized by

  1. Internal structure of the nanogratings generated inside bulk fused silica by ultrafast laser direct writing

    Energy Technology Data Exchange (ETDEWEB)

    Sharma, S. P.; Vilar, R. [ICEMS—Instituto de Ciência e Engenharia de Materiais e Superfícies, Avenida Rovisco Pais no 1, 1049-001 Lisbon (Portugal); Instituto Superior Técnico, Avenida Rovisco Pais no 1, 1049-001 Lisbon (Portugal); Oliveira, V. [ICEMS—Instituto de Ciência e Engenharia de Materiais e Superfícies, Avenida Rovisco Pais no 1, 1049-001 Lisbon (Portugal); Instituto Superior de Engenharia de Lisboa, Avenida Conselheiro Emídio Navarro no 1, 1959-007 Lisbon (Portugal); Herrero, P. [Instituto de Ciencia de Materiales de Madrid (ICMM-CSIC), Cantoblanco, Madrid 28049 (Spain)

    2014-08-07

    The aim of the present work was to characterize the internal structure of nanogratings generated inside bulk fused silica by ultrafast laser processing and to study the influence of diluted hydrofluoric acid etching on their structure. The nanogratings were inscribed at a depth of 100 μm within fused silica wafers by a direct writing method, using 1030 nm radiation wavelength and the following processing parameters: E = 5 μJ, τ = 560 fs, f = 10 kHz, and v = 100 μm/s. The results achieved show that the laser-affected regions are elongated ellipsoids with a typical major diameter of about 30 μm and a minor diameter of about 6 μm. The nanogratings within these regions are composed of alternating nanoplanes of damaged and undamaged material, with an average periodicity of 351 ± 21 nm. The damaged nanoplanes contain nanopores randomly dispersed in a material containing a large density of defects. These nanopores present a roughly bimodal size distribution with average dimensions for each class of pores 65 ± 20 × 16 ± 8 × 69 ± 16 nm{sup 3} and 367 ± 239 × 16 ± 8 × 360 ± 194 nm{sup 3}, respectively. The number and size of the nanopores increases drastically when an hydrofluoric acid treatment is performed, leading to the coalescence of these voids into large planar discontinuities parallel to the nanoplanes. The preferential etching of the damaged material by the hydrofluoric acid solution, which is responsible for the pores growth and coalescence, confirms its high defect density.

  2. The Structure Evolution of Fused Silica Induced by CO2 Laser Irradiation

    Institute of Scientific and Technical Information of China (English)

    LIU Chun-Ming; LV Hai-Bing; ZHENG Wan-Guo; ZU Xiao-Tao; JIANG Yong; LUO Cheng-Si; SHI Xiao-Yan; REN Wei; XIANG Xia; WANG Hai-Jun; HE Shao-Bo; YUAN Xiao-Dong

    2012-01-01

    The structure evolution of fused silica induced by CO2 laser irradiation (with a wavelength of 10.6 μm) is studied in detail.In the non-evaporation mitigation process,the irradiation time should be long enough to completely eliminate damage.However,there is a raised rim around the mitigated site.The rim height is enhanced when the irradiation time increases,and the mitigated site can lead to off-axis and on-axis downstream light intensification.Volume shrinkage occurs during the irradiation and rapid cooling processes,and this may be due to a decrease in the Si O Si bond angle.The distribution of debris overlaps with the maximum phase retardance induced by stress.The debris arouses an enhanced light absorption in the region from 220nm to 800nm.%The structure evolution of fused silica induced by CO2 laser irradiation (with a wavelength of 10.6 μm) is studied in detail. In the non-evaporation mitigation process, the irradiation time should be long enough to completely eliminate damage. However, there is a raised rim around the mitigated site. The rim height is enhanced when the irradiation time increases, and the mitigated site can lead to off-axis and on-axis downstream light intensification. Volume shrinkage occurs during the irradiation and rapid cooling processes, and this may be due to a decrease in the Si-O-Si bond angle. The distribution of debris overlaps with the maximum phase retardance induced by stress. The debris arouses an enhanced light absorption in the region from 220 nm to 800 nm.

  3. Microstructuring of fused silica by laser-induced backside wet etching using picosecond laser pulses

    Energy Technology Data Exchange (ETDEWEB)

    Ehrhardt, M. [Leibniz-Institute of Surface Modification, Permoserstr. 15, 04318 Leipzig (Germany); Raciukaitis, G.; Gecys, P. [Laboratory for Applied Research, Institute of Physics, Savanoriu Ave. 231, LT-02300 Vilnius (Lithuania); Zimmer, K., E-mail: martin.ehrhardt@iom-leipzig.de [Leibniz-Institute of Surface Modification, Permoserstr. 15, 04318 Leipzig (Germany)

    2010-09-15

    The laser-induced backside wet etching (LIBWE) is an advanced laser processing method used for structuring transparent materials. LIBWE with nanosecond laser pulses has been successfully demonstrated for various materials, e.g. oxides (fused silica, sapphire) or fluorides (CaF{sub 2}, MgF{sub 2}), and applied for the fabrication of microstructures. In the present study, LIBWE of fused silica with mode-locked picosecond (t{sub p} = 10 ps) lasers at UV wavelengths ({lambda}{sub 1} = 355 nm and {lambda}{sub 2} = 266 nm) using a (pyrene) toluene solution was demonstrated for the first time. The influence of the experimental parameters, such as laser fluence, pulse number, and absorbing liquid, on the etch rate and the resulting surface morphology were investigated. The etch rate grew linearly with the laser fluence in the low and in the high fluence range with different slopes. Incubation at low pulse numbers as well as a nearly constant etch rate after a specific pulse number for example were observed. Additionally, the etch rate depended on the absorbing liquid used; whereas the higher absorption of the admixture of pyrene in the used toluene enhances the etch rate and decreases the threshold fluence. With a {lambda}{sub 1} = 266 nm laser set-up, an exceptionally smooth surface in the etch pits was achieved. For both wavelengths ({lambda}{sub 1} = 266 nm and {lambda}{sub 2} = 355 nm), LIPSS (laser-induced periodic surface structures) formation was observed, especially at laser fluences near the thresholds of 170 and 120 mJ/cm{sup 2}, respectively.

  4. Post-processing of fused silica and its effects on damage resistance to nanosecond pulsed UV lasers.

    Science.gov (United States)

    Ye, Hui; Li, Yaguo; Zhang, Qinghua; Wang, Wei; Yuan, Zhigang; Wang, Jian; Xu, Qiao

    2016-04-10

    HF-based (hydrofluoric acid) chemical etching has been a widely accepted technique to improve the laser damage performance of fused silica optics and ensure high-power UV laser systems at designed fluence. Etching processes such as acid concentration, composition, material removal amount, and etching state (etching with additional acoustic power or not) may have a great impact on the laser-induced damage threshold (LIDT) of treated sample surfaces. In order to find out the effects of these factors, we utilized the Taguchi method to determine the etching conditions that are helpful in raising the LIDT. Our results show that the most influential factors are concentration of etchants and the material etched away from the viewpoint of damage performance of fused silica optics. In addition, the additional acoustic power (∼0.6  W·cm-2) may not benefit the etching rate and damage performance of fused silica. Moreover, the post-cleaning procedure of etched samples is also important in damage performances of fused silica optics. Different post-cleaning procedures were, thus, experiments on samples treated under the same etching conditions. It is found that the "spraying + rinsing + spraying" cleaning process is favorable to the removal of etching-induced deposits. Residuals on the etched surface are harmful to surface roughness and optical transmission as well as laser damage performance.

  5. Coupling semiconductor nanocrystals to a fused-silica microsphere: a quantum-dot microcavity with extremely high Q factors.

    Science.gov (United States)

    Fan, X; Palinginis, P; Lacey, S; Wang, H; Lonergan, M C

    2000-11-01

    We demonstrate a quantum-dot microcavity by coupling core-shell semiconductor nanocrystals to a fused-silica microsphere. We show that the composite microcavity can feature Q factors of the order of 10(8), providing a model system for investigating cavity QED and microlasers at the level of single quantum dots.

  6. CO2 laser microprocessing for laser damage growth mitigation of fused silica optics

    Science.gov (United States)

    Doualle, Thomas; Gallais, Laurent; Monneret, Serge; Bouillet, Stephane; Bourgeade, Antoine; Ameil, Christel; Lamaignère, Laurent; Cormont, Philippe

    2017-01-01

    We report on the development of a mitigation process to prevent the growth of UV nanosecond laser-initiated damage sites under successive irradiations of fused silica components. The developed process is based on fast microablation of silica as it has been proposed by Bass et al. [Bass et al., Proc. SPIE 7842, 784220 (2010)]. This is accomplished by the displacement of the CO2 laser spot with a fast galvanometer beam scanner to form a crater with a typical conical shape to mitigate large (millimetric) and deep (few hundred microns) damage sites. We present the developed experimental system and process for this application. Particularly, we detail and evaluate a method based on quantitative phase imaging to obtain fast and accurate three-dimensional topographies of the craters. The morphologies obtained through different processes are then studied. Mitigation of submillimetric nanosecond damage sites is demonstrated through different examples. Experimental and numerical studies of the downstream intensifications, resulting in cone formation on the surface, are presented to evaluate and minimize the downstream intensifications. Eventually, the laser damage test resistance of the mitigated sites is evaluated at 355, 2.5 ns, and we discuss on the efficiency of the process for our application.

  7. Investigation of stress induced by CO2 laser processing of fused silica optics for laser damage growth mitigation.

    Science.gov (United States)

    Gallais, Laurent; Cormont, Philippe; Rullier, Jean-Luc

    2009-12-21

    Laser damage mitigation' is a process developed to prevent the growth of nanosecond laser-initiated damage sites under successive irradiation. It consists of re-fusing the damage area with a CO2 laser. In this paper we investigate the stress field created around mitigated sites which could have an influence on the efficiency of the process. A numerical model of CO2 laser interaction with fused silica is developed. It takes into account laser energy absorption, heat transfer, thermally induced stress and birefringence. Residual stress near mitigated sites in fused silica samples is characterized with specific photoelastic methods and theoretical data are compared to experiments. The stress distribution and quantitative values of stress levels are obtained for sites treated with the CO2 laser in various conditions of energy deposition (beam size, pulse duration, incident power). The results provided evidence that the presence of birefringence/residual stress around the mitigated sites has an effect on their laser damage resistance.

  8. Optical and electrical properties of boron doped diamond thin conductive films deposited on fused silica glass substrates

    Energy Technology Data Exchange (ETDEWEB)

    Ficek, M.; Sobaszek, M.; Gnyba, M. [Department of Metrology and Optoelectronics, Gdansk University of Technology, 11/12G. Narutowicza St., 80-233 Gdansk (Poland); Ryl, J. [Department of Electrochemistry, Corrosion and Material Engineering, Gdansk University of Technology, 11/12 Narutowicza St., 80-233 Gdansk (Poland); Gołuński, Ł. [Department of Metrology and Optoelectronics, Gdansk University of Technology, 11/12G. Narutowicza St., 80-233 Gdansk (Poland); Smietana, M.; Jasiński, J. [Institute of Microelectronics and Optoelectronics, Warsaw University of Technology, 75 Koszykowa St., 00-662 Warsaw (Poland); Caban, P. [Institute of Electronic Materials Technology, 133 Wolczynska St., 01-919 Warsaw (Poland); Bogdanowicz, R., E-mail: rbogdan@eti.pg.gda.pl [Department of Metrology and Optoelectronics, Gdansk University of Technology, 11/12G. Narutowicza St., 80-233 Gdansk (Poland); Materials and Process Simulation Center, California Institute of Technology, Pasadena, CA 91125 (United States)

    2016-11-30

    Highlights: • Growth of 60% of transmittance diamond films with resistivity as low as 48 Ω cm. • Two step seeding process of fused silica: plasma hydrogenation and wet seeding. • Nanodiamond seeding density of 2 × 10{sup 10} cm{sup −2} at fused silica substrates. • High refractive index (2.4 @550 nm) was achieved for BDD films deposited at 500 °C. - Abstract: This paper presents boron-doped diamond (BDD) film as a conductive coating for optical and electronic purposes. Seeding and growth processes of thin diamond films on fused silica have been investigated. Growth processes of thin diamond films on fused silica were investigated at various boron doping level and methane admixture. Two step pre-treatment procedure of fused silica substrate was applied to achieve high seeding density. First, the substrates undergo the hydrogen plasma treatment then spin-coating seeding using a dispersion consisting of detonation nanodiamond in dimethyl sulfoxide with polyvinyl alcohol was applied. Such an approach results in seeding density of 2 × 10{sup 10} cm{sup −2}. The scanning electron microscopy images showed homogenous, continuous and polycrystalline surface morphology with minimal grain size of 200 nm for highly boron doped films. The sp{sup 3}/sp{sup 2} ratio was calculated using Raman spectra deconvolution method. A high refractive index (range of 2.0–2.4 @550 nm) was achieved for BDD films deposited at 500 °C. The values of extinction coefficient were below 0.1 at λ = 550 nm, indicating low absorption of the film. The fabricated BDD thin films displayed resistivity below 48 Ohm cm and transmittance over 60% in the visible wavelength range.

  9. HF-based etching processes for improving laser damage resistance of fused silica optical surfaces

    Energy Technology Data Exchange (ETDEWEB)

    Suratwala, T I; Miller, P E; Bude, J D; Steele, R A; Shen, N; Monticelli, M V; Feit, M D; Laurence, T A; Norton, M A; Carr, C W; Wong, L L

    2010-02-23

    The effect of various HF-based etching processes on the laser damage resistance of scratched fused silica surfaces has been investigated. Conventionally polished and subsequently scratched fused silica plates were treated by submerging in various HF-based etchants (HF or NH{sub 4}F:HF at various ratios and concentrations) under different process conditions (e.g., agitation frequencies, etch times, rinse conditions, and environmental cleanliness). Subsequently, the laser damage resistance (at 351 or 355 nm) of the treated surface was measured. The laser damage resistance was found to be strongly process dependent and scaled inversely with scratch width. The etching process was optimized to remove or prevent the presence of identified precursors (chemical impurities, fracture surfaces, and silica-based redeposit) known to lead to laser damage initiation. The redeposit precursor was reduced (and hence the damage threshold was increased) by: (1) increasing the SiF{sub 6}{sup 2-} solubility through reduction in the NH4F concentration and impurity cation impurities, and (2) improving the mass transport of reaction product (SiF{sub 6}{sup 2-}) (using high frequency ultrasonic agitation and excessive spray rinsing) away from the etched surface. A 2D finite element crack-etching and rinsing mass transport model (incorporating diffusion and advection) was used to predict reaction product concentration. The predictions are consistent with the experimentally observed process trends. The laser damage thresholds also increased with etched amount (up to {approx}30 {micro}m), which has been attributed to: (1) etching through lateral cracks where there is poor acid penetration, and (2) increasing the crack opening resulting in increased mass transport rates. With the optimized etch process, laser damage resistance increased dramatically; the average threshold fluence for damage initiation for 30 {micro}m wide scratches increased from 7 to 41 J/cm{sup 2}, and the statistical

  10. Aptamer modified organic-inorganic hybrid silica monolithic capillary columns for highly selective recognition of thrombin.

    Science.gov (United States)

    Deng, Nan; Liang, Zhen; Liang, Yu; Sui, Zhigang; Zhang, Liyuan; Wu, Qi; Yang, Kaiguang; Zhang, Lihua; Zhang, Yukui

    2012-12-04

    A novel kind of aptamer modified organic-inorganic hybrid silica monolithic capillary column has been developed, via the covalent bonding of 5'-NH(2)-modified aptamer for human α-thrombin on hybrid silica monolith, prepared by sol-gel method, with tetraethoxysilane and 3-aminopropyltriethoxysilane as precursors. Due to the large specific surface area of the hybrid matrix, the average coverage density of aptamer reached 568 pmol/μL, and the thrombin binding capacity was 1.15 μg/μL, 14 times higher than that of aptamer modified open tubular capillaries. By such an affinity capillary column, the limit of detection of thrombin was decreased to 3.4 nM with a UV detector. Furthermore, even when thrombin was mixed with 1000 times more concentrated human serum, it could be selectively enriched and detected with the signal-to-noise ratio as ca.10. These results indicate that the developed preparation strategy for aptamer based hybrid silica monolithic capillary column might provide an effective method to achieve highly selective recognition of trace targets.

  11. One-pot preparation of glutathione-silica hybrid monolith for mixed-mode capillary liquid chromatography based on "thiol-ene" click chemistry.

    Science.gov (United States)

    Lin, Zian; Tan, Xiaoqing; Yu, Ruifang; Lin, Jiashi; Yin, Xiaofei; Zhang, Lan; Yang, Huanghao

    2014-08-15

    A novel glutathione (GSH)-silica hybrid monolithic column synthesized via a combination of thiol-ene click reaction and one-pot process was described, where thiol-end GSH organic monomer and 2,2-azobisisobutyronitrile (AIBN) were mixed with hydrolyzed tetramethyloxysilane (TMOS) and γ-methacryloxypropyltrimethoxysilane (γ-MAPS) and then introduced into a fused-silica capillary for simultaneous polycondensation and "thiol-ene" click reaction to form the GSH-silica hybrid monolith. The effects of the molar ratio of TMOS/γ-MAPS, the amount of GSH, and the volume of porogen on the morphology, permeability and pore properties of the prepared GSH-silica hybrid monoliths were studied in detail. A uniform monolithic network with high porosity was obtained. A series of test compounds including alkylbenzenes, amides, and anilines were used to evaluate the retention behaviors of the GSH-silica hybrid monolithic column. The results demonstrated that the prepared GSH-silica hybrid monolith exhibited multiple interactions including hydrophobicity, hydrophilicity, as well as cation exchange interaction. The run-to-run, column-to-column and batch-to-batch reproducibilities of the GSH-silica hybrid monolith for phenols' retention were satisfactory with the relative standard deviations (RSDs) less than 1.3% (n=5), 2.6% (n=3) and 3.2% (n=3), respectively, indicating the effectiveness and practicability of the proposed method. In addition, the GSH-silica hybrid monolith was applied to the separation of nucleotides, peptides and protein tryptic digests, respectively. The successful applications suggested the potential of the GSH-silica hybrid monolith in complex sample analysis.

  12. Phenyl Functionalized Sol-gel Silica Sorbent for Capillary Microextraction and Chromia-Based Sol-gel Ucon Stationary Phase for Capillary Gas Chromatography

    Science.gov (United States)

    McLean, Michael M.

    The first chapter of this thesis presents an introduction to sol-gel methodology whose usefulness as a synthetic route will be demonstrated with two applications in chromatography. The first application involves the fabrication of a capillary micro-extraction (CME) device by coating a phenyl functionalized extracting phase on the inner surface of a fused silica capillary for analyte pre-concentration. The device was coupled on-line to a RP-HPLC system and practicality was demonstrated using allergens as target analytes. The allergens chosen as model analytes are typically found in fragrance products and food. Most of the 26 fragrance allergens that are monitored by various government authorities have a phenyl organic moiety (a strong chromophore), thus making them appropriate probes for exploring the extraction efficiency of the coating using a UV detector. The CME device showed ppt level limit of detection which makes it suitable for trace analyses of allergens and similar compounds in a variety of matrices. The second application explores the feasibility of using sol-gel derived chromia-based stationary phase in gas chromatographic columns. The organic moiety of the stationary phase was derived from Ucon 75-H-90,000 while the inorganic backbone was prepared using chromium(III) dichloride hydroxide - methacrylic acid - aqua complex, 40% in isopropanol/acetone . Usefulness of prepared chromia-based GC stationary phase was examined for petrochemical application. Promising results were obtained using aliphatic-aromatics, polyaromatic hydrocarbons, BTEX test mixture, cycloalkanes, branched alkanes and akylbenzenes. The column was able to perform without degradation despite being rinsed multiples times sequentially with the following solvents: dichloromethane, methanol, water and finally methanol again. Maximum theoretical plate number calculated is around 2,400 plates/m. The plate number clearly needs improvement but is a promising result for the newly explored

  13. High temperature thermal behaviour modeling of large-scale fused silica optics for laser facility

    Institute of Scientific and Technical Information of China (English)

    Yu Jing-Xia; He Shao-Bo; Xiang Xia; Yuan Xiao-Dong; Zheng Wan-Guo; Lü Hai-Bing; Zu Xiao-Tao

    2012-01-01

    High temperature annealing is often used for the stress control of optical materials.However,weight and viscosity at high temperature may destroy the surface morphology,especially for the large-scale,thin and heavy optics used for large laser facilities.It is necessary to understand the thermal behaviour and design proper support systems for large-scale optics at high temperature.In this work,three support systems for fused silica optics are designed and simulated with the finite element method.After the analysis of the thermal behaviours of different support systems,some advantages and disadvantages can be revealed.The results show that the support with the optical surface vertical is optimal because both pollution and deformation of optics could be well controlled during annealing at high temperature.Annealing process of the optics irradiated by CO2 laser is also simulated.It can be concluded that high temperature annealing can effectively reduce the residual stress.However,the effects of annealing on surface morphology of the optics are complex.Annealing creep is closely related to the residual stress and strain distribution.In the region with large residual stress,the creep is too large and probably increases the deformation gradient which may affect the laser beam propagation.

  14. Spherical Fused Silica Cells Filled with Pure Helium for NMR-Magnetometry

    CERN Document Server

    Maul, Andreas; Heil, Werner; Nikiel, Anna; Otten, Ernst; Petrich, Andreas; Schmidt, Thomas

    2015-01-01

    High magnetic fields (> 1 T) are measured by NMR magnetometers with un-rivaled precision if the precessing spin sample provides long coherence times. The longest coherence times are found in diluted ${}^{3}$He samples, which can be hyperpolarized for sufficient signal strength. In order to have minimal influence on the homogeneity and value of the measured magnetic field the optimal container for the ${}^{3}$He should be a perfect sphere. A fused silica sphere with an inner diameter of 8 mm and an outer diameter of 12 mm was made from two hemispheres by diffusion bonding leaving only a small hole for cleaning and evacuation. This hole was closed in vacuum by a CO${}_{2}$ laser and the inner volume was filled with a few mbars of ${}^3$He via wall permeation. NMR-measurements on such a sample had coherence times of 5 min. While the hemispheres were produced with < 1 $\\mu$m deviation from sphericity, the bonding left a step of ca. 50 $\\mu$m at maximum. The influence of such a mismatch, its orientation and mat...

  15. Wavelength-tunable multicolored femtosecond laser pulse generation in a fused silica glass plate

    Science.gov (United States)

    Kobayashi, Takayoshi; Liu, Jun

    2010-05-01

    We obtained an array of multicolored femtosecond laser pulses with as many as 17 different colors that are spatially isolated. The mechanism of generation was proved to be cascaded four-wave mixing and with the following procedure. The output beam from a femtosecond laser was split into two. One of the two beams was pulse-compressed with a hollow core fiber and the intensity of the other was reduced. The two beams were synchronized and combined with a small crossing angle in a plate of fused silica glass plate. The wavelengths of the sidebands are continuously tunable from near-ultraviolet to near-infrared. The pulse duration, spatial mode, spectrum, and energy stability of the sidebands were studied. As many as fifteen spectral up-shifted pulses and two spectral downshifted pulses were obtained with spectral bandwidths broader than 1.8 octaves. Properties such as pulse energy as high as 1 μmJ, 45 fs pulse duration, smaller than 1.1 times of the diffraction limit Gaussian spatial profile, and better than 2% RMS power stability of the generated sidebands make it can be used in various experiments. The characterization showed that the sidebands have sufficiently good qualities to enable application to for various multicolor femtosecond laser experiments, for example, a multicolor pump-probe experiment.

  16. Generation of microstripe cylindrical and toroidal mirrors by localized laser evaporation of fused silica.

    Science.gov (United States)

    Wlodarczyk, Krystian L; Thomson, Ian J; Baker, Howard J; Hall, Denis R

    2012-09-10

    We report a new technique for the rapid fabrication of microstripe cylindrical and toroidal mirrors with a high ratio (>10) of the two principal radii of curvature (RoC(1)/RoC(2)), and demonstrate their effectiveness as mode-selecting resonator mirrors for high-power planar waveguide lasers. In this process, the larger radius of curvature (RoC(1)) is determined by the planar or cylindrical shape of the fused silica substrate selected for laser processing, whilst the other (RoC(2)) is produced by controlled CO(2) laser-induced vaporization of the glass. The narrow stripe mirror aperture is achieved by applying a set of partially overlapped laser scans, with the incident laser power, the number of laser scans, and their spacing being used to control the curvature produced by laser evaporation. In this work, a 1 mm diameter laser spot is used to produce grooves of cylindrical/toroidal shape with 240 μm width and 16 mm length. After high reflectance coating, these grooves are found to provide excellent mode selectivity as resonator mirrors for a 150 μm core Yb:YAG planar waveguide laser, producing high brightness output at more than 300 W. The results show clearly that the laser-generated microstripe mirrors can improve the optical performance of high-power planar waveguide lasers when applied in a low-loss mode-selective resonator configuration.

  17. Fracture Strength of Fused Silica From Photonic Signatures Around Collision Sites

    Science.gov (United States)

    Yost, William T.; Cramer, K Elliott

    2015-01-01

    Impact sites in glass affect its fracture strength. An analytical model that predicts fracture strength from grey-field polariscope (GFP) readings (photoelastic retardations) has been developed and reported in the literature. The model is suggestive that stress fields, resulting from impact damage, destablizes sites within the glass, which lead to pathways that cause strength degradation. Using data collected from fused silica specimens fabricated from outer window panes that were designed for the space shuttle, the model was tested against four categories of inflicted damage. The damage sites were cored from the window carcasses, examined with the GFP and broken using the ASTM Standard C1499-09 to measure the fracture strength. A correlation is made between the fracture strength and the photoelastic retardation measured at the damage site in each specimen. A least-squares fit is calculated. The results are compared with the predictions from the model. A plausible single-sided NDE damage site inspection method (a version of which is planned for glass inspection in the Orion Project) that relates photoelastic retardation in glass components to its fracture strength is presented.

  18. Morphology and mechanisms of picosecond ablation of metal films on fused silica substrates

    Science.gov (United States)

    Bass, Isaac L.; Negres, Raluca A.; Stanion, Ken; Guss, Gabe; Keller, Wesley J.; Matthews, Manyalibo J.; Rubenchik, Alexander M.; Yoo, Jae Hyuck; Bude, Jeffrey D.

    2016-12-01

    The ablation of magnetron sputtered metal films on fused silica substrates by a 1053 nm, picosecond class laser was studied as part of a demonstration of its use for in-situ characterization of the laser spot under conditions commonly used at the sample plane for laser machining and damage studies. Film thicknesses were 60 and 120 nm. Depth profiles and SEM images of the ablation sites revealed several striking and unexpected features distinct from those typically observed for ablation of bulk metals. Very sharp thresholds were observed for both partial and complete ablation of the films. Partial film ablation was largely independent of laser fluence with a surface smoothness comparable to that of the unablated surface. Clear evidence of material displacement was seen at the boundary for complete film ablation. These features were common to a number of different metal films including Inconel on commercial neutral density filters, stainless steel, and aluminum. We will present data showing the morphology of the ablation sites on these films as well as a model of the possible physical mechanisms producing the unique features observed.

  19. Stable structure and optical properties of fused silica with NBOHC-E‧ defect

    Science.gov (United States)

    Lu, Peng-Fei; Wu, Li-Yuan; Yang, Yang; Wang, Wei-Zheng; Zhang, Chun-Fang; Yang, Chuang-Hua; Su, Rui; Chen, Jun

    2016-08-01

    First-principles method is used to simulate the stable structure and optical properties of a 96-atom fused silica. The preferable structure of NBOHC-E‧ (non-bridging oxygen hole center (NBOHC) and E‧ center) pair defect is predicted to be located at 2.4 Å for the Si-O bond length. The quasi-particle G0W0 calculations are performed and an accurate band gap is obtained in order to calculate the optical absorption properties. With the stretching of the Si1-O1 bond, an obvious redshift can be observed in the absorption spectrum. In the case of NBOHC-E‧ pair, the p-orbital DOS of Si1 atom will shift to the conduction band. Two obvious absorption peaks can be observed in the absorption spectrum. The calculation reproduced the peak positions of the well-known optical absorption bands. Project supported by the National Basic Research Program of China (Grant No. 2014CB643900), the Open Fund of IPOC (BUPT), the Open Program of State Key Laboratory of Functional Materials for Informatics, the National Natural Science Foundation for Theoretical Physics Special Fund “Cooperation Program” (Grant No. 11547039), and Shaanxi Provincial Institute of Scientific Research Plan Projects, China (Grant No. SLGKYQD2-05).

  20. Influence of secondary treatment with CO2 laser irradiation for mitigation site on fused silica surface

    Science.gov (United States)

    Jiang, Yong; Zhou, Qiang; Qiu, Rong; Gao, Xiang; Wang, Hui-Li; Yao, Cai-Zhen; Wang, Jun-Bo; Zhao, Xin; Liu, Chun-Ming; Xiang, Xia; Zu, Xiao-Tao; Yuan, Xiao-Dong; Miao, Xin-Xiang

    2016-10-01

    The ablation debris and raised rim, as well as residual stress and deep crater will be formed during the mitigation of damage site with a CO2 laser irradiation on fused silica surface, which greatly affects the laser damage resistance of optics. In this study, the experimental study combined with numerical simulation is utilized to investigate the effect of the secondary treatment on a mitigated site by CO2 laser irradiation. The results indicate that the ablation debris and the raised rim can be completely eliminated and the depth of crater can be reduced. Notable results show that the residual stress of the mitigation site after treatment will reduce two-thirds of the original stress. Finally, the elimination and the controlling mechanism of secondary treatment on the debris and raised rim, as well as the reasons for changing the profile and stress are analyzed. The results can provide a reference for the optimization treatment of mitigation sites by CO2 laser secondary treatment. Project supported by the National Natural Science Foundation of China (Grant Nos. 61505170, 61505171, and 51535003), the Joint Fund of the National Natural Science Foundation of China, the Chinese Academy of Engineering Physics (Grant No. U1530109), and the China Postdoctoral Science Foundation (Grant No. 2016M592709).

  1. Material removal and surface figure during pad polishing of fused silica

    Energy Technology Data Exchange (ETDEWEB)

    Suratwala, T I; Feit, M D; Steele, W A

    2009-05-04

    The material removal and surface figure after ceria pad polishing of fused silica glass have been measured and analyzed as a function of kinematics, loading conditions, and polishing time. Also, the friction at the workpiece/lap interface, the slope of the workpiece relative to the lap plane, and lap viscoelastic properties have been measured and correlated to material removal. The results show that the relative velocity between the workpiece & lap (determined by the kinematics) and the pressure distribution determine the spatial and temporal material removal and hence the final surface figure of the workpiece. In the case where the applied loading and relative velocity distribution over the workpiece are spatially uniform, a significant non-uniform spatial material removal from the workpiece surface is observed. This is due to a non-uniform pressure distribution resulting from: (1) a moment caused by a pivot point and interface friction forces; (2) viscoelastic relaxation of the polyurethane lap; and (3) a physical workpiece/lap interface mismatch. Both the kinematics and these contributions to the pressure distribution are quantitatively described, and then combined to form a spatial and temporal Preston model & code for material removal (called Surface Figure or SurF{copyright}). The surface figure simulations are consistent with the experiment for a wide variety of polishing conditions. This study is an important step towards deterministic full-aperture polishing, which would allow optical glass fabrication to be performed in a more repeatable, less iterative, and hence more economical manner.

  2. Determination of laser damage initiation probability and growth on fused silica scratches

    Energy Technology Data Exchange (ETDEWEB)

    Norton, M A; Carr, C W; Cross, D A; Negres, R A; Bude, J D; Steele, W A; Monticelli, M V; Suratwala, T I

    2010-10-26

    Current methods for the manufacture of optical components inevitably leaves a variety of sub-surface imperfections including scratches of varying lengths and widths on even the finest finishes. It has recently been determined that these finishing imperfections are responsible for the majority of laser-induced damage for fluences typically used in ICF class lasers. We have developed methods of engineering subscale parts with a distribution of scratches mimicking those found on full scale fused silica parts. This much higher density of scratches provides a platform to measure low damage initiation probabilities sufficient to describe damage on large scale optics. In this work, damage probability per unit scratch length was characterized as a function of initial scratch width and post fabrication processing including acid-based etch mitigation processes. The susceptibility of damage initiation density along scratches was found to be strongly affected by the post etching material removal and initial scratch width. We have developed an automated processing procedure to document the damage initiations per width and per length of theses scratches. We show here how these tools can be employed to provide predictions of the performance of full size optics in laser systems operating at 351 nm. In addition we use these tools to measure the growth rate of a damage site initiated along a scratch and compare this to the growth measured on an isolated damage site.

  3. Spherical fused silica cells filled with pure helium for nuclear magnetic resonance-magnetometry

    Energy Technology Data Exchange (ETDEWEB)

    Maul, Andreas; Blümler, Peter, E-mail: bluemler@uni-mainz.de; Heil, Werner; Nikiel, Anna; Otten, Ernst [Institute of Physics, Johannes Gutenberg University, Staudingerweg 7, 55128 Mainz (Germany); Petrich, Andreas; Schmidt, Thomas [ifw Günter-Köhler-Institut für Fügetechnik und Werkstoffprüfung GmbH, Otto-Schott-Str. 13, 07745 Jena (Germany)

    2016-01-15

    High magnetic fields (>1 T) are measured by NMR magnetometers with unrivaled precision if the precessing spin sample provides long coherence times. The longest coherence times are found in diluted {sup 3}He samples, which can be hyperpolarized for sufficient signal strength. In order to have minimal influence on the homogeneity and value of the measured magnetic field, the optimal container for the {sup 3}He should be a perfect sphere. A fused silica sphere with an inner diameter of 8 mm and an outer diameter of 12 mm was made from two hemispheres by diffusion bonding leaving only a small hole for cleaning and evacuation. This hole was closed in vacuum by a CO{sub 2} laser and the inner volume was filled with a few mbars of {sup 3}He via wall permeation. NMR-measurements on such a sample had coherence times of 5 min. While the hemispheres were produced with <1 μm deviation from sphericity, the bonding left a step of ca. 50 μm at maximum. The influence of such a mismatch, its orientation, and the immediate environment of the sample is analyzed by FEM-simulations and discussed in view of coherence times and absolute field measurements.

  4. [Reparation and application of perfluorodecyl modified silica monolithic capillary column in extraction and enrichment of perfluorooctane sulfonates].

    Science.gov (United States)

    Huang, Ke; Zhou, Naiyuan; Chen, Bo

    2011-10-01

    A perfluorodecyl modified silica monolithic capillary column has been prepared by using sol-gel method. The preparation steps included hydrolysis of alkoxy silane, fasculation of silanol, gelation, aging, meso-pore preparation, drying and surface modification. It could be used as a solid phase extraction (SPE) microcolumn for extraction and enrichment of perfluorooctane sulfonate (PFOS). The enrichment characteristics and efficiency of the perfluorodecyl modified monolithic silica capillary column has been investigated and compared with C18 silica monolithic capillary column. The results indicated that the perfluorodecyl modified silica monolithic capillary column ( 15 cm x 75 microm) had a higher adsorption capacity and a better enrichment selectivity for PFOS. The average adsorption capacity of the perfluorodecyl modified silica monolithic capillary column was 75 ng. And when the PFOS mass concentration in sample was 0. 25 mg/L, the enrichment factor was 29-fold in average. Owing to the good performance of the perfluorodecyl modified silica monolithic capillary column, it can be used for the extraction and enrichment of trace PFOS in water to meet the requirements of water quality monitoring and analysis.

  5. Second harmonic generation via femtosecond laser fabrication of poled, quasi-phase-matched waveguides in fused silica.

    Science.gov (United States)

    Ng, Jason C; Herman, Peter R; Qian, Li

    2017-01-15

    Second harmonic generation (SHG) is demonstrated in femtosecond laser written waveguides in fused silica through a combination of thermal poling and laser-based quasi-phase-matching (QPM) techniques. Quasi-phase-matching was controlled by the periodic erasure of induced nonlinearity through femtosecond laser erasure. A maximum SHG conversion efficiency of 6.6±0.5×10-5%/W is reported for the fundamental wavelength of 1552.8 nm with a phase-matching bandwidth of 4.4 nm for a 10.0 mm long waveguide. For a shorter sample, an effective second-order nonlinearity of χ(2)=0.012±0.001  pm/V was measured. Chirped QPM structures for wider SHG bandwidths also were demonstrated. Such periodically poled waveguides are promising for introducing nonlinear optical components within the 3D passive optical circuits that can be flexibly formed in fused silica by femtosecond laser writing.

  6. Detailed subsurface damage measurement and efficient damage-free fabrication of fused silica optics assisted by ion beam sputtering.

    Science.gov (United States)

    Liao, Wenlin; Dai, Yifan; Liu, Zongzheng; Xie, Xuhui; Nie, Xuqing; Xu, Mingjin

    2016-02-22

    Formation of subsurface damage has an inseparable relationship with microscopic material behaviors. In this work, our research results indicate that the formation process of subsurface damage often accompanies with the local densification effect of fused silica material, which seriously influences microscopic material properties. Interestingly, we find ion beam sputtering (IBS) is very sensitive to the local densification, and this microscopic phenomenon makes IBS as a promising technique for the detection of nanoscale subsurface damages. Additionally, to control the densification effect and subsurface damage during the fabrication of high-performance optical components, a combined polishing technology integrating chemical-mechanical polishing (CMP) and ion beam figuring (IBF) is proposed. With this combined technology, fused silica without subsurface damage is obtained through the final experimental investigation, which demonstrates the feasibility of our proposed method.

  7. An AC phase measuring interferometer for measuring dn/dT of fused silica and calcium fluoride at 193 nm

    Energy Technology Data Exchange (ETDEWEB)

    Shagam, R.N.

    1998-09-01

    A novel method for the measurement of the change in index of refraction vs. temperature (dn/dT) of fused silica and calcium fluoride at the 193 nm wavelength has been developed in support of thermal modeling efforts for the development of 193 nm-based photolithographic exposure tools. The method, based upon grating lateral shear interferometry, uses a transmissive linear grating to divide a 193 nm laser beam into several beam paths by diffraction which propagate through separate identical material samples. One diffracted order passing through one sample overlaps the undiffracted beam from a second sample and forms interference fringes dependent upon the optical path difference between the two samples. Optical phase delay due to an index change from heating one of the samples causes the interference fringes to change sinusoidally with phase. The interferometer also makes use of AC phase measurement techniques through lateral translation of the grating. Results for several samples of fused silica and calcium fluoride are demonstrated.

  8. Monolithic silica-based capillary reversed-phase liquid chromatography/electrospray mass spectrometry for plant metabolomics

    NARCIS (Netherlands)

    Tolstikov, V.V.; Lommen, A.; Nakanishi, K.; Tanaka, N.; Fiehn, O.

    2003-01-01

    Application of C18 monolithic silica capillary columns in HPLC coupled to ion trap mass spectrometry detection was studied for probing the metabolome of the model plant Arabidopsis thaliana. It could be shown that the use of a long capillary column is an easy and effective approach to reduce ionizat

  9. Optical and electrical properties of boron doped diamond thin conductive films deposited on fused silica glass substrates

    Science.gov (United States)

    Ficek, M.; Sobaszek, M.; Gnyba, M.; Ryl, J.; Gołuński, Ł.; Smietana, M.; Jasiński, J.; Caban, P.; Bogdanowicz, R.

    2016-11-01

    This paper presents boron-doped diamond (BDD) film as a conductive coating for optical and electronic purposes. Seeding and growth processes of thin diamond films on fused silica have been investigated. Growth processes of thin diamond films on fused silica were investigated at various boron doping level and methane admixture. Two step pre-treatment procedure of fused silica substrate was applied to achieve high seeding density. First, the substrates undergo the hydrogen plasma treatment then spin-coating seeding using a dispersion consisting of detonation nanodiamond in dimethyl sulfoxide with polyvinyl alcohol was applied. Such an approach results in seeding density of 2 × 1010 cm-2. The scanning electron microscopy images showed homogenous, continuous and polycrystalline surface morphology with minimal grain size of 200 nm for highly boron doped films. The sp3/sp2 ratio was calculated using Raman spectra deconvolution method. A high refractive index (range of 2.0-2.4 @550 nm) was achieved for BDD films deposited at 500 °C. The values of extinction coefficient were below 0.1 at λ = 550 nm, indicating low absorption of the film. The fabricated BDD thin films displayed resistivity below 48 Ohm cm and transmittance over 60% in the visible wavelength range.

  10. High resolution characterization of modifications in fused silica after exposure to low fluence 355 nm laser at different repetition frequencies.

    Science.gov (United States)

    Li, C H; Ju, X; Jiang, X D; Huang, J; Zhou, X D; Zheng, Z; Wu, W D; Zheng, W G; Li, Z X; Wang, B Y; Yu, X H

    2011-03-28

    We report on the characterization of modifications in fused silica after exposure to low fluence (2 J/cm2) 355 nm laser at repetition frequencies of 1 Hz, 5 Hz and 10 Hz. Synchrotron based XRF spectroscopy is employed to study concentration variation of metal inclusions in the surface layer. Positron annihilation lifetime spectroscopy is used to probe atomic size defects variation in bulk silica. FT-IR is used to characterize changes of bond length and angle of Si-O-Si covalent bond of irradiated silica. Compared to the basic frequency, the big loss of cerium and iron concentration, the size enlargement of vacancy cluster and the decrease of Si-O-Si covalent bond length after 10 Hz laser irradiation are illustrated by our data. These tiny modifications provide important data to investigate laser damage mechanism.

  11. Dental composite resins containing silica-fused ceramic single-crystalline whiskers with various filler levels.

    Science.gov (United States)

    Xu, H H

    1999-07-01

    Currently available direct-filling composite resins are susceptible to fracture and hence are not recommended for use in large stress-bearing posterior restorations involving cusps. The glass fillers in composites provide only limited reinforcement because of the brittleness and low strength of glass. The aim of the present study was to use ceramic single-crystalline whiskers as fillers to reinforce composites, and to investigate the effect of whisker filler level on composite properties. Silica particles were fused onto the whiskers to facilitate silanization and to roughen the whiskers, thereby improving retention in the matrix. The composite flexural strength, elastic modulus, hardness, and degree of polymerization conversion were measured as a function of whisker filler mass fraction, which ranged from 0% to 70%. Selected composites were polished simulating clinical procedures, and the surface roughness was measured with profilometry. The whisker composite with a filler mass fraction of 55% had a flexural strength (mean +/- SD; n = 6) of 196+/-10 MPa, significantly higher than 83+/-14 MPa of a microfill and 120+/-16 MPa of a hybrid composite control (family confidence coefficient = 0.95; Tukey's multiple comparison). The composite modulus and hardness increased monotonically with filler level. The flexural strength first increased, then plateaued with increasing filler level. The degree of conversion decreased with increasing filler level. The whisker composite had a polished surface roughness similar to that of a conventional hybrid composite (p>0.1; Student's t). To conclude, ceramic whisker reinforcement can significantly improve the mechanical properties of composite resins; the whisker filler level plays a key role in determining composite properties; and the reinforcement mechanisms appear to be crack pinning by whiskers and friction from whisker pullout resisting crack propagation.

  12. Influence of Cutting Speed on Subsurface Damage Morphology and Distribution in Ground Fused Silica

    Directory of Open Access Journals (Sweden)

    Georg Schnurbusch

    2017-08-01

    Full Text Available In optical fabrication, brittle-hard materials are used for numerous applications. Especially for high-performance optics for laser or lithography applications, a complex and consistent production chain is necessary to account for the material properties. Particularly in pre-processing, e.g., for shaping optical components, brittle material behavior is dominant which leads to a rough surface layer with cracks that reach far below the surface. This so called subsurface damage (SSD needs to be removed in subsequent processes like polishing. Therefore, it is essential to know the extent of the SSD induced by shaping for an efficient design of precise corrective processes and for process improvement. Within this work the influence of cutting speed on SSD, in fused silica, induced by grinding has been investigated. To analyze the subsurface crack distribution and the maximum crack depth magnetorheological finishing has been appointed to polish a wedge into the ground surface. The depth profile of SSD was analyzed by image processing. For this purpose a coherent area of the polished wedge has been recorded by stitching microscopy. Taking the form deviation of the ground surface in to account to determine the actual depth beneath surface, the accuracy of the SSD-evaluation could be improved significantly. The experiments reveal a clear influence of the cutting speed on SSD, higher cutting speeds generate less SSD. Besides the influence on the maximum crack depth an influence on the crack length itself could be verified. Based on image analysis it was possible, to predict the maximum depth of cracks by means of crack length.

  13. Ultra-high-Q microcavities fabricated on fused silica chips with three-dimentional arrangement by femtosecond laser direct writing

    CERN Document Server

    Lin, Jintian; Ma, Yaoguang; Fang, Wei; He, Fei; Qiao, Lingling; Tong, Limin; Cheng, Ya; Xu, Zhizhan

    2011-01-01

    We report on the fabrication of ultra-high-Q whispering gallery microcavities on a fused silica chip by femtosecond laser microfabriction, enabled by the high spatial resolution and three-dimensional nature of femtosecond laser direct writing. The processing mainly consists of two steps: (1) formation of freestanding microdisks by femtosecond laser direct writing and subsequent chemical wet etching; and (2) transformation of microdisks to microtoroids by annealing with CO2 laser. We show that three-dimensionally arranged ultra-high Q microcavities with a Q-factor up to 1.07x10^6 can be achieved.

  14. Formation of laser-induced periodic surface structures on fused silica upon two-color double-pulse irradiation

    Science.gov (United States)

    Höhm, S.; Herzlieb, M.; Rosenfeld, A.; Krüger, J.; Bonse, J.

    2013-12-01

    The formation of laser-induced periodic surface structures (LIPSS) upon irradiation of fused silica with multiple irradiation sequences consisting of laser pulse pairs (50 fs single-pulse duration) of two different wavelengths (400 and 800 nm) is studied experimentally. Parallel polarized double-pulse sequences with a variable delay Δt between -10 and +10 ps and between the individual fs-laser pulses were used to investigate the LIPSS periods versus Δt. These two-color experiments reveal the importance of the ultrafast energy deposition to the silica surface by the first laser pulse for LIPSS formation. The second laser pulse subsequently reinforces the previously seeded spatial LIPSS frequencies.

  15. Formation of laser-induced periodic surface structures on fused silica upon two-color double-pulse irradiation

    Energy Technology Data Exchange (ETDEWEB)

    Höhm, S.; Herzlieb, M.; Rosenfeld, A. [Max-Born-Institut für Nichtlineare Optik und Kurzzeitspektroskopie (MBI), Max-Born-Straße 2A, D-12489 Berlin (Germany); Krüger, J.; Bonse, J. [BAM Bundesanstalt für Materialforschung und –prüfung, Unter den Eichen 87, D-12205 Berlin (Germany)

    2013-12-16

    The formation of laser-induced periodic surface structures (LIPSS) upon irradiation of fused silica with multiple irradiation sequences consisting of laser pulse pairs (50 fs single-pulse duration) of two different wavelengths (400 and 800 nm) is studied experimentally. Parallel polarized double-pulse sequences with a variable delay Δt between −10 and +10 ps and between the individual fs-laser pulses were used to investigate the LIPSS periods versus Δt. These two-color experiments reveal the importance of the ultrafast energy deposition to the silica surface by the first laser pulse for LIPSS formation. The second laser pulse subsequently reinforces the previously seeded spatial LIPSS frequencies.

  16. Time dependency of the laser-induced nanostructuring process of chromium layers with different thicknesses on fused silica

    Energy Technology Data Exchange (ETDEWEB)

    Lorenz, P., E-mail: pierre.lorenz@iom-leipzig.de [Leibniz-Institut für Oberflächenmodifizierung e. V., Permoserstr. 15, D-04318 Leipzig (Germany); Klöppel, M. [Institute of Scientific Computation, Department of Mathematics, TU Dresden, D-01062 Dresden (Germany); Smausz, T. [Department of Optics and Quantum Electronics, University of Szeged, H-6720 Szeged, Dóm tér 9 (Hungary); MTA-SZTE Research Group on Photoacoustic Spectroscopy, University of Szeged, H-6720 Szeged, Dóm tér 9 (Hungary); Csizmadia, T. [Department of Optics and Quantum Electronics, University of Szeged, H-6720 Szeged, Dóm tér 9 (Hungary); Ehrhardt, M.; Zimmer, K. [Leibniz-Institut für Oberflächenmodifizierung e. V., Permoserstr. 15, D-04318 Leipzig (Germany); Hopp, B. [Department of Optics and Quantum Electronics, University of Szeged, H-6720 Szeged, Dóm tér 9 (Hungary)

    2015-05-01

    Highlights: • The ns laser-induced melting effect of thin Cr layers on fused silica was studied. • The molten layer was analyzed by study of the time-dependent optical properties. • The liquid phase lifetime Δt{sub LF} depends on the metal thickness and the fluence. • The Δt{sub LF} dependency can be well described by an analytic function. • The comparison of the results with FEM simulation yields to a moderate agreement. - Abstract: Nanostructures exhibit a raised importance in manifold application fields like electronics and optics. The laser irradiation of thin metal layers allows the fabrication of metal nanostructures induced by a melting and deformation process where the resultant structures are dependent on the laser and metal layer parameters. However, for an optimization of this process a detailed physical understanding is necessary. Therefore, the dynamics of the metal layer deformation process was measured by time-dependent reflection and transmission as well as shadow graph measurements at different KrF excimer laser parameters (laser fluence and number of laser pulses) and metal layer thicknesses were used. Magnetron-sputtered thin chromium films with a thickness from 10 to 100 nm on fused silica substrates were studied. Based on the optical measurements the liquid phase lifetime of the metal was estimated and compared with the calculated lifetime using a simple thermodynamic model.

  17. Results of applying a non-evaporative mitigation technique to laser-initiated surface damage on fused-silica

    Energy Technology Data Exchange (ETDEWEB)

    Adams, J J; Bolourchi, M; Bude, J D; Guss, G M; Matthews, M J; Nostrand, M C

    2010-10-26

    We present results from a study to determine an acceptable CO{sub 2} laser-based non-evaporative mitigation protocol for use on surface damage sites in fused-silica optics. A promising protocol is identified and evaluated on a set of surface damage sites created under ICF-type laser conditions. Mitigation protocol acceptability criteria for damage re-initiation and growth, downstream intensification, and residual stress are discussed. In previous work, we found that a power ramp at the end of the protocol effectively minimizes the residual stress (<25 MPa) left in the substrate. However, the biggest difficulty in determining an acceptable protocol was balancing between low re-initiation and problematic downstream intensification. Typical growing surface damage sites mitigated with a candidate CO{sub 2} laser-based mitigation protocol all survived 351 nm, 5 ns damage testing to fluences >12.5 J/cm{sup 2}. The downstream intensification arising from the mitigated sites is evaluated, and all but one of the sites has 100% passing downstream damage expectation values. We demonstrate, for the first time, a successful non-evaporative 10.6 {micro}m CO{sub 2} laser mitigation protocol applicable to fused-silica optics used on fusion-class lasers like the National Ignition Facility (NIF).

  18. Mitigation of Laser Damage Growth in Fused Silica NIF Optics with a Galvanometer Scanned Carbon Dioxide Laser

    Energy Technology Data Exchange (ETDEWEB)

    Bass, I L; Draggoo, V; Guss, G M; Hackel, R P; Norton, M A

    2006-04-06

    Economic operation of the National Ignition Facility at the Lawrence Livermore National Laboratory depends on controlling growth of laser damage in the large, high cost optics exposed to UV light at 351 nm. Mitigation of the growth of damage sites on fused silica surfaces greater than several hundred microns in diameter has been previously reported by us using galvanometer scanning of a tightly focused 10.6 {micro}m CO{sub 2} laser spot over an area encompassing the laser damage. Further investigation revealed that fused silica vapor re-deposited on the surface as ''debris'' led to laser damage at unexpectedly low fluences when exposed to multiple laser shots at 351 nm. Additionally, laser power and spatial mode fluctuations in the mitigation laser led to poor repeatability of the process. We also found that the shape of the mitigation pit could produce downstream intensification that could damage other NIF optics. Modifications were made to both the laser system and the mitigation process in order to address these issues. Debris was completely eliminated by these changes, but repeatability and downstream intensification issues still persist.

  19. Localized CO2 laser treatment and post-heating process to reduce the growth coefficient of fused silica surface damage

    Institute of Scientific and Technical Information of China (English)

    Shizhen Xu; Xiaotao Zu; Xiaodong Yuan

    2011-01-01

    The lifetime of optical components in high-fluence ultraviolet (UV) laser applications is typically limited by laser-initiated damage and its subsequent growth. Using 10.6-μm CO2 laser pulses, we successfully mitigate 355-nm laser induced damage sites on fused silica surface with dimensions less than 200 μm.The damage threshold increases and the damage growth mitigates. However, the growth coefficients of new damage on the CO2 laser processed area are higher than those of the original sample. The damage grows with crack propagation for residual stress after CO2 laser irradiation. Furthermore, post-heating is beneficial to the release of residual stress and slows down the damage growth.%@@ The lifetime of optical components in high-fluence ultraviolet (UV) laser applications is typically limited by laser-initiated damage and its subsequent growth.Using 10.6-μm CO2 laser pulses, we successfully mitigate 355-nm laser induced damage sites on fused silica surface with dimensions less than 200 μm.The damage threshold increases and the damage growth mitigates.However, the growth coefficients of new damage on the CO2 laser processed area are higher than those of the original sample.The damage grows with crack propagation for residual stress after CO2 laser irradiation.Furthermore, post-heating is beneficial to the release of residual stress and slows down the damage growth.

  20. Formation of plano-convex micro-lens array in fused silica glass using CO2 laser assisted reshaping technique

    CERN Document Server

    Sohn, Ik-Bu; Yoo, Dongyoon; Noh, Young-Chul; Ahsan, Md Shamim; Sung, Jae-Hee; Lee, Seong-Ku

    2016-01-01

    We report on fabricating high-fill-factor plano-convex spherical and square micro-lens arrays on fused silica glass surface using CO2 laser assisted reshaping technique. Initially, periodic micro-pillars have been encoded on the glass surface by means of a femtosecond laser beam. Afterwards, the micro-pillars are polished several times by irradiating a CO2 laser beam on top of the micro-pillars. Consequently, spherical micro-lens array with micro-lens size of 50 um x 50 um and square micro-lens array with micro-lens size of 100 um x 100 um are formed on fused silica glass surface. We also study the intensity distribution of light passed through the spherical micro-lens array engraved glass sample. The simulation result shows that, the focal length of the spherical micro-lens array is 35 um. Furthermore, we investigate the optical properties of the micro-lens array engraved glass samples. The proposed CO2 laser based reshaping technique is simple and fast that shows promises in fabrication arrays of smooth mic...

  1. Combined Advanced Finishing and UV-Laser Conditioning for Producing UV-Damage-Resistant Fused Silica Optics

    Energy Technology Data Exchange (ETDEWEB)

    Menapace, J A; Penetrante, B; Golini, D; Slomba, A; Miller, P E; Parham, T; Nichols, M; Peterson, J

    2001-11-01

    Laser induced damage initiation on fused silica optics can limit the lifetime of the components when used in high power UV laser environments. Foe example in inertial confinement fusion research applications, the optics can be exposed to temporal laser pulses of about 3-nsec with average fluences of 8 J/cm{sup 2} and peak fluences between 12 and 15 J/cm{sup 2}. During the past year, we have focused on optimizing the damage performance at a wavelength of 355-nm (3{omega}), 3-nsec pulse length, for optics in this category by examining a variety of finishing technologies with a challenge to improve the laser damage initiation density by at least two orders of magnitude. In this paper, we describe recent advances in improving the 3{omega} damage initiation performance of laboratory-scale zirconium oxide and cerium oxide conventionally finished fused silica optics via application of processes incorporating magnetorheological finishing (MRF), wet chemical etching, and UV laser conditioning. Details of the advanced finishing procedures are described and comparisons are made between the procedures based upon large area 3{omega} damage performance, polishing layer contamination, and optical subsurface damage.

  2. The Effect of HF/NH4F Etching on the Morphology of Surface Fractures on Fused Silica

    Energy Technology Data Exchange (ETDEWEB)

    Wong, L; Suratwala, T; Feit, M D; Miller, P E; Steele, R A

    2008-04-03

    The effects of HF/NH{sub 4}F, wet chemical etching on the morphology of individual surface fractures (indentations, scratches) and of an ensemble of surface fractures (ground surfaces) on fused silica glass has been characterized. For the individual surface fractures, a series of static or dynamic (sliding) Vickers and Brinnell indenters were used to create radial, lateral, Hertzian cone and trailing indentation fractures on a set of polished fused silica substrates which were subsequently etched. After short etch times, the visibility of both surface and subsurface cracks is significantly enhanced when observed by optical microscopy. This is attributed to the removal of the polishing-induced Bielby layer and the increased width of the cracks following etching allowing for greater optical scatter at the fracture interface. The removal of material during etching was found to be isotropic except in areas where the etchant has difficulty penetrating or in areas that exhibit significant plastic deformation/densification. Isolated fractures continue to etch, but will never be completely removed since the bottom and top of the crack both etch at the same rate. The etching behavior of ensembles of closely spaced cracks, such as those produced during grinding, has also been characterized. This was done using a second set of fused silica samples that were ground using either fixed or loose abrasives. The resulting samples were etched and both the etch rate and the morphology of the surfaces were monitored as a function of time. Etching results in the formation of a series of open cracks or cusps, each corresponding to the individual fractures originally on the surface of the substrate. During extended etching, the individual cusps coalesce with one another, providing a means of reducing the depth of subsurface damage and the peak-to-valley roughness. In addition, the material removal rate of the ground surfaces was found to scale with the surface area of the cracks as a

  3. Multilevel kinoform microlens arrays in fused silica for high-power laser optics

    Science.gov (United States)

    Atuchin, Victor V.; Soldatenkov, I. S.; Kirpichnikov, A. V.; Mikhailov, E. V.; Pestryakov, Efim V.; Sheglov, Dmitriy V.

    2004-03-01

    Diffraction microlens arrays has been fabricated in silica substrates by deep UV photolithography and wet chemical etching. The calculated kinoform profile has been approximated by multistep function and this microrelief has been transfered into the surface with wet etching through the photoresist mask. The diffraction efficiency of eight-level kinoform microlens is as high as 85%.

  4. Polarization-independent etching of fused silica based on electrons dynamics control by shaped femtosecond pulse trains for microchannel fabrication.

    Science.gov (United States)

    Yan, X; Jiang, L; Li, X; Zhang, K; Xia, B; Liu, P; Qu, L; Lu, Y

    2014-09-01

    We propose an approach to realize polarization-independent etching of fused silica by using temporally shaped femtosecond pulse trains to control the localized transient electrons dynamics. Instead of nanograting formation using traditional unshaped pulses, for the pulse delay of pulse trains larger than 1 ps, coherent field-vector-related coupling is not possible and field orientation is lost. The exponential growth of the periodic structures is interrupted. In this case, disordered and interconnected nanostructures are formed, which is probably the main reason of etching independence on the laser polarization. As an application example, square-wave-shaped and arc-shaped microchannels are fabricated by using pulse trains to demonstrate the advantage of the proposed method in fabricating high-aspect-ratio and three-dimensional microchannels.

  5. Observation of nonlinear optical phenomena in fused silica and air using a 100 GW, 1.54 um source.

    Energy Technology Data Exchange (ETDEWEB)

    Rudd, James Van; Law, R. J.; Luk, Ting Shan; Naudeau, Madeline L.; Nelson, Thomas Robert; Cameron, Stewart M.

    2006-02-01

    A 100-GW optical parametric chirped-pulse amplifier system is used to study nonlinear effects in the 1.54 {micro}m regime. When focusing this beam in air, strong third-harmonic generation (THG) is observed, and both the spectra and efficiency are measured. Broadening is observed on only the blue side of the third-harmonic signal and an energy conversion efficiency of 0.2% is achieved. When propagated through a 10-cm block of fused silica, a collimated beam is seen to collapse and form multiple filaments. The measured spectral features span 400-2100 nm. The spectrum is dominated by previously unobserved Stokes emissions and broad emissions in the visible.

  6. Mechanical quality factor measurements of monolithically suspended fused silica test masses of the GEO 600 gravitational wave detector

    Energy Technology Data Exchange (ETDEWEB)

    Smith, J R [Max-Planck-Institute for Gravitational Physics (Albert-Einstein-Institute) and University of Hannover, Callinstr. 38, D-30167 Hannover (Germany); Cagnoli, G [Institute for Gravitational Research, Department of Physics and Astronomy, University of Glasgow, Glasgow G12 8QQ (United Kingdom); Crooks, D R M [Institute for Gravitational Research, Department of Physics and Astronomy, University of Glasgow, Glasgow G12 8QQ (United Kingdom); Fejer, M M [Edward L Ginzton Laboratory, Stanford University, Stanford, CA 94305-4088 (United States); Gossler, S [Max-Planck-Institute for Gravitational Physics (Albert-Einstein-Institute) and University of Hannover, Callinstr. 38, D-30167 Hannover (Germany); Lueck, H [Max-Planck-Institute for Gravitational Physics (Albert-Einstein-Institute) and University of Hannover, Callinstr. 38, D-30167 Hannover (Germany); Rowan, S [Institute for Gravitational Research, Department of Physics and Astronomy, University of Glasgow, Glasgow G12 8QQ (United Kingdom); Hough, J [Institute for Gravitational Research, Department of Physics and Astronomy, University of Glasgow, Glasgow G12 8QQ (United Kingdom); Danzmann, K [Max-Planck-Institute for Gravitational Physics (Albert-Einstein-Institute) and University of Hannover, Callinstr. 38, D-30167 Hannover (Germany)

    2004-03-07

    Internal thermal noise is expected to be a limiting noise source in the most sensitive frequency band of the GEO 600 gravitational wave detector. Because thermal noise is directly related to energy dissipation, care has been taken to construct test mass suspensions from low-dissipation materials and to eliminate inter-material rubbing where possible. Recently, the GEO 600 team finished the installation of triple-pendulum suspensions for the optics of the Michelson interferometer. Each of these triple pendulums incorporates a monolithic fused silica pendulum as the lowest stage. We have made internal mode quality factor measurements of three monolithically suspended test masses. Using these measurements we estimate of the level of internal thermal noise in the GEO 600 interferometer.

  7. Mechanical quality factor measurements of monolithically suspended fused silica test masses of the GEO 600 gravitational wave detector

    Science.gov (United States)

    Smith, J. R.; Cagnoli, G.; Crooks, D. R. M.; Fejer, M. M.; Goßler, S.; Lück, H.; Rowan, S.; Hough, J.; Danzmann, K.

    2004-03-01

    Internal thermal noise is expected to be a limiting noise source in the most sensitive frequency band of the GEO 600 gravitational wave detector. Because thermal noise is directly related to energy dissipation, care has been taken to construct test mass suspensions from low-dissipation materials and to eliminate inter-material rubbing where possible. Recently, the GEO 600 team finished the installation of triple-pendulum suspensions for the optics of the Michelson interferometer. Each of these triple pendulums incorporates a monolithic fused silica pendulum as the lowest stage. We have made internal mode quality factor measurements of three monolithically suspended test masses. Using these measurements we estimate of the level of internal thermal noise in the GEO 600 interferometer.

  8. DEVELOPMENT OF FUSED-CORE SILICA HPLC COLUMNS AND THEIR RECENT PHARMACEUTICAL AND BIOLOGICAL APPLICATIONS: A REVIEW

    Directory of Open Access Journals (Sweden)

    Ruwida Kamour*, Amal Ammar, Mohamed El-Attug and Tariq Almog

    2013-11-01

    Full Text Available In many analytical procedures, fast and reliable analysis technique is required. The development of HPLC stationary phases were in line with these goals. To achieve these goals of fast and efficient analysis, work was focused on reducing particle size of packing materials. Therefore, the development of superficially porous silica particles provided a new approach with overwhelming operating results to insure fast and reliable analysis at decreased system back pressure values. This work presents features and development aspects of fused core technology. Also it describes their chromatographic properties in comparison with monolithic and sub-2 µm particle columns. In addition, there is a discussion of its applicability to be used with conventional HPLC instruments. Finally, it outlines some of its recent applications in biological and pharmaceutical field.

  9. Effect of rapid thermal annealing on polycrystalline InGaN thin films deposited on fused silica substrates

    Energy Technology Data Exchange (ETDEWEB)

    Kazazis, S.A., E-mail: kazazis@physics.uoc.gr [Department of Physics, University of Crete, P.O. Box 2208, 71003 Heraklion (Greece); Papadomanolaki, E. [Department of Physics, University of Crete, P.O. Box 2208, 71003 Heraklion (Greece); Androulidaki, M.; Tsagaraki, K.; Kostopoulos, A.; Aperathitis, E. [Microelectronics Research Group, IESL-FORTH, P.O. Box 1385, 71110 Heraklion (Greece); Iliopoulos, E. [Department of Physics, University of Crete, P.O. Box 2208, 71003 Heraklion (Greece); Microelectronics Research Group, IESL-FORTH, P.O. Box 1385, 71110 Heraklion (Greece)

    2016-07-29

    In this work, we report on the effects of Rapid Thermal Annealing (RTA) on the structural, electrical and optical properties of polycrystalline InGaN thin films deposited on amorphous fused silica substrates by molecular beam deposition. Films with 20%, 35% and 50% indium content were grown and subjected to post-deposition RTA treatments. Annealing promoted crystallization in the case of the film with 0.5 InN mole fraction while in the lower indium content cases no apparent effect on the improvement of crystallinity was observed. For RTA temperature above 550 °C, film resistivity was reduced by at least two orders of magnitude due to annealing-induced increased carrier concentration. The optical properties of the films were systematically studied by variable angle spectroscopic ellipsometry. In the highest indium content films, a monotonic optical band gap widening was observed upon annealing, explained by the Burstein–Moss effect. In contrast, photoluminescence peak position was not affected by the resulting Fermi level changes. This is attributed to the different mechanisms between optical absorption and emission in such highly doped semiconductors. - Highlights: • Polycrystalline InGaN films were deposited on fused silica substrates. • Rapid thermal annealing effect on structural, electrical and optical properties studied. • Films' resistivity significantly reduced after annealing at 550 °C, in all InN content cases. • In higher indium content films, optical band gap blueshifts upon annealing, due to Burstein–Moss effect. • Photoluminescence emission position was unaffected by the band gap shift.

  10. Comparison of laser-based mitigation of fused silica surface damage using mid- versus far-infrared lasers

    Energy Technology Data Exchange (ETDEWEB)

    Yang, S T; Matthews, M J; Elhadj, S; Cooke, D; Guss, G M; Draggoo, V G; Wegner, P J

    2009-12-16

    Laser induced growth of optical damage can limit component lifetime and therefore operating costs of large-aperture fusion-class laser systems. While far-infrared (IR) lasers have been used previously to treat laser damage on fused silica optics and render it benign, little is known about the effectiveness of less-absorbing mid-IR lasers for this purpose. In this study, they quantitatively compare the effectiveness and efficiency of mid-IR (4.6 {micro}m) versus far-IR (10.6 {micro}m) lasers in mitigating damage growth on fused silica surfaces. The non-linear volumetric heating due to mid-IR laser absorption is analyzed by solving the heat equation numerically, taking into account the temperature-dependent absorption coefficient {alpha}(T) at {lambda} = 4.6 {micro}m, while far-IR laser heating is well-described by a linear analytic approximation to the laser-driven temperature rise. In both cases, the predicted results agree well with surface temperature measurements based on infrared radiometry, as well as sub-surface fictive temperature measurements based on confocal Raman microscopy. Damage mitigation efficiency is assessed using a figure of merit (FOM) relating the crack healing depth to laser power required, under minimally-ablative conditions. Based on their FOM, they show that for cracks up to at least 500 {micro}m in depth, mitigation with a 4.6 {micro}m mid-IR laser is more efficient than mitigation with a 10.6 {micro}m far-IR laser. This conclusion is corroborated by direct application of each laser system to the mitigation of pulsed laser-induced damage possessing fractures up to 225 {micro}m in depth.

  11. An AFM determination of the effects on surface roughness caused by cleaning of fused silica and glass substrates in the process of optical biosensor preparation.

    Science.gov (United States)

    Henke, Lisa; Nagy, Noemi; Krull, Ulrich J

    2002-06-01

    The covalent attachment of organic films and of biological molecules to fused silica and glass substrates is important for many applications. For applications such as biosensor development, it is desired that the immobilised molecules be assembled in a uniform layer on the surface so as to provide for reproducibility and speed of surface interactions. For optimal derivatisation the surface must be appropriately cleaned to remove contamination, to create surface attachment sites such as hydroxyl groups, and to control surface roughness. The irregularity of the surface can be significant in defining the integrity and density of immobilised films. Numerous cleaning methods exist for fused silica and glass substrates and these include gas plasmas, and combinations of acids, bases and organic solvents that are allowed to react at varying temperatures. For many years, we have used a well established method based on a combination of washing with basic peroxide followed by acidic peroxide to clean and hydroxylate the surface of fused silica and glass substrates before oligonucleotide immobilisation. Atomic force microscopy (AFM) has been used to evaluate the effect of cleaning on surface roughness for various fused silica and glass samples. The results indicate that surface roughness remains substantial after use of this common cleaning routine, and can provide a surface area that is more than 10% but less than 30% larger than anticipated from geometric considerations of a planar surface.

  12. Effects of Ti charge state, ion size and beam-induced compaction on the formation of Ag metal nanoparticles in fused silica

    Science.gov (United States)

    Magruder, R. H.; Meldrum, A.; Haglund, R. F.

    2015-04-01

    Metal nanoparticles formed by ion implantation in fused silica exhibit linear and nonlinear optical properties that can be altered by co-doping the silica substrate with transition-metal ions. For example, implantation of scandium in fused silica creates a directional optical dichroism due to the different spatial distribution of silver nanoparticles subsequently formed by Ag ion implantation. In this paper, we show that implantation of titanium ions alters the short- and intermediate-range order in the silica and thereby alters the diffusion and nucleation processes that lead to formation of silver nanoparticles. In particular, the dichroic response observed for Ag nanoparticles in Sc-implanted silica is, with one exception, in Ti-implanted silica. Compaction of the silica due to the ion implantation process appears to be similar for both Sc and Ti implantations, based on the observed shift of the 1,124 cm-1 transverse-optical phonon mode in the infrared reflectance spectrum. However, differences in chemical reactivity, bond lengths and electronic structure of Sc and Ti produce changes in electronic structure and strain that are sensitively reflected in the reflectance spectra of the Ag nanoparticles. These differences lead to modifications in the size, shape and spatial distributions of the silver nanoparticles and offer a powerful means of controlling their optical properties.

  13. Thermo-mechanical simulations of CO{sub 2} laser–fused silica interactions

    Energy Technology Data Exchange (ETDEWEB)

    Doualle, T.; Gallais, L., E-mail: laurent.gallais@fresnel.fr [Aix-Marseille Université, CNRS, Centrale Marseille, Institut Fresnel UMR 7249, 13013 Marseille (France); Cormont, P.; Hébert, D.; Rullier, J.-L. [CEA-CESTA, 15 Avenue des Sablières, CS 60001, F33116 Le Barp Cedex (France); Combis, P. [CEA DAM Ile-de-France, F-91297 Arpajon (France)

    2016-03-21

    CO{sub 2} laser heating of silica glass is used in many scientific and industrial applications. Particularly, localized CO{sub 2} laser heating of silica glass has demonstrated its ability to mitigate surface damage on optics used for high power laser applications. To develop such applications, the control of temperature, heat affected area, and resulting mechanical stresses are critical. Therefore, it is necessary to understand the silica transformation, the material ejection, and the thermo-mechanical stresses induced by the laser heating and subsequent cooling. In this paper, we detail the development of comprehensive thermo-mechanical numerical simulations of these physical processes, based on finite-element method. The approach is developed for 2D or 3D cases to tackle the case of a moving beam at the surface of the sample, and we particularly discuss the choice of the different parameters based on bibliographic inputs. The thermal and mechanical numerical results have been compared to different dedicated experimental studies: infrared thermography measurements at the surface of the irradiated area, optical profilometry measurements of the laser-processed sites, and photo-elastic measurements. Very consistent results are obtained between numerical and experimental results for the description of the temperature gradients, the material ejection, and the residual stresses.

  14. Thermo-mechanical simulations of CO2 laser-fused silica interactions

    Science.gov (United States)

    Doualle, T.; Gallais, L.; Cormont, P.; Hébert, D.; Combis, P.; Rullier, J.-L.

    2016-03-01

    CO2 laser heating of silica glass is used in many scientific and industrial applications. Particularly, localized CO2 laser heating of silica glass has demonstrated its ability to mitigate surface damage on optics used for high power laser applications. To develop such applications, the control of temperature, heat affected area, and resulting mechanical stresses are critical. Therefore, it is necessary to understand the silica transformation, the material ejection, and the thermo-mechanical stresses induced by the laser heating and subsequent cooling. In this paper, we detail the development of comprehensive thermo-mechanical numerical simulations of these physical processes, based on finite-element method. The approach is developed for 2D or 3D cases to tackle the case of a moving beam at the surface of the sample, and we particularly discuss the choice of the different parameters based on bibliographic inputs. The thermal and mechanical numerical results have been compared to different dedicated experimental studies: infrared thermography measurements at the surface of the irradiated area, optical profilometry measurements of the laser-processed sites, and photo-elastic measurements. Very consistent results are obtained between numerical and experimental results for the description of the temperature gradients, the material ejection, and the residual stresses.

  15. Femtosecond laser writing of waveguide retarders in fused silica for polarization control in optical circuits.

    Science.gov (United States)

    Fernandes, Luís A; Grenier, Jason R; Herman, Peter R; Aitchison, J Stewart; Marques, Paulo V S

    2011-09-12

    Femtosecond laser (300 fs, 500 kHz, 522 nm) fabrication of optical waveguides in bulk silica glass is extended to waveguide retarders. We study the merits of nanograting orientation (perpendicular or parallel to the waveguide) for generating high and low birefringence waveguides. This is used together with other exposure condition to control the waveguide birefringence between 10⁻⁵ and 10⁻⁴ permitting for the simultaneous fabrication of the waveguides and the tuning of the retardance demonstrating quarter and half-wave retarders in the 1200 nm to 1700 nm spectrum. The wavelength dependence of the birefringence is also characterized over a range of exposure conditions.

  16. Study of CO2 laser smoothing of surface roughness in fused silica

    Energy Technology Data Exchange (ETDEWEB)

    Shen, N; Matthews, J; Fair, J E; Britten, J A; Nguyen, H T; Cooke, D; Elhadj, S; Henshaw, D; Guss, G M; Guss, G M; Yang, T

    2009-11-03

    Small micrometer-sized roughness on optical surfaces, caused by laser damage and/or redeposition of laser ablated material, can cause local electric field intensification which may lead to damage initiation both on the optics and/or downstream. We examined the smoothing of etched periodic surface structures on SiO{sub 2} substrate with 10.6 {micro}m CO{sub 2} laser using atomic force microscopy. The characteristic surface tension driven mass flow of the glass under different laser parameters were simulated using computational fluid dynamics and correlated with experimental results. We found that during CO{sub 2} laser polishing the estimate viscosity of the silica glass appears to be higher than typical literature values measured at a temperature similar to the laser heating conditions. This discrepancy can be explained by the observation that at high temperature, a significant portion of the hydroxyl content in the layer of heated silica glass can diffuse out resulting in a much stiffer glass.

  17. ANALYSIS OF ANIONIC METALLIZED AZO AND FORMAZAN DYES BY CAPILLARY ELECTROPHORESIS/MASS SPECTROMETRY

    Science.gov (United States)

    Capillary electrophoresis-mass spectrometry was applied to the separation of several anionic dyes containing copper(II), chromium(III), or cobalt(III) as part of the dye molecule. The dyes were separated using a 110 cmX50 mu m uncoated fused-silica capillary and a 5 mM ammonium a...

  18. Comparing the use of 4.6 um lasers versus 10.6 um lasers for mitigating damage site growth on fused silica surfaces

    Energy Technology Data Exchange (ETDEWEB)

    Yang, S T; Matthews, M J; Elhadj, S; Cooke, D; Guss, G M; Draggoo, V G; Wegner, P J

    2010-10-21

    The advantage of using mid-infrared (IR) 4.6 {micro}m lasers, versus far-infrared 10.6 {micro}m lasers, for mitigating damage growth on fused silica is investigated. In contrast to fused silica's high absorption at 10.6 {micro}m, silica absorption at 4.6 {micro}m is two orders of magnitude less. The much reduced absorption at 4.6 {micro}m enables deep heat penetration into fused silica when it is heated using the mid-IR laser, which in turn leads to more effective mitigation of damage sites with deep cracks. The advantage of using mid-IR versus far-IR laser for damage growth mitigation under non-evaporative condition is quantified by defining a figure of merit (FOM) that relates the crack healing depth to laser power required. Based on our FOM, we show that for damage cracks up to at least 500 {micro}m in depth, mitigation using a 4.6 {micro}m mid-IR laser is more efficient than mitigation using a 10.6 {micro}m far-IR laser.

  19. Effect of rogue particles on the sub-surface damage of fused silica during grinding/polishing

    Energy Technology Data Exchange (ETDEWEB)

    Suratwala, T I; Steele, R; Feit, M D; Wong, L; Miller, P E; Menapace, J A; Davis, P J

    2007-05-02

    The distribution and characteristics of surface cracks (i.e., sub-surface damage or scratching) on fused silica formed during grinding/polishing resulting from the addition of rogue particles in the base slurry has been investigated. Fused silica samples (10 cm diameter x 1 cm thick) were: (1) ground by loose abrasive grinding (alumina particles 9-30 {micro}m) on a glass lap with the addition of larger alumina particles at various concentrations with mean sizes ranging from 15-30 {micro}m, or (2) polished (using 0.5 {micro}m cerium oxide slurry) on various laps (polyurethanes pads or pitch) with the addition of larger rogue particles (diamond (4-45 {micro}m), pitch, dust, or dried Ceria slurry agglomerates) at various concentrations. For the resulting ground samples, the crack distributions of the as-prepared surfaces were determined using a polished taper technique. The crack depth was observed to: (1) increase at small concentrations (>10{sup -4} fraction) of rogue particles; and (2) increase with rogue particle concentration to crack depths consistent with that observed when grinding with particles the size of the rogue particles alone. For the polished samples, which were subsequently etched in HF:NH{sub 4}F to expose the surface damage, the resulting scratch properties (type, number density, width, and length) were characterized. The number density of scratches increased exponentially with the size of the rogue diamond at a fixed rogue diamond concentration suggesting that larger particles are more likely to lead to scratching. The length of the scratch was found to increase with rogue particle size, increase with lap viscosity, and decrease with applied load. At high diamond concentrations, the type of scratch transitioned from brittle to ductile and the length of the scratches dramatically increased and extended to the edge of the optic. The observed trends can explained semi-quantitatively in terms of the time needed for a rogue particle to penetrate into a

  20. Microstructure variation in fused silica irradiated by different fluence of UV laser pulses with positron annihilation lifetime and Raman scattering spectroscopy

    Science.gov (United States)

    Li, Chunhong; Zheng, Wanguo; Zhu, Qihua; Chen, Jun; Wang, B. Y.; Ju, Xin

    2016-10-01

    We present an original study on the non-destructive evaluation of the microstructure evolution of fused silica induced by pulsed UV laser irradiation at low fluence (less than 50% Fth). Positron annihilation spectroscopy discloses that the spatial size of the vacancy cluster is increased exponentially with the linearly elevated laser fluence. Particularly, the vacancy cluster size in bulk silica is significantly increased by 14.5% after irradiated by pulsed 355 nm laser at F = 14 J/cm2 (50% Fth), while the void size varies only ∼2%. UV laser-excited Raman results suggest that the bond length and average bond angle of Sisbnd Osbnd Si bridging bond are both slightly reduced. Results reveals that the rearrangement process of (Sisbnd O)n fold rings and breakage of the Sisbnd O bridging bond in bulk silica occurred during pulsed UV laser irradiation. The micro-structural changes were taken together to clarify the effect of sub-threshold laser fluence on material stability of silica glass. The obtained data provide important information for studying material stability and controlling the lifetime of fused silica optics for high power laser system.

  1. High-resolution 3-D imaging of surface damage sites in fused silica with Optical Coherence Tomography

    Energy Technology Data Exchange (ETDEWEB)

    Guss, G; Bass, I; Hackel, R; Mailhiot, C; Demos, S G

    2007-10-30

    In this work, we present the first successful demonstration of a non-contact technique to precisely measure the 3D spatial characteristics of laser induced surface damage sites in fused silica for large aperture laser systems by employing Optical Coherence Tomography (OCT). What makes OCT particularly interesting in the characterization of optical materials for large aperture laser systems is that its axial resolution can be maintained with working distances greater than 5 cm, whether viewing through air or through the bulk of thick optics. Specifically, when mitigating surface damage sites against further growth by CO{sub 2} laser evaporation of the damage, it is important to know the depth of subsurface cracks below the damage site. These cracks are typically obscured by the damage rubble when imaged from above the surface. The results to date clearly demonstrate that OCT is a unique and valuable tool for characterizing damage sites before and after the mitigation process. We also demonstrated its utility as an in-situ diagnostic to guide and optimize our process when mitigating surface damage sites on large, high-value optics.

  2. Comparison of neutron and gamma irradiation effects on KU1 fused silica monitored by electron paramagnetic resonance

    Energy Technology Data Exchange (ETDEWEB)

    Bravo, D. [Department Fisica de Materiales, Universidad Autonoma de Madrid, E-28049 Madrid (Spain)], E-mail: david.bravo@uam.es; Lagomacini, J.C. [Department Fisica de Materiales, Universidad Autonoma de Madrid, E-28049 Madrid (Spain); Leon, M.; Martin, P. [Materiales para Fusion, CIEMAT, Avda. Complutense 22, E-28040 Madrid (Spain); Martin, A. [Department Fisica e Instalaciones, ETS Arquitectura UPM, E-28040 Madrid (Spain); Lopez, F.J. [Department Fisica de Materiales, Universidad Autonoma de Madrid, E-28049 Madrid (Spain); Ibarra, A. [Materiales para Fusion, CIEMAT, Avda. Complutense 22, E-28040 Madrid (Spain)

    2009-06-15

    Electron paramagnetic resonance (EPR) studies have been carried out on KU1 fused silica irradiated with neutrons at fluences 10{sup 21} and 10{sup 22} n/m{sup 2}, and gamma-ray doses up to 12 MGy. The effects of post-irradiation thermal annealing treatments, up to 850 deg. C, have also been investigated. Paramagnetic oxygen-related defects (POR and NBOHC) and E'-type defects have been identified and their concentration has been measured as a function of neutron fluence, gamma dose and post-irradiation annealing temperature. It is found that neutrons at the highest fluence generate a much higher concentration of defects (mainly E' and POR, both at concentrations about 5 x 10{sup 18} spins/cm{sup 3}) than gamma irradiations at the highest dose (mainly E' at a concentration about 4 x 10{sup 17} spins/cm{sup 3}). Moreover, for gamma-irradiated samples a lower treatment temperature (about 400 deg. C) is required to annihilate most of the observed defects than for neutron-irradiated ones (about 600 deg. C)

  3. Single molecule kinetics of horseradish peroxidase exposed in large arrays of femtoliter-sized fused silica chambers.

    Science.gov (United States)

    Ehrl, Benno N; Liebherr, Raphaela B; Gorris, Hans H

    2013-08-07

    Large arrays of femtoliter-sized chambers were etched into the surface of fused silica slides to enclose and observe hundreds of single horseradish peroxidase (HRP) molecules in parallel. Individual molecules of HRP oxidize the fluorogenic substrate Amplex Red to fluorescent resorufin in separate chambers, which was monitored by fluorescence microscopy. Photooxidation of Amplex Red and photobleaching of resorufin have previously limited the analysis of HRP in femtoliter arrays. We have strongly reduced these effects by optimizing the fluorescence excitation and detection scheme to yield accurate single molecule substrate turnover rates. We demonstrate the presence of long-lived kinetic states of single HRP molecules that are individually different for each molecule in the array. The large number of molecules investigated in parallel provides excellent statistics on the activity distribution in the enzyme population, which is similar to that reported for other enzymes such as β-galactosidase. We have further confirmed that the product formation of HRP in femtoliter chambers is 10-fold lower than that in the bulk solution due to the particular two-step redox reaction mechanism of HRP.

  4. Sub-wavelength ripples in fused silica after irradiation of the solid/liquid interface with ultrashort laser pulses.

    Science.gov (United States)

    Böhme, R; Vass, C; Hopp, B; Zimmer, K

    2008-12-10

    Laser-induced backside wet etching (LIBWE) is performed using ultrashort 248 nm laser pulses with a pulse duration of 600 fs to obtain sub-wavelength laser-induced periodic surface structures (LIPSS) on the back surface of fused silica which is in contact with a 0.5 mol l(-1) solution of pyrene in toluene. The LIPSS are strictly one-dimensional patterns, oriented parallel to the polarization of the laser radiation, and have a constant period of about 140 nm at all applied laser fluences (0.33-0.84 J cm(-2)) and pulse numbers (50-1000 pulses). The LIPSS amplitude varies due to the inhomogeneous fluence in the laser spot. The LIPSS are examined with scanning electron microscopy (SEM) and atomic force microscopy (AFM). Their power spectral density (PSD) distribution is analysed at a measured area of 10 µm × 10 µm. The good agreement of the measured and calculated LIPSS periods strongly supports a mechanism based on the interference of surface-scattered and incident waves.

  5. Design and Simulation of a Fused Silica Space Cell Culture and Observation Cavity with Microfluidic and Temperature Controlling

    Directory of Open Access Journals (Sweden)

    Shangchun Fan

    2013-01-01

    Full Text Available We report a principle prototype of space animal cell perfusion culture and observation. Unlike previous work, our cell culture system cannot only realize microfluidic and temperature controlling, automatic observation, and recording but also meet an increasing cell culture at large scale operation and overcome shear force for animal cells. A key component in the system is ingenious structural fused silica cell culture cavity with the wedge-shaped connection. Finite volume method (FVM is applied to calculate its multipoint flow field, pressure field, axial velocity, tangential velocity, and radial velocity. In order to provide appropriate flow rate, temperature, and shear force for space animal cell culture, a closed-loop microfluidic circuit and proportional, integrating, and differentiation (PID algorithm are employed. This paper also illustrates system architecture and operating method of the principle prototype. The dynamic culture, autofocus observation, and recording of M763 cells are performed successfully within 72 h in the laboratory environment. This research can provide a reference for space flight mission that carries an apparatus with similar functions.

  6. Correlating optical damage threshold with intrinsic defect populations in fused silica as a function of heat treatment temperature

    Energy Technology Data Exchange (ETDEWEB)

    Shen, N. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Matthews, M. J. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Elhadj, S. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Miller, P. E. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Nelson, A. J. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Hamilton, J. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)

    2013-04-03

    Here, chemical vapor deposition (CVD) is used for the production of fused silica optics in high-power laser applications. However, relatively little is known about the ultraviolet laser damage threshold of CVD films and how they relate to intrinsic defects produced during deposition. We present here a study relating structural and electronic defects in CVD films to 355 nm pulsed-laser damage threshold as a function of post-deposition annealing temperature (THT). Plasma-enhanced CVD based on SiH4/N2O under oxygen-rich conditions was used to deposit 1.5, 3.1 and 6.4 µm thick films on etched SiO2 substrates. Rapid annealing was performed using a scanned CO2 laser beam up to THT ~ 2100 K. The films were then characterized using x-ray photoemission spectroscopy, Fourier transform infrared spectroscopy (FTIR) and photoluminescence spectroscopy. A gradual transition in the damage threshold of annealed films was observed for THT values up to 1600 K, correlating with a decrease in non-bridging silanol and oxygen deficient centres. An additional sharp transition in damage threshold also occurs at ~1850 K indicating substrate annealing. Based on our results, a mechanism for damage-related defect annealing is proposed, and the potential of using high-THT CVD SiO2 to mitigate optical damage is also discussed.

  7. Characterization of Optical and Electrical Properties of Transparent Conductive Boron-Doped Diamond thin Films Grown on Fused Silica

    Directory of Open Access Journals (Sweden)

    Bogdanowicz Robert

    2014-12-01

    Full Text Available Abstract A conductive boron-doped diamond (BDD grown on a fused silica/quartz has been investigated. Diamond thin films were deposited by the microwave plasma enhanced chemical vapor deposition (MW PECVD. The main parameters of the BDD synthesis, i.e. the methane admixture and the substrate temperature were investigated in detail. Preliminary studies of optical properties were performed to qualify an optimal CVD synthesis and film parameters for optical sensing applications. The SEM micro-images showed the homogenous, continuous and polycrystalline surface morphology; the mean grain size was within the range of 100-250 nm. The fabricated conductive boron-doped diamond thin films displayed the resistivity below 500 mOhm cm-1 and the transmittance over 50% in the VIS-NIR wavelength range. The studies of optical constants were performed using the spectroscopic ellipsometry for the wavelength range between 260 and 820 nm. A detailed error analysis of the ellipsometric system and optical modelling estimation has been provided. The refractive index values at the 550 nm wavelength were high and varied between 2.24 and 2.35 depending on the percentage content of methane and the temperature of deposition.

  8. Laser-induced damage characteristics in fused silica surface due to mechanical and chemical defects during manufacturing processes

    Science.gov (United States)

    Li, Yaguo; Yuan, Zhigang; Wang, Jian; Xu, Qiao

    2017-06-01

    Mechanical and chemical defects incurred by grinding and polishing as well as post-processing have been recognized as the most influential culprits that hamper the elevation of laser power/energy in high peak power/energy laser systems. In order to find out the causes for limiting the operational power of laser systems, the effects of these defects on laser damage and removal and mitigation of the defects were investigated in detail in the article. Cracks and scratches were created, annealed, etched and damaged so as to reveal the likely effects of mechanical defects on damage and potential techniques to reduce their influence. The results show that HF-based etching can open and smooth cracks/scratches, improving laser-induced damage threshold (LIDT) at scratches by up to >250%. Thermal annealing did heal, to some extent, cracks but the LIDT is little improved. Both HF-etching and leaching proves to be effective in removing metallic contamination during polishing process and handling of optics, which can "contribute" to damage/damage density in fused silica. However, HF-based etching may degrade surface roughness, from 20 nm under some conditions when >20 μm material was etched away while the surface roughness was perceptibly altered by leaching (30 J/cm2 (355 nm @3 ns, beam diameter 400 μm @1/e2), a significant progress.

  9. Residual stress and damage-induced critical fracture on CO2 laser treated fused silica

    Energy Technology Data Exchange (ETDEWEB)

    Matthews, M; Stolken, J; Vignes, R; Norton, M

    2009-11-02

    Localized damage repair and polishing of silica-based optics using mid- and far-IR CO{sub 2} lasers has been shown to be an effective method for increasing optical damage threshold in the UV. However, it is known that CO{sub 2} laser heating of silicate surfaces can lead to a level of residual stress capable of causing critical fracture either during or after laser treatment. Sufficient control of the surface temperature as a function of time and position is therefore required to limit this residual stress to an acceptable level to avoid critical fracture. In this work they present the results of 351 nm, 3 ns Gaussian damage growth experiments within regions of varying residual stress caused by prior CO{sub 2} laser exposures. Thermally stressed regions were non-destructively characterized using polarimetry and confocal Raman microscopy to measure the stress induced birefringence and fictive temperature respectively. For 1 {approx} 40s square pulse CO{sub 2} laser exposures created over 0.5-1.25 kW/cm{sup 2} with a 1-3 mm 1/e{sup 2} diameter beam (T{sub max} {approx} 1500-3000 K), the critical damage site size leading to fracture increases weakly with peak temperature, but shows a stronger dependence on cooling rate, as predicted by finite element hydrodynamics simulations. Confocal micro-Raman was used to probe structural changes to the glass over different thermal histories and indicated a maximum fictive temperature of 1900K for T{sub max} {ge} 2000 K. The effect of cooling rate on fictive temperature caused by CO{sub 2} laser heating are consistent with finite element calculations based on a Tool-Narayanaswamy relaxation model.

  10. A fully automated linear polyacrylamide coating and regeneration method for capillary electrophoresis of proteins.

    Science.gov (United States)

    Bodnar, Judit; Hajba, Laszlo; Guttman, Andras

    2016-12-01

    Surface modification of the inner capillary wall in CE of proteins is frequently required to alter EOF and to prevent protein adsorption. Manual protocols for such coating techniques are cumbersome. In this paper, an automated covalent linear polyacrylamide coating and regeneration process is described to support long-term stability of fused-silica capillaries for protein analysis. The stability of the resulting capillary coatings was evaluated by a large number of separations using a three-protein test mixture in pH 6 and 3 buffer systems. The results were compared to that obtained with the use of bare fused-silica capillaries. If necessary, the fully automated capillary coating process was easily applied to regenerate the capillary to extend its useful life-time.

  11. Enantiomer separation of acidic chiral compounds on a quinine-silica/zirconia hybrid monolith by capillary electrochromatography.

    Science.gov (United States)

    Tran, Le Ngoc; Park, Jung Hag

    2015-05-29

    A weak anion-exchanger chiral selector, quinine-incorporated silica/zirconia hybrid monolithic (QUI-S/ZHM) capillary column was prepared by sol-gel technology. The performance of the QUI-S/ZHM column was investigated for enantioresolution of a set of acidic chiral drugs and dinitrobenzoyl (DNB)-amino acids by capillary electrochromatography in aqueous organic mobile phases composed of acetonitrile (ACN) and triethylammonium acetate (TEAA) buffer. Effects of several parameters including the ACN content, concentration and pH of the mobile phase on the chiral separation were examined. Baseline resolutions of all the compounds were obtained in the mobile phase consisting of 70:30 ACN/TEAA (10mM, pH 6) under applied voltage of -10kV at 25°C within 20min.

  12. Chromatographic comparison of bupivacaine imprinted polymers prepared in crushed monolith, microsphere, silica-based composite and capillary monolith formats.

    Science.gov (United States)

    Oxelbark, Joakim; Legido-Quigley, Cristina; Aureliano, Carla S A; Titirici, Maria-Magdalena; Schillinger, Eric; Sellergren, Börje; Courtois, Julien; Irgum, Knut; Dambies, Laurent; Cormack, Peter A G; Sherrington, David C; De Lorenzi, Ersilia

    2007-08-10

    A comprehensive comparison of five chromatographic stationary phases based on molecularly imprinted polymers is presented. Efficiency, imprinting factors, water compatibility and batch-to-batch reproducibility are discussed for crushed monolith, microspheres, two silica-based composites and capillary monoliths, all imprinted with the local anaesthetic bupivacaine. Synthesis protocol and chromatographic test conditions have been kept fixed within certain limits, in order to provide further insight into the strengths and weaknesses of the different formats. Excluding microparticles, all formats give satisfactory performance, especially in aqueous mobile phases. An assessment of batch-to-batch reproducibility in different mobile phases adds further value to this comparison study.

  13. Laser-induced periodic surface structures on fused silica upon cross-polarized two-color double-fs-pulse irradiation

    Energy Technology Data Exchange (ETDEWEB)

    Höhm, S., E-mail: hoehm@mbi-berlin.de.de [Max-Born-Institut für Nichtlineare Optik und Kurzzeitspektroskopie (MBI), Max-Born-Straße 2A, D-12489 Berlin (Germany); Herzlieb, M.; Rosenfeld, A. [Max-Born-Institut für Nichtlineare Optik und Kurzzeitspektroskopie (MBI), Max-Born-Straße 2A, D-12489 Berlin (Germany); Krüger, J. [BAM Bundesanstalt für Materialforschung und–prüfung, Unter den Eichen 87, D-12205 Berlin (Germany); Bonse, J., E-mail: joern.bonse@bam.de [BAM Bundesanstalt für Materialforschung und–prüfung, Unter den Eichen 87, D-12205 Berlin (Germany)

    2015-05-01

    Graphical abstract: - Highlights: • LIPSS formation on fused silica is studied upon cross-polarized two-color (400 and 800 nm) double-fs-pulse irradiation. • LIPSS orientation follows the polarization of the first pulse. • LIPSS periods are determined by the wavelength of the first pulse. • LIPSS area is increased for temporally overlapping pulses due to nonlinear absorption. - Abstract: The dynamics of the formation of laser-induced periodic surface structures (LIPSS) on fused silica upon irradiation with linearly polarized fs-laser pulses (50 fs pulse duration) is studied by cross-polarized two-color double-fs-pulse experiments. In order to analyze the relevance of temporally distributed energy deposition in the early stage of LIPSS formation, a Mach-Zehnder interferometer was used for generating multiple double-pulse sequences at two different wavelengths (400 and 800 nm). The inter-pulse delay between the individual cross-polarized pulses of each sequence was systematically varied in the sub-ps range and the resulting LIPSS morphologies were characterized by scanning electron microscopy. It is found that the polarization of the first laser pulse arriving to the surface determines the orientation and the periodicity of the LIPSS. These two-color experiments further confirm the importance of the ultrafast energy deposition to the silica surface for LIPSS formation, particularly by the first laser pulse of each sequence. The second laser pulse subsequently reinforces the previously seeded spatial LIPSS characteristics (period, orientation)

  14. Development of a laser damage growth mitigation process, based on CO2 laser micro processing, for the Laser MegaJoule fused silica optics

    Science.gov (United States)

    Doualle, Thomas; Gallais, Laurent; Monneret, Serge; Bouillet, Stephane; Bourgeade, Antoine; Ameil, Christel; Lamaignère, Laurent; Cormont, Philippe

    2016-12-01

    In the context of high power laser systems, the laser damage resistance of fused silica surfaces at 351 nm in the nanosecond regime is a major concern. Under successive nanosecond laser irradiations, an initiated damage can grow which can make the component unsuitable. The localized CO2 laser processing has demonstrated its ability to mitigate (stopping) laser damage growth. In order to mitigate large damage sites (millimetric), a method based on fast microablation of silica has been proposed by Bass et al. [Bass et al., Proc. SPIE 7842, 784220 (2010)]. This is accomplished by scanning of the CO2 laser spot with a fast galvanometer beam scanner to form a crater with a typical conical shape. The objective of the present work is to develop a similar fast micro-ablation process for application to the Laser MegaJoule optical components. We present in this paper the developed experimental system and process. We describe also the characterization tools used in this study for shape measurements which are critical for the application. Experimental and numerical studies of the downstream intensifications, resulting of cone formation on the fused silica surface, are presented. The experimental results are compared to numerical simulations for different crater shape in order to find optimal process conditions to minimize the intensifications in the LMJ configuration. We show the laser damage test experimental conditions and procedures to evaluate the laser damage resistance of the mitigated sites and discuss the efficiency of the process for our application.

  15. Silica sulfuric acid: a reusable solid catalyst for one pot synthesis of densely substituted pyrrole-fused isocoumarins under solvent-free conditions

    Directory of Open Access Journals (Sweden)

    Sudipta Pathak

    2013-11-01

    Full Text Available A convenient and efficient methodology for the synthesis of densely substituted pyrrole-fused isocoumarins, which employs solid-supported silica sulfuric acid (SSA as catalyst, has been developed. When the mixture of ninhydrin adducts of acetylacetone/ethyl acetoacetate and primary amines was heated on the solid surface of SSA under solvent-free conditions, the pyrrole-fused isocoumarins were formed in good yields. This synthetic method has several advantages such as the employment of solvent-free reaction conditions without the use of any toxic reagents and metal catalysts, the ease of product isolation, the use of a recyclable catalyst, the low cost, the easy availability of the starting materials, and the excellent yields of products.

  16. Bacterial surface layer proteins as a novel capillary coating material for capillary electrophoretic separations

    Energy Technology Data Exchange (ETDEWEB)

    Moreno-Gordaliza, Estefanía, E-mail: emorenog@ucm.es [Division of Analytical Biosciences, Leiden Academic Centre for Drug Research, Universiteit Leiden, Einsteinweg 55, 2300, RA, Leiden (Netherlands); Department of Analytical Chemistry, Faculty of Chemistry, Universidad Complutense de Madrid, Avda. Complutense s/n, 28040, Madrid (Spain); Stigter, Edwin C.A. [Division of Analytical Biosciences, Leiden Academic Centre for Drug Research, Universiteit Leiden, Einsteinweg 55, 2300, RA, Leiden (Netherlands); Department of Molecular Cancer Research, Universitair Medisch Centrum Utrecht, Wilhelmina Kinder Ziekenhuis, Lundlaan 6, 3584, EA Utrecht (Netherlands); Lindenburg, Petrus W.; Hankemeier, Thomas [Division of Analytical Biosciences, Leiden Academic Centre for Drug Research, Universiteit Leiden, Einsteinweg 55, 2300, RA, Leiden (Netherlands)

    2016-06-07

    A novel concept for stable coating in capillary electrophoresis, based on recrystallization of surface layer proteins on hydrophobized fused silica capillaries, was demonstrated. Surface layer protein A (SlpA) from Lactobacillus acidophilus bacteria was extracted, purified and used for coating pre-silanized glass substrates presenting different surface wettabilities (either hydrophobic or hydrophilic). Contact angle determination on SlpA-coated hydrophobic silica slides showed that the surfaces turned to hydrophilic after coating (53 ± 5°), due to a protein monolayer formation by protein-surface hydrophobic interactions. Visualization by atomic force microscopy demonstrated the presence of a SlpA layer on methylated silica slides displaying a surface roughness of 0.44 ± 0.02 nm. Additionally, a protein layer was visualized by fluorescence microscopy in methylated silica capillaries coated with SlpA and fluorescein isothiocyanate-labeled. The SlpA-coating showed an outstanding stability, even after treatment with 20 mM NaOH (pH 12.3). The electroosmotic flow in coated capillaries showed a partial suppression at pH 7.50 (3.8 ± 0.5 10{sup −9} m{sup 2} V{sup −1} s{sup −1}) when compared with unmodified fused silica (5.9 ± 0.1 10{sup −8} m{sup 2} V{sup −1} s{sup −1}). To demonstrate the potential of this novel coating, the SlpA-coated capillaries were applied for the first time for electrophoretic separation, and proved to be very suitable for the isotachophoretic separation of lipoproteins in human serum. The separations showed a high degree of repeatability (absolute migration times with 1.1–1.8% coefficient-of-variation (CV) within a day) and 2–3% CV inter-capillary reproducibility. The capillaries were stable for more than 100 runs at pH 9.40, and showed to be an exceptional alternative for challenging electrophoretic separations at long-term use. - Highlights: • New coating using recrystallized surface-layer proteins on

  17. Capillary electrophoresis using core-based hyperbranched polyethyleneimine (CHPEI) static-coated capillaries.

    Science.gov (United States)

    Boonyakong, Cheerapa; Tucker, Sheryl A

    2009-10-01

    With unique 3-D architecture, the application of core-based hyperbranched polyethyleneimine (CHPEI), as a capillary coating in capillary electrophoresis, is demonstrated by manipulation of the electroosmotic mobility (EOF). CHPEI coatings (CHPEI5, M(w) approximately 5000 and CHPEI25, M(w) approximately 25,000) were physically adsorbed onto the inner surface of bare fused-silica capillary (BFS) via electrostatic interaction of the oppositely charged molecules by rinsing the capillaries with different CHPEI aqueous solutions. The EOF values of the coated capillaries were measured over the pH range of 4.0-9.0. At higher pH (pH >6) the coated capillary surface possesses excess negative charges, which causes the reversal of the EOF. The magnitudes of the EOF obtained from the coated capillaries were three-fold lower than that of BFS capillary. Desirable reproducibility of the EOF with % RSD (n = 5) capillaries were successfully utilized to separate phenolic compounds, B vitamins, as well as basic drugs and related compounds with reasonable analysis time (capillary and capillary).

  18. Evaluation of migration behaviour of therapeutic peptide hormones in capillary electrophoresis using polybrene-coated capillaries.

    Science.gov (United States)

    Aptisa, Ghiulendan; Benavente, Fernando; Sanz-Nebot, Victoria; Chirila, Elisabeta; Barbosa, José

    2010-02-01

    Modelling electrophoretic mobility as a function of pH can be simultaneously used for determination of ionization constants and for rapid selection of the optimum pH for separation of mixtures of the modelled compounds. In this work, equations describing the effect of pH on electrophoretic behaviour were used to investigate migration of a series of polyprotic amphoteric peptide hormones between pH 2 and 12 in polybrene-coated capillaries. Polybrene (hexadimethrin bromide) is a polymer composed of quaternary amines that is strongly adsorbed by the fused-silica inner surface, preventing undesired interactions between the peptides and the inner capillary wall. In polybrene-coated capillaries the separation voltage must be reversed, because of the anodic electroosmotic flow promoted by the polycationic polymer attached to the inner capillary wall. The possibility of using polybrene-coated capillaries for determination of accurate ionization constants has been evaluated and the optimum pH for separation of a mixture of the peptide hormones studied has been selected. Advantages and disadvantages of using bare fused-silica and polybrene-coated capillaries for these purposes are discussed.

  19. Separation and quantification of cellulases and hemicellulases by capillary electrophoresis

    DEFF Research Database (Denmark)

    Jørgensen, Henning; Kutter, Jörg Peter; Olsson, Lisbeth

    2003-01-01

    . Current methods are limited in their ability to quantify all of these enzymes when all are present simultaneously in a mixture. Five different cellulases (two cellobiohydrolases and three endoglucanases) and one hemicellulase (endoxylanase) were separated using capillary electrophoresis (CE) in a fused...... silica capillary at pH values close to neutral. The improvement of the separation of these six proteins by the addition of alpha, omega-diaminoalkanes with chain lengths from three to seven carbon units was investigated. Dynamically coating the capillary with 1,3-diaminopropane resulted in separation...

  20. Inflammatory and cytotoxic responses of an alveolar-capillary coculture model to silica nanoparticles: Comparison with conventional monocultures

    Directory of Open Access Journals (Sweden)

    Stauber Roland

    2011-01-01

    Full Text Available Abstract Background To date silica nanoparticles (SNPs play an important role in modern technology and nanomedicine. SNPs are present in various materials (tyres, electrical and thermal insulation material, photovoltaic facilities. They are also used in products that are directly exposed to humans such as cosmetics or toothpaste. For that reason it is of great concern to evaluate the possible hazards of these engineered particles for human health. Attention should primarily be focussed on SNP effects on biological barriers. Accidentally released SNP could, for example, encounter the alveolar-capillary barrier by inhalation. In this study we examined the inflammatory and cytotoxic responses of monodisperse amorphous silica nanoparticles (aSNPs of 30 nm in size on an in vitro coculture model mimicking the alveolar-capillary barrier and compared these to conventional monocultures. Methods Thus, the epithelial cell line, H441, and the endothelial cell line, ISO-HAS-1, were used in monoculture and in coculture on opposite sides of a filter membrane. Cytotoxicity was evaluated by the MTS assay, detection of membrane integrity (LDH release, and TER (Transepithelial Electrical Resistance measurement. Additionally, parameters of inflammation (sICAM-1, IL-6 and IL-8 release and apoptosis markers were investigated. Results Regarding toxic effects (viability, membrane integrity, TER the coculture model was less sensitive to apical aSNP exposure than the conventional monocultures of the appropriate cells. On the other hand, the in vitro coculture model responded with the release of inflammatory markers in a much more sensitive fashion than the conventional monoculture. At concentrations that were 10-100fold less than the toxic concentrations the apically exposed coculture showed a release of IL-6 and IL-8 to the basolateral side. This may mimic the early inflammatory events that take place in the pulmonary alveoli after aSNP inhalation. Furthermore, a number

  1. Cycloaliphatic epoxy resin coating for capillary electrophoresis.

    Science.gov (United States)

    Shah, Roopa S; Wang, Qinggang; Lee, Milton L

    2002-04-05

    Coating the interior surface of a fused-silica capillary with a polymeric material has long been used in capillary electrophoresis (CE) to reduce or eliminate electroosmotic flow and suppress adsorption. A cycloaliphatic epoxide-based resin was bonded to silane treated capillaries and crosslinked with a curing agent. The epoxy resin coating significantly reduced electroosmotic flow over a pH range of 3-10. This coating was sufficiently hydrophilic to suppress protein adsorption. The epoxy resin coated capillary was used to separate several acidic and basic proteins and peptides. Separation efficiencies greater than 400,000 theoretical plates were achieved. The relative standard deviations in migration times for proteins were methods.

  2. The effect of pulse duration on the growth rate of laser-induced damage sites at 351 nm on fused silica surfaces

    Energy Technology Data Exchange (ETDEWEB)

    Negres, R A; Norton, M A; Liao, Z M; Cross, D A; Bude, J D; Carr, C W

    2009-10-29

    Past work in the area of laser-induced damage growth has shown growth rates to be primarily dependent on the laser fluence and wavelength. More recent studies suggest that growth rate, similar to the damage initiation process, is affected by a number of additional parameters including pulse duration, pulse shape, site size, and internal structure. In this study, we focus on the effect of pulse duration on the growth rate of laser damage sites located on the exit surface of fused silica optics. Our results demonstrate, for the first time, a significant dependence of growth rate at 351 nm on pulse duration from 1 ns to 15 ns as {tau}{sup 0.3} for sites in the 50-100 {micro}m size range.

  3. Formation of laser-induced periodic surface structures on fused silica upon multiple cross-polarized double-femtosecond-laser-pulse irradiation sequences

    Energy Technology Data Exchange (ETDEWEB)

    Rohloff, M.; Das, S. K.; Hoehm, S.; Grunwald, R.; Rosenfeld, A. [Max-Born-Institut fuer Nichtlineare Optik und Kurzzeitspektroskopie (MBI), Max-Born-Strasse 2A, D-12489 Berlin (Germany); Krueger, J.; Bonse, J. [BAM Bundesanstalt fuer Materialforschung und -pruefung, Unter den Eichen 87, D-12205 Berlin (Germany)

    2011-07-01

    The formation of laser-induced periodic surface structures (LIPSS) upon irradiation of fused silica with multiple irradiation sequences consisting of five Ti:sapphire femtosecond (fs) laser pulse pairs (150 fs, 800 nm) is studied experimentally. A Michelson interferometer is used to generate near-equal-energy double-pulse sequences with a temporal pulse delay from -20 to +20 ps between the cross-polarized individual fs-laser pulses ({approx}0.2 ps resolution). The results of multiple double-pulse irradiation sequences are characterized by means of Scanning Electron and Scanning Force Microscopy. Specifically in the sub-ps delay domain striking differences in the surface morphologies can be observed, indicating the importance of the laser-induced free-electron plasma in the conduction band of the solids for the formation of LIPSS.

  4. Polymer optical fiber fuse

    CERN Document Server

    Mizuno, Yosuke; Tanaka, Hiroki; Nakamura, Kentaro

    2013-01-01

    Although high-transmission-capacity optical fibers are in demand, the problem of the fiber fuse phenomenon needs to be resolved to prevent the destruction of fibers. As polymer optical fibers become more prevalent, clarifying their fuse properties has become important. Here, we experimentally demonstrate a fuse propagation velocity of 21.9 mm/s, which is 1 to 2 orders of magnitude slower than that in standard silica fibers. The achieved threshold power density and proportionality constant between the propagation velocity and the power density are respectively 1/186 of and 16.8 times the values for silica fibers. An oscillatory continuous curve instead of periodic voids is formed after the passage of the fuse. An easy fuse termination method is presented herein, along with its potential plasma applications.

  5. One-pot preparation of mercaptotetrazole-silica hybrid monoliths by the thiol-ene click reaction for mixed-mode capillary liquid chromatography.

    Science.gov (United States)

    Wang, Haojiang; Hu, Wenli; Zheng, Qiong; Bian, Wei; Lin, Zian

    2017-06-01

    A novel mercaptotetrazole-silica hybrid monolithic column was prepared for capillary liquid chromatography, in which the thiol-end mercaptotetrazole was mixed with hydrolyzed γ-methacryloxypropyltrimethoxysilane and tetramethyloxysilane for the co-polycondensation and thiol-ene click reaction in a one-pot process. The effects of the molar ratio of silanes, the amount of mercaptotetrazole, and the volume of porogen on the morphology, permeability and pore properties of the as-prepared mercaptotetrazole-silica hybrid monoliths were investigated in detail. A series of test compounds including alkylbenzenes, amides and anilines were employed for evaluating the retention behaviors of the mercaptotetrazole-silica hybrid monolithic columns. The results demonstrated that the mercaptotetrazole-silica hybrid monoliths exhibited hydrophobic, hydrophilic as well as ion-exchange interaction. The run-to-run, column-to-column and batch-to-batch reproducibilities of the mercaptotetrazole-silica hybrid monoliths were satisfactory with the relative standard deviations less than 1.4 (n = 5), 3.9 (n = 3) and 4.0% (n = 5), respectively. In addition, the mercaptotetrazole-silica hybrid monolith was further applied to the separation of sulfonamides, nucleobases and protein tryptic digests. These successful applications confirmed the promising potential of the mercaptotetrazole-silica hybrid monolith in the separation of complex samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Influence of fused Silica and chills incorporation on Corrosion, Thermal and Chemical composition of ASTM A 494 M Grade Nickel alloy

    Science.gov (United States)

    Purushotham, G.; Hemanth, Joel

    2016-09-01

    A review of a host of relevant literature on the composites leads to some important observations on the gap that prevails for developing the composite with increased strength to weight ratio, improved thermal properties and reduced corrosion rate with the addition of fused SiO2 dispersoid for the nickel based alloy. In the arena of engineering, metallurgists look for techniques to improve the thermal, corrosion and chemical properties of the materials. In this connection an investigation has been carried out to fabricate and evaluate the corrosion, chemical and thermal properties of chilled composites consisting of nickel matrix with fused silica particles (size 40-150 μm) in the matrix. The main objective of the present research is to obtain fine grain Ni/SiO2 chilled sound composite having very good properties. The dispersoid added ranged from 3 to 12 wt. % in steps of 3%. The subsequent composites cast in molds containing metallic and non-metallic chill blocks (MS, SiC & Cu) were tested for their microstructure, chemical, thermal properties and corrosion behavior.

  7. Temperature-dependent strain and temperature sensitivities of fused silica single mode fiber sensors with pulse pre-pump Brillouin optical time domain analysis

    Science.gov (United States)

    Bao, Yi; Chen, Genda

    2016-06-01

    This paper reports a distributed temperature and strain sensor based on pulse pre-pump Brillouin optical time domain analysis. An uncoated, telecom-grade fused silica single-mode fiber as a distributed sensor was calibrated for its sensitivity coefficients under various strains and temperatures up to 800 °C. The Brillouin frequency of fiber samples changed nonlinearly with temperature and linearly with strain. The temperature sensitivity decreased from 1.113 to 0.830 MHz /°C in the range of 22-800 °C. The strain sensitivity was reduced from 0.054 to 0.042 MHz /μɛ as the temperature increased from 22 to 700 °C and became unstable at higher temperatures due to creep effect. The strain measurement range was reduced from 19 100 to 6000 μɛ in the temperature range of 22-800 °C due to fused silica’s degradation. The calibrated fiber optic sensor demonstrated adequate accuracy and precision for strain and temperature measurements and stable performance in heating-cooling cycles. It was validated in an application setting.

  8. Growth of carbon nanofiber coatings on nickel thin films on fused silica by catalytic thermal chemical vapor deposition: On the use of titanium, titanium–tungsten and tantalum as adhesion layers

    NARCIS (Netherlands)

    Thakur, D.B.; Tiggelaar, R.M.; Gardeniers, J.G.E.; Lefferts, L.; Seshan, K.

    2009-01-01

    Coatings of carbon nanofiber (CNF) layers were synthesized on fused silica substrates using a catalytic thermal chemical vapor deposition process (C-TCVD). The effects of various adhesion layers–titanium, titanium–tungsten and tantalum–under the nickel thin film on the attachment of carbon nanofiber

  9. Laser-induced periodic surface structures on fused silica upon cross-polarized two-color double-fs-pulse irradiation

    Science.gov (United States)

    Höhm, S.; Herzlieb, M.; Rosenfeld, A.; Krüger, J.; Bonse, J.

    2015-05-01

    The dynamics of the formation of laser-induced periodic surface structures (LIPSS) on fused silica upon irradiation with linearly polarized fs-laser pulses (50 fs pulse duration) is studied by cross-polarized two-color double-fs-pulse experiments. In order to analyze the relevance of temporally distributed energy deposition in the early stage of LIPSS formation, a Mach-Zehnder interferometer was used for generating multiple double-pulse sequences at two different wavelengths (400 and 800 nm). The inter-pulse delay between the individual cross-polarized pulses of each sequence was systematically varied in the sub-ps range and the resulting LIPSS morphologies were characterized by scanning electron microscopy. It is found that the polarization of the first laser pulse arriving to the surface determines the orientation and the periodicity of the LIPSS. These two-color experiments further confirm the importance of the ultrafast energy deposition to the silica surface for LIPSS formation, particularly by the first laser pulse of each sequence. The second laser pulse subsequently reinforces the previously seeded spatial LIPSS characteristics (period, orientation).

  10. Cryogenic surface distortion and hysteresis of a 50 CM diameter fused silica mirror cooled to 77 K

    Science.gov (United States)

    Young, Jeffrey A.; Howard, Steven D.; Augason, Gordon C.; Melugin, Ramsey K.

    1990-11-01

    A 50 cm diameter, lightweight, Amersil TO8E, fused-natural-quartz mirror with a single arch cross section was tested at the NASA/Ames Research Center Cryogenic Optics Test Facility to measure cryogenic distortion and hysteresis. The mirror was cooled to 77 K in four serial tests and the mirror figure was measured with a phase-measuring interferometer. On the basis of the repeatability of room temperature and cryogenic optical measurements, it was determined that the Single Arch Mirror had no measurable hysteresis and displayed repeatable cryogenic distortion. The Cryogenic Optics Test Facility, optical and thermal test methods, test results, and measurement accuracy are described.

  11. Effect of the Silanization Conditions on Chromatographic Behavior of an Open-tubular Capillary Column Coated with a Modified Silica-gel Thin Layer

    OpenAIRE

    Yusuke, Nakano; Shinya, Kitagawa; Kanji, Miyabe; Takao, Tsuda

    2005-01-01

    The performance of an open-tubular capillary column coated with a modified silica-gel thin layer was investigated, particularly concerning the effect of the silanization process on it. Although the increase in the octadecyltriethoxysilane (ODTES) concentration in the silanization process could enhance the retention factor of naphthalene, its theoretical plate number was significantly reduced (ODTES, 5 to 50%; k, 0.2 to 4.3; N, 79600 to 2600 m-1). Namely, the increase in the retention factor w...

  12. High Q silica microbubble resonators fabricated by heating a pressurized glass capillary

    Science.gov (United States)

    Yu, Zhe; Liu, Tiegen; Jiang, Junfeng; Liu, Kun; Chen, Wenjie; Zhang, Xuezhi; Lin, Xujun; Liu, Wenhui

    2014-11-01

    Microbubble resonators combine the unique properties of whispering gallery mode resonators with the capability of integrated microfluidics. The microbubble resonator is fabricated by heating the tapered tip of a pressurized glass capillary with oxyhydrogen flame. Firstly, a microtube with a diameter of 250um is stretched under heating of oxyhydrogen flame, the heating zone length is set to be 20mm and the length of stretch is set to be 7000um.Then nitrogen will be pumped in to the tapered microtube with the pressure of 0.1Mpa, the tapered tip will be heated by the oxyhydrogen flame continuously until a microbubble forms. An optical fiber taper with a diameter of 2 um, fabricated by stretching a single-mode optical fiber under flame was brought in contact with the microbubble to couple the light from a 1550nm tunable diode laser into the whispering gallery mode. The microbubble resonator has a Q factors up to 1.5 × 107 around 1550nm. Different concentrations of ethanol solution (from 5% to 30%) are filled into it in order to test the refractive index sensing capabilities of such resonator, which shows a sensitivity of 82nm/RIU.

  13. Effects of Gas Flow Rates on Fused Silica Glass%气体流量对熔石英玻璃的影响

    Institute of Scientific and Technical Information of China (English)

    黄耀松; 郑丽丽; 任祝寅; 张辉

    2015-01-01

    大尺寸熔石英玻璃的折射率均匀性对其光学特性有重要影响,本文对利用SiCl4水解合成熔石英玻璃的过程开展数值模拟研究,揭示 H2和 O2当量比以及载料气与 SiCl4质量比对温度分布和组分浓度分布的影响,及其对熔石英玻璃折射率均匀性潜在的影响.研究结果表明,在径向方向上,火焰温度分布呈现“高-低-高”的 M 型分布规律;增大 H2/O2当量比,会使轴向火焰预热区变短,当量比为1.0时,会产生一个比较长的火焰射流长度及宽的径向高温区,但是羟基浓度变化比较大,导致熔石英玻璃折射率不均匀性增加;采用小的当量比对提高玻璃折射率均匀性有一定的作用,因为在小的当量比下玻璃体沉积面上的温度梯度以及羟基浓度梯度较小,但是同时会降低火焰整体温度以及 SiO2生成量;另外,增加载料气对 SiCl4的质量比会降低玻璃体沉积面的温度变化,有利于改善折射率均匀性,但是与此同时,玻璃体沉积面上羟基浓度梯度增加了,对熔石英玻璃的折射率均匀性会产生不良影响.%The refractive index homogeneity of large-sized fused silica glass has great impact on its optical character-istics.In this paper,a numerical study on synthesis of fused silica glass by SiCl4 hydrolysis deposition is per-formed.The effects of the equivalence ratio of H2 to O2 and the mass ratio of carrier gas to SiCl4 on temperature pro-file and species concentration distributions are investigated,together with their potential impact on the homogeneity of refractive index of large-sized fused silica glass.It is found that the temperature profile in radial direction exhibits a high-low-high M-shape profile,and the increase of equivalence ratio of H2 to O2 results in a shorter axial preheating region.A long flame length and a broad high-temperature region can be obtained when the equivalence ratio is 1.0, but the

  14. Capillary Condensation Pathways of CO2 under Templated Mesoporous Silica Confinement

    Science.gov (United States)

    Wang, Bo; Sokol, Paul

    2014-03-01

    Adsorption of CO2 in porous medium has been of great current interest due to its potential for mitigating the global warming caused by greenhouse gases. In particular, the behavior of confined CO2 in mesoporous media near room temperature is particularly relevant to sequestration efforts. Realistic mesoporous systems, such as shales and coals, represent a complex fractal pore structure that complicates the interpretation of adsorption studies. We present the results of a study focused on the adsorption of CO2 in model mesoporous media with well-defined pore structures. Templated porous glasses, such as MCM-41 which has a regular network of 1D pores, provide an ideal system for fundamental studies of the adsorption process. In this study, we focus on the structure of adsorbed CO2 films which evolves in a mixture of phases and the development of nucleation occurs during the formation of high density liquid CO2 inside the confining matrix. We have used Small Angle Neutron Scattering to study the spatial distribution of material radially and transversely within the pores. The 30m SANS NG7 at NIST was used to map out the details of CO2 condensation pathway under mesoporous silica confinement.

  15. Capillary Column Coated With Heptakis(2,3,6-tri-O-octyl)-β-cyclodextrin Using Sol-gel Technology

    Institute of Scientific and Technical Information of China (English)

    Xiao Xia GE; Ruo Nong FU; Rong Ji DAI; Li Wen LIU; Mei Ling QI

    2004-01-01

    Heptakis(2,3,6-tri-O-octyl)-β-cyclodextrin was coated onto the fused silica capillary by sol-gel technology.Column efficiency and column selectivity were studied. The results indicated that high ability of separation was acquired. Positional isomers of aromatic compounds were well separated.

  16. Toward high-throughput monitoring of metallodrug-protein interaction using capillary electrophoresis in chemically modified capillaries.

    Science.gov (United States)

    Shmykov, Alexei Y; Filippov, Vladimir N; Foteeva, Lidia S; Keppler, Bernhard K; Timerbaev, Andrei R

    2008-08-15

    The performance of capillary electrophoresis (CE) operating with a sulfonated capillary for the separation of protein adducts of anticancer ruthenium(III)-based drugs was evaluated. The coated capillary was shown to yield improved resolution of albumin- and transferrin-bound species of ruthenium compared with that attained with the bare fused-silica capillary. The coating also showed an increased reproducibility of migration times and peak areas and allowed reasonably high efficiency separation of analytes (up to 1300 theoretical plates per meter), which display high affinity toward a fused-silica surface. In addition, due to rather high electroosmotic flow (EOF, > 45 x 10(-5)cm(2)V(-1)s(-1)) in the coated capillary, it enabled fast counter-EOF monitoring of albumin and transferrin adducts. This benefit, together with requiring only a short flush with the background electrolyte to have migration times reproducible (at capillary holding promise for CE examination of fast reactions such as those accompanying protein-drug interactions and biotransformations associated with drug delivery via protein binding.

  17. Two-dimensional capillary electrophoresis using tangentially connected capillaries.

    Science.gov (United States)

    Sahlin, Eskil

    2007-06-22

    A novel type of fused silica capillary system is described where channels with circular cross-sections are tangentially in contact with each other and connected through a small opening at the contact area. Since the channels are not crossing each other in the same plane, the capillaries can easily be filled with different solutions, i.e. different solutions will be in contact with each other at the contact point. The system has been used to perform different types of two-dimensional separations and the complete system is fully automated where a high voltage switch is used to control the location of the high voltage in the system. Using two model compounds it is demonstrated that a type of two-dimensional separation can be performed using capillary zone electrophoresis at two different pH values. It is also shown that a compound with acid/base properties can be concentrated using a dynamic pH junction mechanism when transferred from the first separation to the second separation. In addition, the system has been used to perform a comprehensive two-dimensional capillary electrophoresis separation of tryptic digest of bovine serum albumin using capillary zone electrophoresis followed by micellar electrokinetic chromatography.

  18. Bi-stage time evolution of nano-morphology on inductively coupled plasma etched fused silica surface caused by surface morphological transformation

    Science.gov (United States)

    Jiang, Xiaolong; Zhang, Lijuan; Bai, Yang; Liu, Ying; Liu, Zhengkun; Qiu, Keqiang; Liao, Wei; Zhang, Chuanchao; Yang, Ke; Chen, Jing; Jiang, Yilan; Yuan, Xiaodong

    2017-07-01

    In this work, we experimentally investigate the surface nano-roughness during the inductively coupled plasma etching of fused silica, and discover a novel bi-stage time evolution of surface nano-morphology. At the beginning, the rms roughness, correlation length and nano-mound dimensions increase linearly and rapidly with etching time. At the second stage, the roughening process slows down dramatically. The switch of evolution stage synchronizes with the morphological change from dual-scale roughness comprising long wavelength underlying surface and superimposed nano-mounds to one scale of nano-mounds. A theoretical model based on surface morphological change is proposed. The key idea is that at the beginning, etched surface is dual-scale, and both larger deposition rate of etch inhibitors and better plasma etching resistance at the surface peaks than surface valleys contribute to the roughness development. After surface morphology transforming into one-scale, the difference of plasma resistance between surface peaks and valleys vanishes, thus the roughening process slows down.

  19. Optical Evaluation of Digital Micromirror Devices (DMDs) with UV-Grade Fused Silica, Sapphire, and Magnesium Fluoride Windows and Longterm Reflectance of Bare Devices

    Science.gov (United States)

    Quijada, Manuel A.; Travinsky, Anton; Vorobiev, Dmitry; Ninkov, Zoran; Raisanen, Alan; Robberto, Massimo; Heap, Sara

    2016-01-01

    Digital micromirror devices (DMDs) are commercial micro-electromechanical systems, consisting of millions of mirrors which can be individually addressed and tilted into one of two states (+/-12deg). These devices were developed to create binary patterns in video projectors, in the visible range. Commercially available DMDs are hermetically sealed and extremely reliable. Recently, DMDs have been identified as an alternative to microshutter arrays for space-based multi-object spectrometers (MOS). Specifically, the MOS at the heart of the proposed Galactic Evolution Spectroscopic Explorer (GESE) uses the DMD as a reprogrammable slit mask. Unfortunately, the protective borosilicate windows limit the use of DMDs in the UV and IR regimes, where the glass has insufficient throughput. In this work, we present our efforts to replace standard DMD windows with custom windows made from UV-grade fused silica, low-absorption optical sapphire (LAOS) and magnesium fluoride (MgF2). We present transmission measurements of the antireflection coated windows and the reflectance of bare (window removed) DMDs. Furthermore, we investigated the long-term stability of the DMD reflectance and experiments for coating DMD active area with a layer of pure aluminum (Al) to boost reflectance performance in the UV spectral range (200-400 nm).

  20. Formation of laser-induced periodic surface structures on fused silica upon multiple parallel polarized double-femtosecond-laser-pulse irradiation sequences

    Energy Technology Data Exchange (ETDEWEB)

    Rosenfeld, Arkadi, E-mail: rosenfeld@mbi-berlin.de [Max-Born-Institut fuer Nichtlineare Optik und Kurzzeitspektroskopie (MBI), Max-Born-Strasse 2A, D-12489 Berlin (Germany); Rohloff, Marcus; Hoehm, Sandra [Max-Born-Institut fuer Nichtlineare Optik und Kurzzeitspektroskopie (MBI), Max-Born-Strasse 2A, D-12489 Berlin (Germany); Krueger, Joerg [BAM Bundesanstalt fuer Materialforschung und -pruefung, Unter den Eichen 87, D-12205 Berlin (Germany); Bonse, Joern, E-mail: joern.bonse@bam.de [BAM Bundesanstalt fuer Materialforschung und -pruefung, Unter den Eichen 87, D-12205 Berlin (Germany)

    2012-09-15

    Highlights: Black-Right-Pointing-Pointer LIPSS formation studied for double-fs-pulses (160 fs, 800 nm) of different fluences. Black-Right-Pointing-Pointer Close to the damage threshold predominantly HSFL are observed. Black-Right-Pointing-Pointer The HSFL period remains almost constant {approx}375 nm (delay independent). Black-Right-Pointing-Pointer At high fluences and for short delays a transient metallic state is created (LSFL regime). Black-Right-Pointing-Pointer A transition of the LSFL period from 750 to 530 nm is observed in the sub-ps delay range. - Abstract: The formation of laser-induced periodic surface structures (LIPSS) upon irradiation of fused silica with multiple irradiation sequences of parallel polarized Ti:sapphire femtosecond laser pulse pairs (160 fs pulse duration, 800 nm central wavelength) was studied experimentally. For that purpose, a Michelson interferometer was used to generate near-equal-energy double-pulse sequences allowing the temporal pulse delay between the parallel-polarized individual fs-laser pulses to be varied between 0 and 40 ps with {approx}0.2 ps temporal resolution. The surface morphologies of the irradiated surface areas were characterized by means of scanning electron and scanning force microscopy. In the sub-ps delay range a strong decrease of the LIPSS periods and the ablation crater depths with the double-pulse delay was observed indicating the importance of the laser-induced free-electron plasma in the conduction band of the solids for the formation of LIPSS.

  1. Optical and structural properties of polycrystalline CVD diamond films grown on fused silica optical fibres pre-treated by high-power sonication seeding

    Science.gov (United States)

    Bogdanowicz, R.; Śmietana, M.; Gnyba, M.; Gołunski, Ł.; Ryl, J.; Gardas, M.

    2014-09-01

    In this paper, the growth of polycrystalline chemical vapour deposition (CVD) diamond thin films on fused silica optical fibres has been investigated. The research results show that the effective substrate seeding process can lower defect nucleation, and it simultaneously increases surface encapsulation. However, the growth process on glass requires high seeding density. The effects of suspension type and ultrasonic power were the specific objects of investigation. In order to increase the diamond density, glass substrates were seeded using a high-power sonication process. The highest applied power of sonotrode reached 72 W during the performed experiments. The two, most common diamond seeding suspensions were used, i.e. detonation nanodiamond dispersed in (a) dimethyl sulfoxide and (b) deionised water. The CVD diamond nucleation and growth processes were performed using microwave plasma assisted chemical vapour deposition system. Next, the seeding efficiency was determined and compared using the numerical analysis of scanning electron microscopy images. The molecular composition of nucleated diamond was examined with micro-Raman spectroscopy. The sp3/sp2 band ratio was calculated using Raman spectra deconvolution method. Thickness, roughness, and optical properties of the nanodiamond films in UV-vis wavelength range were investigated by means of spectroscopic ellipsometry. It has been demonstrated that the high-power sonication process can improve the seeding efficiency on glass substrates. However, it can also cause significant erosion defects at the fibre surface. We believe that the proposed growth method can be effectively applied to manufacture the novel optical fibre sensors. Due to high chemical and mechanical resistance of CVD diamond films, deposition of such films on the sensors is highly desirable. This method enables omitting the deposition of an additional adhesion interlayer at the glass-nanocrystalline interface, and thus potentially increases

  2. Evaluation of Superparamagnetic Silica Nanoparticles for Extraction of Triazines in Magnetic in-Tube Solid Phase Microextraction Coupled to Capillary Liquid Chromatography

    Science.gov (United States)

    González-Fuenzalida, R. A.; Moliner-Martínez, Y.; Prima-Garcia, Helena; Ribera, Antonio; Campins-Falcó, P.; Zaragozá, Ramon J.

    2014-01-01

    The use of magnetic nanomaterials for analytical applications has increased in the recent years. In particular, magnetic nanomaterials have shown great potential as adsorbent phase in several extraction procedures due to the significant advantages over the conventional methods. In the present work, the influence of magnetic forces over the extraction efficiency of triazines using superparamagnetic silica nanoparticles (NPs) in magnetic in tube solid phase microextraction (Magnetic-IT-SPME) coupled to CapLC has been evaluated. Atrazine, terbutylazine and simazine has been selected as target analytes. The superparamagnetic silica nanomaterial (SiO2-Fe3O4) deposited onto the surface of a capillary column gave rise to a magnetic extraction phase for IT-SPME that provided a enhancemment of the extraction efficiency for triazines. This improvement is based on two phenomena, the superparamegnetic behavior of Fe3O4 NPs and the diamagnetic repulsions that take place in a microfluidic device such a capillary column. A systematic study of analytes adsorption and desorption was conducted as function of the magnetic field and the relationship with triazines magnetic susceptibility. The positive influence of magnetism on the extraction procedure was demonstrated. The analytical characteristics of the optimized procedure were established and the method was applied to the determination of the target analytes in water samples with satisfactory results. When coupling Magnetic-IT-SPME with CapLC, improved adsorption efficiencies (60%–63%) were achieved compared with conventional adsorption materials (0.8%–3%).

  3. Preparation and evaluation of open tubular C18-silica monolithic microcartridges for preconcentration of peptides by on-line solid phase extraction capillary electrophoresis.

    Science.gov (United States)

    Ortiz-Villanueva, Elena; Benavente, Fernando; Giménez, Estela; Yilmaz, Fatma; Sanz-Nebot, Victoria

    2014-10-10

    In this study, C18-silica monoliths were synthesized as a porous layer in open tubular capillary columns, to be cut later into microcartridges for the analysis of neuropeptides by on-line solid-phase extraction capillary electrophoresis with UV and MS detection (SPE-CE-UV and SPE-CE-MS). First, several types of C18-silica monolithic (MtC18) microcartridges were used to analyse standard solutions of five neuropeptides (i.e. dynorphin A (1-7), substance P (7-11), endomorphin 1, methionine enkephalin and [Ala]-methionine enkephalin). The MtC18 sorbents were especially selective against endomorphin 1 and substance P (7-11)). The best results in terms of sensitivity and inter-microcartridge reproducibility were achieved with the microcartridges obtained from a 10-cm open tubular capillary column with a thin monolithic coating with large through-pores (1-5μm). Run-to-run repeatability, microcartridge durability, linearity ranges and LODs were studied by MtC18-SPE-CE-MS. As expected due to their greater selectivity, the best LOD enhancement was obtained for End1 and SP (7-11) (50 times with regard to CE-MS). Finally, the suitability of the methodology for analysing biological fluids was tested with plasma samples spiked with End1 and SP (7-11). Results obtained were promising because both neuropeptides could be detected at 0.05μgmL(-1), which was almost the same concentration level as for the standard solutions (0.01μgmL(-1)).

  4. Synthesis of robust hierarchical silica monoliths by surface-mediated solution/precipitation reactions over different scales: designing capillary microreactors for environmental applications.

    Science.gov (United States)

    García-Aguilar, J; Miguel-García, I; Berenguer-Murcia, Á; Cazorla-Amorós, D

    2014-12-24

    A synthetic procedure to prepare novel materials (surface-mediated fillings) based on robust hierarchical monoliths is reported. The methodology includes the deposition of a (micro- or mesoporous) silica thin film on the support followed by growth of a porous monolithic SiO2 structure. It has been demonstrated that this synthesis is viable for supports of different chemical nature with different inner diameters without shrinkage of the silica filling. The formation mechanism of the surface-mediated fillings is based on a solution/precipitation process and the anchoring of the silica filling to the deposited thin film. The interaction between the two SiO2 structures (monolith and thin film) depends on the porosity of the thin film and yields composite materials with different mechanical stability. By this procedure, capillary microreactors have been prepared and have been proved to be highly active and selective in the total and preferential oxidation of carbon monoxide (TOxCO and PrOxCO).

  5. Fused Zirconia

    Institute of Scientific and Technical Information of China (English)

    2011-01-01

    ScopeThis standard specifies the terms,definitions,classification,brands,technical requirements,test methods,inspection rules,packing,marking,transportation,storage,and quality certificate of fused zirconia.This standard is applicable to monoclinic fused zirconia and partially stabilized fused zirconia.

  6. The analysis of the effect of homogeneous mechanical stress on the acoustic wave propagation in the "La3Ga5SiO14/fused silica" piezoelectric layered structure.

    Science.gov (United States)

    Burkov, S I; Zolotova, O P; Sorokin, B P; Turchin, P P

    2015-01-01

    The results of computer simulation taking into account the linear and nonlinear material constants have been presented. Study of the influence of external uniaxial mechanical stress on the dispersive characteristics of elastic waves in piezoelectric structures as "La3Ga5SiO14/fused silica" has been executed. The comparison of elastic wave velocity changes under the influence of an uniaxial stress while a full set of nonlinear material constants of crystalline layer+geometric nonlinearity, or only geometric nonlinearity of the layer induced by the static deformation of a substrate, has been fulfilled.

  7. Laser welding of fused silica glass with sapphire using a non- stoichiometric, fresnoitic Ba2TiSi2O8·3 SiO2 thin film as an absorber

    Science.gov (United States)

    de Pablos-Martín, A.; Lorenz, M.; Grundmann, M.; Höche, Th.

    2017-07-01

    Laser welding of dissimilar materials is challenging, due to their difference in coefficients of thermal expansion (CTE). In this work, fused silica-to-sapphire joints were achieved by employment of a ns laser focused in the intermediate Si-enriched fresnoitic glass thin film sealant. The microstructure of the bonded interphase was analyzed down to the nanometer scale and related to the laser parameters used. The crystallization of fresnoite in the glass sealant upon laser process leads to an intense blue emission intensity under UV excitation. This crystallization is favored in the interphase with the silica glass substrate, rather than in the border with the sapphire. The formation of SiO2 particles was confirmed, as well. The bond quality was evaluated by scanning acoustic microscopy (SAM). The substrates remain bonded even after heat treatment at 100 °C for 30 min, despite the large CTE difference between both substrates.

  8. Novel cationic polyelectrolyte coatings for capillary electrophoresis.

    Science.gov (United States)

    Duša, Filip; Witos, Joanna; Karjalainen, Erno; Viitala, Tapani; Tenhu, Heikki; Wiedmer, Susanne K

    2016-01-01

    The use of bare fused silica capillary in CE can sometimes be inconvenient due to undesirable effects including adsorption of sample or instability of the EOF. This can often be avoided by coating the inner surface of the capillary. In this work, we present and characterize two novel polyelectrolyte coatings (PECs) poly(2-(methacryloyloxy)ethyl trimethylammonium iodide) (PMOTAI) and poly(3-methyl-1-(4-vinylbenzyl)-imidazolium chloride) (PIL-1) for CE. The coated capillaries were studied using a series of aqueous buffers of varying pH, ionic strength, and composition. Our results show that the investigated polyelectrolytes are usable as semi-permanent (physically adsorbed) coatings with at least five runs stability before a short coating regeneration is necessary. Both PECs showed a considerably decreased stability at pH 11.0. The EOF was higher using Good's buffers than with sodium phosphate buffer at the same pH and ionic strength. The thickness of the PEC layers studied by quartz crystal microbalance was 0.83 and 0.52 nm for PMOTAI and PIL-1, respectively. The hydrophobicity of the PEC layers was determined by analysis of a homologous series of alkyl benzoates and expressed as the distribution constants. Our result demonstrates that both PECs had comparable hydrophobicity, which enabled separation of compounds with log Po/w > 2. The ability to separate cationic drugs was shown with β-blockers, compounds often misused in doping. Both coatings were also able to separate hydrolysis products of the ionic liquid 1,5-diazabicyclo[4.3.0]non-5-ene acetate at highly acidic conditions, where bare fused silica capillaries failed to accomplish the separation.

  9. Influence of clay and silica on permeability and capillary entry pressure of chalk reservoirs in the North Sea

    DEFF Research Database (Denmark)

    Røgen, Birte; Fabricius, Ida Lykke

    2002-01-01

    The permeability and capillary entry pressure of chalk reservoirs are controlled by their porosity and specific surface area. Measured permeabilities are in the range 0.025-5.3 mD and are successfully predicted by use of the Kozeny equation. In this paper we focus on the factors that control...

  10. Histidine-modified organic-silica hybrid monolithic column for mixed-mode per aqueous and ion-exchange capillary electrochromatography.

    Science.gov (United States)

    Tang, Sheng; Liu, Shujuan; Liang, Xiaojing; Tang, Xiaofen; Wu, Xingcai; Guo, Yong; Liu, Xia; Jiang, Shengxiang

    2015-06-01

    A novel organic-silica hybrid monolith was prepared through the binding of histidine onto the surface of monolithic matrix for mixed-mode per aqueous and ion-exchange capillary electrochromatography. The imidazolium and amino groups on the surface of the monolithic stationary phase were used to generate an anodic electro-osmotic flow as well as to provide electrostatic interaction sites for the charged compounds at low pH. Typical per aqueous chromatographic behavior was observed in water-rich mobile phases. Various polar and hydrophilic analytes were selected to evaluate the characteristics and chromatographic performance of the obtained monolith. Under per aqueous conditions, the mixed-mode mechanism of hydrophobic and ion-exchange interactions was observed and the resultant monolithic column proved to be very versatile for the efficient separations of these polar and hydrophilic compounds (including amides, nucleosides and nucleotide bases, benzoic acid derivatives, and amino acids) in highly aqueous mobile phases. The successful applications suggested that the histidine-modified organic-silica hybrid monolithic column could offer a wide range of retention behaviors and flexible selectivities toward polar and hydrophilic compounds.

  11. Effect of the silanization conditions on chromatographic behavior of an open-tubular capillary column coated with a modified silica-gel thin layer.

    Science.gov (United States)

    Nakano, Yusuke; Kitagawa, Shinya; Miyabe, Kanji; Tsuda, Takao

    2005-10-01

    The performance of an open-tubular capillary column coated with a modified silica-gel thin layer was investigated, particularly concerning the effect of the silanization process on it. Although the increase in the octadecyltriethoxysilane (ODTES) concentration in the silanization process could enhance the retention factor of naphthalene, its theoretical plate number was significantly reduced (ODTES, 5 to 50%; k, 0.2 to 4.3; N, 79600 to 2600 m(-1)). Namely, the increase in the retention factor was accompanied by a decrease in the theoretical plate number. A similar phenomenon was also observed when octadecyldimethylchlorosilane (ODCS) was used as the silanization regent. However, increases in both the retention factor and the theoretical plate number could be achieved (sample, naphthalene; k, 0.05 to 0.09; N, 149000 to 220000 m(-1)) by a NaOH treatment to the fabricated thin porous silica-gel layer before silanization with ODCS. The electrochromatographic separation of proteins and peptides by using the NaOH-treated column could obtain more peaks than electrophoretic separation.

  12. Preparation and characterization of silica monolith modified with bovine serum albumin-gold nanoparticles conjugates and its use as chiral stationary phases for capillary electrochromatography.

    Science.gov (United States)

    Lu, Junyu; Ye, Fanggui; Zhang, Aizhu; Wei, Zong; Peng, Yan; Zhao, Shulin

    2011-08-01

    This paper describes the development of silica monolith modified with bovine serum albumin-gold nanoparticles (BSA-GNPs) conjugates as chiral stationary phases for capillary electrochromatography (CEC). The bare monolithic silica column was prepared by a sol-gel process and has been modified chemically with 3-mercaptopropyltrimethoxysilane to provide thiol groups, followed by immobilization of gold nanoparticles via the formation of an Au-S bond and modification with BSA as the chiral selector via the nitrogen lone pair of electrons. It has been demonstrated that the monolithic chiral stationary phases can be used for the enantioseparation of a number of phenylthiocarbamyl amino acids (PTC-D/L-AAs) by CEC. Ten pairs of tested amino acids enantiomers were successfully resolved within 18 min under optimized conditions, and the resolution values were in the range of 1.486-2.083. With PTC-D/L-tryptophan used as the probe solute, the influences of applied voltage, organic modifier and buffer pH in mobile phase on apparent retention factor, enantioselectivity and resolution factor were also investigated.

  13. 不同形态石英玻璃的析晶动力学研究%Crystallization kinetics of different morphologies of fused silica glass

    Institute of Scientific and Technical Information of China (English)

    温广武; 雷廷权; 周玉

    2001-01-01

    应用XRD技术对三种形态(块状,粉末和纤维)石英玻璃在1 200~1 500℃范围内的等温析晶动力学过程进行了实验研究.实验结果表明,不同形态石英玻璃的析晶产物都是低温方石英,但形态不同的石英玻璃的析晶开始温度,同一温度下的析晶量及析晶量随温度的变化关系是不同的.三种形态石英玻璃析晶动力学可较好地用Avrami方程表示,其中块状,粉末和纤维的平均n值分别为1.65,1.68和1.92,活化能分别为495,445和430 kJ/mo1.析晶中的成核为表面成核机制.晶体生长受扩散和重排双重控制,随比表面和杂质含量的增大(块状→粉末→纤维),控制因素中扩散的比例降低,而重排的比例上升,因而n值上升而活化能下降,析晶倾向增大.%Kinetics of crystallization process of three forms (bulk, powder and fiber) of fused silica has been inves-tigated by means of XRD in the range of 1 200~1500 ℃. The results show that, the crystalline phases precipitatedare cristobalite in all specimens, but there are some difference in the starting temperature, degree of crystallinityand the variation of crystallinity with temperature among them. The kinetics of crystallization can be formulated withAvrami equation with n values of 1.65,1.68 and 1.92, and the activation energy of 495,445 and 430 kJ/mol forbulk, powder and fiber specimens, respectively. The nucleation can be thought of the surface mechanism and thecrystal growth is controlled by both diffusion and re-arrangement of atoms. With increasing specific area and impu-rity, the weight of the diffusion factor is decreased whereas that of the re-arrangement is increased, and thus the nvalue increases and the activation energy decreases. Therefore, the tendency to crystallization increases.

  14. Fast capillary electrophoresis-time-of-flight mass spectrometry using capillaries with inner diameters ranging from 75 to 5 μm.

    Science.gov (United States)

    Grundmann, Marco; Matysik, Frank-Michael

    2011-04-01

    Fast electrophoretic separations in fused silica capillaries (CE) coupled to time-of-flight mass spectrometry (TOF-MS) are presented. CE separations of the model analytes (epinephrine, norepinephrine, dopamine, histidine, and isoproterenol) under conditions of high electric field strengths of up to 1.25 kV cm(-1) are completed in 20 s. Coupling of CE with TOF-MS is accomplished using a coaxial sheath liquid electrospray ionization interface. The influence of parameters inherent to the interface and their effects, including suction pressure and dilution, are discussed. In addition to standard capillaries of 75 and 50 μm inner diameter (ID), separations in capillaries with IDs of 25, 15, and 5 μm have been successfully applied to this setup. The analytical performance is compared over this range of capillary dimensions, and both advantages and disadvantages are discussed.

  15. Synthesis and characterization of a multimode stationary phase: Congo red derivatized silica in nano-flow HPLC.

    Science.gov (United States)

    Zhang, Yi; Zhang, Yan; Wang, Guan; Chen, Wujuan; He, Pingang; Wang, Qingjiang

    2016-02-01

    A novel Congo red (CR) derivatized silica stationary phase was prepared and packed into a fused silica capillary tube for nano-flow HPLC. A variety of analytes including poly-aromatic hydrocarbons, parabens, acids, sulfonamides, bases, and nucleosides were successfully separated using the CR. In comparison with commercial ODS columns, this new stationary phase has a different separation mechanism (hydrophobically-assisted ion-exchange), which was evident in the separation of benzoic acid derivatives and sulfonamides. The successful application of CR-bonded silica stationary phase in the HILIC and PALC modes demonstrates the effectiveness of this potential chromatographic material in nano flow HPLC.

  16. Analysis of urinary drugs of abuse by a multianalyte capillary electrophoretic immunoassay.

    Science.gov (United States)

    Caslavska, J; Allemann, D; Thormann, W

    1999-04-09

    This paper characterizes a novel multianalyte competitive binding, electrokinetic capillary-based immunoassay for urinary methadone, opiates, benzoylecgonine (cocaine metabolite) and amphetamines. After incubation of 25 microliters urine with the reactants for several minutes in the presence of an internal standard, a small aliquot of the mixture is applied onto a fused-silica capillary and the unbound fluorescein labelled drug tracers are monitored by capillary electrophoresis with on-column laser induced fluorescence detection. The multianalyte assay is shown to be rapid, simple, quantitative, capable of recognizing urinary drug concentrations > or = 30 ng/ml and suitable for screening of patient urines. Data are demonstrated to compare well with those obtained by routine screening methods based on enzyme multiplied immunoassay techniques and fluorescence polarization immunoassays. The electrokinetic capillary assay has been validated via analysis of external quality control urines and confirmation analysis of patient urines using GC-MS.

  17. Pneumatic Microvalve-Based Hydrodynamic Sample Injection for High-Throughput, Quantitative Zone Electrophoresis in Capillaries

    Energy Technology Data Exchange (ETDEWEB)

    Kelly, Ryan T.; Wang, Chenchen; Rausch, Sarah J.; Lee, Cheng S.; Tang, Keqi

    2014-07-01

    A hybrid microchip/capillary CE system was developed to allow unbiased and lossless sample loading and high throughput repeated injections. This new hybrid CE system consists of a polydimethylsiloxane (PDMS) microchip sample injector featuring a pneumatic microvalve that separates a sample introduction channel from a short sample loading channel and a fused silica capillary separation column that connects seamlessly to the sample loading channel. The sample introduction channel is pressurized such that when the pneumatic microvalve opens briefly, a variable-volume sample plug is introduced into the loading channel. A high voltage for CE separation is continuously applied across the loading channel and the fused silica capillary separation column. Analytes are rapidly separated in the fused silica capillary with high resolution. High sensitivity MS detection after CE separation is accomplished via a sheathless CE/ESI-MS interface. The performance evaluation of the complete CE/ESI-MS platform demonstrated that reproducible sample injection with well controlled sample plug volumes could be achieved by using the PDMS microchip injector. The absence of band broadening from microchip to capillary indicated a minimum dead volume at the junction. The capabilities of the new CE/ESI-MS platform in performing high throughput and quantitative sample analyses were demonstrated by the repeated sample injection without interrupting an ongoing separation and a good linear dependence of the total analyte ion abundance on the sample plug volume using a mixture of peptide standards. The separation efficiency of the new platform was also evaluated systematically at different sample injection times, flow rates and CE separation voltages.

  18. One-pot preparation of a mixed-mode organic-silica hybrid monolithic capillary column and its application in determination of endogenous gibberellins in plant tissues.

    Science.gov (United States)

    Zhang, Zheng; Hao, Yan-Hong; Ding, Jun; Xu, Sheng-Nan; Yuan, Bi-Feng; Feng, Yu-Qi

    2015-10-16

    A newly improved one-pot method, based on "thiol-ene" click chemistry and sol-gel approach in microemulsion system, was developed for the preparation of C8/PO(OH)2-silica hybrid monolithic capillary column. The prepared monolith possesses large specific surface area, narrow mesopore size distribution and high column efficiency. The monolithic column was demonstrated to have cation exchange/reversed-phase (CX/RP) mixed-mode retention for analytes on nano-liquid chromatography (nano-LC). On the basis of the developed nano-LC system with MS detector coupled to pipette tip solid phase extraction (PT-SPE) and derivatization process, we then realized simultaneous determination of 10 gibberellins (GAs) with low limits of detection (LODs, 0.003-0.025 ng/mL). Furthermore, 6 endogenous GAs in only 5mg rice leaves (fresh weight) were successfully detected and quantified. The developed PT-SPE-nano-LC-MS strategy may offer promising applications in the determination of low abundant bioactive molecules from complex matrix.

  19. Derivatized nanoparticle coated capillaries for purification and micro-extraction of proteins and peptides.

    Science.gov (United States)

    Bakry, R; Gjerde, D; Bonn, G K

    2006-06-01

    Various methods are used to enrich or purify a protein of interest from other proteins and components in a crude cell lysate or other sample. One of the most powerful methods is affinity purification, also called affinity chromatography, whereby the proteins of interest are purified by virtue of their specific binding properties to an immobilized ligand. Affinity purification is becoming more widely used for exploring post-translation modifications and protein-protein interactions, especially with a view toward developing new general tag systems and strategies of chemical derivatization on peptides for affinity selection. Our work was aimed to immobilize proteins or ligands for affinity purification of antibodies, fusion-tagged proteins and other proteins and peptides. Selected proteins or peptides are efficiently extracted and enriched using chemically derivatized walls of a fused silica capillary column. In this paper, we present an open tubular capillary, where the inner wall of a fused silica capillary was derivatized by covalent binding of modified polystyrene latex particles. The capillaries were derivatized with iminodiacetic acid and loaded with Fe3+ or Ni2+ for the purification and enrichment of phosphopeptides or His-tagged proteins, respectively. The latex coated capillaries have been successfully applied to enrich phosphopeptides from beta-casein tryptic digest and ovalbumin tryptic digest at a micro volume scale with recoveries ranging from 92 to 95%. The capillaries have been eluted under conditions compatible with MALDI-MS without any prior desalting step. In another approach, concanavalin A (Con A) or Protein G were immobilized on the epoxy modified latex on the inner wall of the fused silica capillary for the purification of glycoproteins and immunoglobulin, respectively. The design of the capillary and the protocols used for purification permits the direct detection of eluted proteins and peptides with gel electrophoresis or with mass spectrometry

  20. Application of the copolymers containing sulfobetaine methacrylate in protein separation by capillary electrophoresis.

    Science.gov (United States)

    Cao, Fuhu; Tan, Lin; Xiang, Lina; Liu, Songtao; Wang, Yanmei

    2013-01-01

    This study describes the formation of highly efficient antiprotein adsorption random copolymer coating of poly(N,N-dimethylacrylamide-co-sulfobetaine methacrylate) (poly(DMA-co-SBMA)) on the fused-silica capillary inner wall. Firstly, the poly(DMA-co-SBMA)s with different feed ratio (SBMA/DMA) were synthesized via the reversible addition fragmentation chain transfer polymerization. And then, X-ray photoelectron spectroscopy (XPS) and water contact angle (CA) were used to investigate the composition and hydrophilicity of poly(DMA-co-SBMA) coating formed on the glass slide surfaces. CA measurements revealed that the poly(DMA-co-SBMA) coating became more hydrophilic with the increment of feed ratio (SBMA/DMA), and at the same time, the XPS results showed that the coating ability was also increased with the increment of feed ratio. Followed, the copolymer was applied to coat the fused-silica capillary inner wall, and the coated capillary was used to separate the mixture of proteins (lysozyme, cytochrome c, ribonuclease A, and α-chymotrypsinogen A) in a pH range from 3.0 to 5.0. Under the optimum conditions, an excellent separation of basic proteins with peak efficiencies ranging from 551,000 to 1509,000 N/m had been accomplished within 10 min. Furthermore, the effect of coating composition on protein separation was also investigated through the comparison of separation efficiency achieved by using bare, PSBMA- and poly(DMA-co-SBMA)-coated capillary, respectively.

  1. An immobilized carboxyl containing metal-organic framework-5 stationary phase for open-tubular capillary electrochromatography.

    Science.gov (United States)

    Bao, Tao; Tang, Pingxiu; Mao, Zhenkun; Chen, Zilin

    2016-07-01

    A novel capillary column with metal-organic framework-5 (MOF-5) as the stationary phase was prepared for open-tubular capillary electrochromatography (OT-CEC). To grow MOF-5, the fused-silica capillary was functionalized firstly using 3-aminopropyltriethoxysilane and glutaraldehyde as covalent linkers; and then MOF-5 would be immobilized on the inner wall of COOH-terminated capillary by epitaxial growth, to produce a MOF-5-modified capillary. The successful growth of MOF-5 has been characterized and confirmed by scanning electron microscopy, X-Ray diffraction and Fourier transform infrared spectra. The influence of pH value and methanol on electroosmotic flow (EOF) of the MOF-5-modified capillary column was investigated. The EOF showed a pH-dependent from anode to cathode. The immobilization of MOF-5 improved the interactions between analytes and layer on inner wall of the capillary. Excellent separations of substituted benzenes and acidic and basic analytes were obtained on the fabricated capillary columns. The MOF-5-modified capillary columns exhibited good repeatability, with relative standard deviations for intra-day, inter-day runs and column-to-column less than 1.87%, 3.53%, and 8.49%, respectively. Our successful application of MOF-5 paved the way for introducing series of dicarboxylate-based isoreticular MOFs to OT-CEC as novel stationary phase.

  2. Silica- and germania-based dual-ligand sol-gel organic-inorganic hybrid sorbents combining superhydrophobicity and π-π interaction. The role of inorganic substrate in sol-gel capillary microextraction.

    Science.gov (United States)

    Seyyal, Emre; Malik, Abdul

    2017-04-29

    Principles of sol-gel chemistry were utilized to create silica- and germania-based dual-ligand surface-bonded sol-gel coatings providing enhanced performance in capillary microextraction (CME) through a combination of ligand superhydrophobicity and π-π interaction. These organic-inorganic hybrid coatings were prepared using sol-gel precursors with bonded perfluorododecyl (PF-C12) and phenethyl (PhE) ligands. Here, the ability of the PF-C12 ligand to provide enhanced hydrophobic interaction was advantageously combined with π-π interaction capability of the PhE moiety to attain the desired sorbent performance in CME. The effect of the inorganic sorbent component on microextraction performance of was explored by comparing microextraction characteristics of silica- and germania-based sol-gel sorbents. The germania-based dual-ligand sol-gel sorbent demonstrated superior CME performance compared to its silica-based counterpart. Thermogravimetric analysis (TGA) of the created silica- and germania-based dual-ligand sol-gel sorbents suggested higher carbon loading on the germania-based sorbent. This might be indicative of more effective condensation of the organic ligand-bearing sol-gel-active chemical species to the germania-based sol-gel network (than to its silica-based counterpart) evolving in the sol solution. The type and concentration of the organic ligands were varied in the sol-gel sorbents to fine-tune extraction selectivity toward different classes of analytes. Specific extraction (SE) values were used for an objective comparison of the prepared sol-gel CME sorbents. The sorbents with higher content of PF-C12 showed remarkable affinity for aliphatic hydrocarbons. Compared to their single-ligand sol-gel counterparts, the dual-ligand sol-gel coatings demonstrated significantly superior CME performance in the extraction of alkylbenzenes, providing up to ∼65.0% higher SE values. The prepared sol-gel CME coatings provided low ng L(-1) limit of detections (LOD

  3. Novel bimodal porous N-(2-aminoethyl)-3-aminopropyltrimethoxysilane-silica monolithic capillary microextraction and its application to the fractionation of aluminum in rainwater and fruit juice by electrothermal vaporization inductively coupled plasma mass spectrometry

    Science.gov (United States)

    Zheng, Fei; Hu, Bin

    2008-01-01

    A novel bimodal porous N-(2-aminoethyl)-3-aminopropyltrimethoxysilane (AAPTS)-silica monolithic capillary was prepared by sol-gel technology, and used as capillary microextraction (CME) column for aluminum fractionation by electrothermal vaporization inductively coupled plasma mass spectrometry (ETV)-ICP-MS with the use of polytetrafluoroethylene (PTFE) slurry as fluorinating agent. The extraction behaviors of different Al species were studied and it was found that in the pH range of 4-7, labile monomeric Al (free Al 3+, Al-OH and Al-F) could be retained quantitatively on the monolithic capillary, while non-labile monomeric Al (Al-Cit and Al-EDTA) passed through the capillary directly. The labile monomeric Al retained on monolithic capillary was eluted with 10 μL 1 mol L - 1 HCl and the elution was introduced into the ETV for fluorination assisted ETV-ICP-MS determination. The total monomeric Al fraction was also determined by AAPTS-silica monolithic CME-fluorination-assisted electrothermal vaporization (FETV)-ICP-MS after the sample solution was adjusted to pH 8.8. Non-labile monomeric Al was obtained by subtracting labile monomeric Al from the total monomeric Al. Under the optimized conditions, the relative standard deviation (R.S.D) was 6.2% ( C = 1 μg L - 1 , n = 7; sample volume, 5 mL), and the limit of detection was 1.6 ng L - 1 for Al with an enrichment factor of 436 fold and a sampling frequency of 9 h - 1 . The prepared AAPTS-silica monolithic capillary showed an excellent pH tolerance and solvent stability and could be used for more than 250 times without decreasing adsorption efficiency. The developed method was applied to the fraction of Al in rainwater and fruit juice, and the results demonstrated that the established system had advantages over the existing 8-hydroxyquinoline (8-HQ) chelating system for Al fractionation such as wider pH range, higher tolerance of interference and better regeneration.

  4. Capillary electrophoresis with noncovalently bilayer-coated capillaries for stability study of allergenic proteins in simulated gastrointestinal fluids.

    Science.gov (United States)

    Zheng, Chang; Liu, Youping; Zhou, Qiuhong; Di, Xin

    2010-10-15

    A novel noncovalently bilayer-coated capillary using cationic polymer polybrene (PB) and anionic polymer (sodium 4-styrenesulfonate) (PSS) as coatings was prepared. This PB-PSS coating showed good migration-time reproducibility for proteins and high stability in the range of pH 2-10 and in the presence of 1M NaOH, acetonitrile and methanol. Capillary electrophoresis with PB-PSS coated capillaries was successfully applied to quantitatively investigate the stability of bovine serum albumin, ovomucoid, β-lactoglobulin and lysozyme in simulated gastrointestinal fluids. β-lactoglobulin A and β-lactoglobulin B were both stable in simulated gastric fluid with degradation percentages of 34.3% and 17.2% after 60min of incubation, respectively. Bovine serum albumin, ovomucoid and lysozyme were stable in simulated intestinal fluid with degradation percentages of 17.7%, 23.4% and 22.8% after 60min of incubation, respectively. The superiority of the proposed method over sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE) and capillary electrophoresis with untreated fused silica capillaries was demonstrated and emphasized.

  5. DNA Sequencing Using capillary Electrophoresis

    Energy Technology Data Exchange (ETDEWEB)

    Dr. Barry Karger

    2011-05-09

    The overall goal of this program was to develop capillary electrophoresis as the tool to be used to sequence for the first time the Human Genome. Our program was part of the Human Genome Project. In this work, we were highly successful and the replaceable polymer we developed, linear polyacrylamide, was used by the DOE sequencing lab in California to sequence a significant portion of the human genome using the MegaBase multiple capillary array electrophoresis instrument. In this final report, we summarize our efforts and success. We began our work by separating by capillary electrophoresis double strand oligonucleotides using cross-linked polyacrylamide gels in fused silica capillaries. This work showed the potential of the methodology. However, preparation of such cross-linked gel capillaries was difficult with poor reproducibility, and even more important, the columns were not very stable. We improved stability by using non-cross linked linear polyacrylamide. Here, the entangled linear chains could move when osmotic pressure (e.g. sample injection) was imposed on the polymer matrix. This relaxation of the polymer dissipated the stress in the column. Our next advance was to use significantly lower concentrations of the linear polyacrylamide that the polymer could be automatically blown out after each run and replaced with fresh linear polymer solution. In this way, a new column was available for each analytical run. Finally, while testing many linear polymers, we selected linear polyacrylamide as the best matrix as it was the most hydrophilic polymer available. Under our DOE program, we demonstrated initially the success of the linear polyacrylamide to separate double strand DNA. We note that the method is used even today to assay purity of double stranded DNA fragments. Our focus, of course, was on the separation of single stranded DNA for sequencing purposes. In one paper, we demonstrated the success of our approach in sequencing up to 500 bases. Other

  6. Analysis of recombinant human growth hormone by capillary electrophoresis with bilayer-coated capillaries using UV and MS detection.

    Science.gov (United States)

    Catai, Jonatan R; Sastre Toraño, Javier; Jongen, Peter M J M; de Jong, Gerhardus J; Somsen, Govert W

    2007-06-01

    The characterization of recombinant human growth hormone (rhGH; somatropin) by capillary electrophoresis (CE) with UV-absorbance and mass spectrometric (MS) detection using capillaries noncovalently coated with polybrene (PB) and poly(vinyl sulfonic acid) (PVS) is demonstrated. Compared with bare fused-silica capillaries, PB-PVS coated capillaries yielded more favorable migration-time reproducibilities and higher separation efficiencies. Optimal separation conditions for the bilayer-coated capillaries comprised a background electrolyte (BGE) of 400 mM Tris phosphate (pH 8.5) yielding migration-time R.S.D.s of less than 1.0% and plate numbers above 300,000 for intact rhGH. The protein was also analyzed using the CE method described in the European Pharmacopoeia (Ph. Eur.) monograph. The pharmacopoeial method gave much longer analysis times (22 min versus 8 min), lower resolution and plate numbers, and consecutive shifts in migration time for rhGH, indicating possible interactions between the protein and the inner capillary wall. Due to stable migration times obtained with the coated capillaries, reliable profiling and quantification of rhGH and its byproducts in time was possible. Analysis of thermally degraded rhGH revealed the formation of two main degradation products. CE-mass spectrometry (MS) of this sample, using a PB-PVS coated capillary and a BGE of 75 mM ammonium formate (pH 8.5), suggests that these products are desamido forms of rhGH. Analyses of expired rhGH preparations with CE-UV and CE-MS indicated the presence of both deamidation and oxidation products.

  7. 单个脉冲作用下熔融石英的温度和热应力研究%Research on the temperature and thermal stress of fused silica irradiated by a laser pulse

    Institute of Scientific and Technical Information of China (English)

    李世雄; 张正平; 秦水介; 陈德良

    2016-01-01

    The models of temperature and thermal stress distribution in optical material irradiated by a laser pulse are researched theoretically.Based on the pulse characteristics,the temperature distribution models for long pulse and short pulse are built respectively,and on this basis,thermal stress distribution model is further set up.Taking fused silica as an example,the temperature and thermal stress distribution are calculated and analyzed.The results indicate that the temperature distribution profiles at the end of the pulse are same for long pulse and short pulse model.The theoretical analysis shows that the temperature near the spot center reaches the melting point or vapor point of fused silica,which leads to a melt damage or evaporation damage.The temperature rise in the focal areas is nonuniform, which leads to thermal stress.The thermal stress is greater than the fracture strength of sample,which induces the damage,such as thermal cracks.%理论研究单个激光脉冲作用光学材料的温度和热应力分布模型,根据脉冲特征,分别建立适用于短脉冲和长脉冲的温度分布模型;进一步建立单个脉冲作用下的热应力模型。以熔融石英为例数值计算和分析了单个脉冲作用下的温度和热应力分布。研究结果表明,如果只求解单脉冲结束时的温度分布,长脉冲和短脉冲模型计算结果一致。单个激光脉冲辐照熔融石英,材料温度升高,如果温度达到材料融化或汽化温度,将导致材料的熔融汽化破坏,另一方面,在焦点区域温升不均匀,将导致热应力产生,如果热应力达到材料的力学破坏阈值,将诱导材料的热应力损伤。

  8. Thermal stress simulation of laser induced damage of fused silica by contamination on the surface%表面污染物诱导熔石英损伤的热力学数值模拟

    Institute of Scientific and Technical Information of China (English)

    苗心向; 袁晓东; 程晓锋; 贺少勃; 郑万国

    2011-01-01

    为了研究高功率固体激光装置内污染诱导光学元件损伤问题,基于有限元数值方法,结合污染物诱导熔石英损伤机理,给出了熔石英样片在高功率脉冲激光辐照下的温度场和应力场分布.结果表明,激光脉冲辐照过程中主要以污染物的温度升高为主,最高至2800K,而样片温升不大,仅为7K;在激光脉冲辐照后100μs的时间内,样片表面中心快速升温至2200K,而边缘处仅为700K,在较短的距离内温度变化剧烈,由此产生的热应力导致表面发生损伤;损伤区域中心表现为压应力,边缘为拉应力,最大可达30.73MPa.测试了污染物诱导样片损伤斑的微观显微形貌,实验结果和理论计算结果符合较好.%In order to study the laser-induced damage mechanism in inertial confinement fusion system, temperature and thermal stress distributions in the fused silica, heated by repetition frequency laser, were given by means of finite element methods. The simulated results indicate the temperature of the contaminations rise to 2800K during the pulse laser irradiation, but the fused silica' s temperature mainly rise from 300K to 2200K in 100μs after irradiation, and damage induced by the thermal stress occurs. The strong compressive in the damage region is about 30. 73MPa. The highest stress outside the damage region is deviatoric hoop stress. The damage morphologies were tested by means of optical microscopy. The simulated outcomes correspond to the experiment result.

  9. Residual stress calculation method for fused silica polishing surface%熔石英元件抛光加工表面残余应力的计算方法

    Institute of Scientific and Technical Information of China (English)

    王洪祥; 侯晶; 严志龙; 朱本温; 陈贤华

    2015-01-01

    Fused silica glass is non⁃crystalline material, the traditional detection methods have complicated steps and low measurement accuracy, residual stresses are often unable to direct quantitative detection. A new residual stress calculation method for fused silica polishing surface was proposed based on brittle solid fracture mechanics, in which a series of nano⁃indentation experiments were conducted by a sharp indenter, and the sensitive parameters were extracted during indentation process, the experimental data were linear fit and the line slopes were determined, so residual stress was often calculated indirectly by measuring the other physical parameters change caused by residual stress. Comparative analysis showed that the calculation results had in good consistency with the test results obtained by stress birefringence analyzer, so the correctness of the residual stress calculation method was verified.%为解决传统检测方法无法直接定量检测非晶体熔石英玻璃表面残余应力的问题,基于脆性固体断裂力学理论,推导残余应力的理论计算公式,提出光学元件抛光加工表面残余应力计算新方法。采用尖锐压头进行纳米印压实验,提取压痕过程中对残余应力敏感的参数,并对实验数据进行线性拟合,确定拟合线的斜率,通过测量残余应力引起其他物理参数的变化计算残余应力。对比分析结果表明,计算得到残余应力值与应力双折射仪检测得到的数据基本吻合,验证了提出残余应力计算方法的正确性。

  10. Application of isotachophoresis in commercial capillary electrophoresis instrument using C(4) D and UV detection.

    Science.gov (United States)

    Koczka, Péter I; Bodor, Róbert; Masár, Marián; Gáspár, Attila

    2016-09-01

    In this work, we tested the applicability of a commercial CE instrument (Agilent) for capillary ITP (CITP). The fused silica capillaries were flushed with PVP solution before each sample injection to suppress the EOF. As a dual-detection mode, commercial capacitively coupled contactless conductivity detection and ultraviolet detectors were applied. The experiments showed that the detection gap of the capacitively coupled contactless conductivity detection limits the achievable LOD and the separation resolution when the analyte CITP zones are very narrow, therefore long (120 cm) CE capillary was used and it was largely filled with the sample solution. CITP analyses of several real samples (leather extract, red wine, juice, and fizzy drink) have been demonstrated. In peak mode of CITP when the zone of a chromophore analyte is positioned between nonchromophore zones, excellent sensitivity (in submicromolar concentration range) could be achieved by ultraviolet detection. The hazardous chromate in low concentration was determined in the aqueous extract of tanned leather.

  11. Non-Complexing Anions for Quantitative Speciation Studies Using Raman Spectroscopy in Fused Silica High-Pressure Optical Cells Under Hydrothermal Conditions.

    Science.gov (United States)

    Applegarth, Lucas M S G A; Alcorn, Christopher; Bissonette, Katherine; Noël, John; Tremaine, Peter R

    2015-08-01

    This paper reports methods for obtaining time-dependent reduced isotropic Raman spectra of aqueous species in quartz capillary high-pressure optical cells under hydrothermal conditions, as a means of determining quantitative speciation in hydrothermal fluids. The methods have been used to determine relative Raman scattering coefficients and to examine the thermal decomposition kinetics of the non-complexing anions bisulfate (HSO4(-)), perchlorate (CIO4(-)), perrhenate (ReO4(-)), and trifluoromethanesulfonate, or "triflate" (CF3SO3(-)) in acidic and neutral solutions at temperatures up to 400°C and 30 MPa. Arrhenius expressions for calculating the thermal decomposition rate constants are also reported. Thermal stabilities in the acidic solutions followed the order HSO4(-) (stable) > ReO4(-) > CIO4(-) > CF3SO3(-), with half-lives (t1/2) > 7 h at 300°C. In neutral solutions, the order was HSO4(-) (stable) > CF3SO3(-) > ReO4(-) > CIO4(-), with t1/2 > 8 h at 350°C. CF3SO3(-) was extremely stable in neutral solutions, with t1/2 > 11 h at 400°C.

  12. Preparation and evaluation of bonded linear polymethacrylate stationary phases for open tubular capillary electrokinetic chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Tan, Z.J.; Remcho, V.T. [West Virginia Univ., Morgantown, WV (United States)

    1997-02-15

    A new procedure for the preparation of thick polymethacrylate films bonded in 25 {mu}m i.d. fused-silica capillaries is developed. The etched silica surface is first modified with an unsaturated organosilane, which is later incorporated into the polymer film. The capillary is then filled with a monomer solution, and polymerization is initiated by incubation at elevated temperature. This thermoinitiation method enables the use of ordinary polyimide-jacketed capillaries in preparing the columns. The effect of monomer concentration on the resulting polymer film was studied by open tubular capillary electrokinetic chromatography using p-hydroxybenzoates (parabens) as test solutes. Good separations were achieved using short capillaries. Run-to-run retention time reproducibility was excellent, with RSDs of 2% (n = 50) being representative. For the linear polymer films produced, retention of analytes increased as the monomer concentration increased to a certain value, at which point the capacity factors level off with further increases in monomer concentration. The electroosmotic flow velocity decreases with increasing monomer concentration. The efficiency for an unretained test probe (acetone) reaches 270 000 plates/m. 13 refs., 10 figs., 1 tab.

  13. Boron doped Si rich oxide/SiO{sub 2} and silicon rich nitride/SiN{sub x} bilayers on molybdenum-fused silica substrates for vertically structured Si quantum dot solar cells

    Energy Technology Data Exchange (ETDEWEB)

    Lin, Ziyun, E-mail: z.lin@unsw.edu.au; Wu, Lingfeng; Jia, Xuguang; Zhang, Tian; Puthen-Veettil, Binesh; Yang, Terry Chien-Jen; Conibeer, Gavin; Perez-Wurfl, Ivan [School of Photovoltaic and Renewable Energy Engineering, University of New South Wales, Building H6, Tyree Energy Technologies Building, Kensington, New South Wales 2052 (Australia)

    2015-07-28

    Vertically structured Si quantum dots (QDs) solar cells with molybdenum (Mo) interlayer on quartz substrates would overcome current crowding effects found in mesa-structured cells. This study investigates the compatibility between boron (B) doped Si QDs bilayers and Mo-fused silica substrate. Both Si/SiO{sub 2} and Si/SiN{sub x} based QDs bilayers were studied. The material compatibility under high temperature treatment was assessed by examining Si crystallinity, microstress, thin film adhesion, and Mo oxidation. It was observed that the presence of Mo interlayer enhanced the Si QDs size confinement, crystalline fraction, and QDs size uniformity. The use of B doping was preferred compared to phosphine (PH{sub 3}) doping studied previously in terms of better surface and interface properties by reducing oxidized spots on the film. Though crack formation due to thermal mismatch after annealing remained, methods to overcome this problem were proposed in this paper. Schematic diagram to fabricate full vertical structured Si QDs solar cells was also suggested.

  14. Facile one-pot synthesis of a aptamer-based organic-silica hybrid monolithic capillary column by "thiol-ene" click chemistry for detection of enantiomers of chemotherapeutic anthracyclines.

    Science.gov (United States)

    Jiang, Han-Peng; Zhu, Jiu-Xia; Peng, Chunyan; Gao, Jiajia; Zheng, Fang; Xiao, Yu-Xiu; Feng, Yu-Qi; Yuan, Bi-Feng

    2014-10-07

    In the current study, we developed a facile strategy for the one-pot synthesis of an aptamer-based organic-silica hybrid monolithic capillary column. A 5'-SH-modified aptamer, specifically targeting doxorubicin, was covalently modified in the hybrid silica monolithic column by a sol-gel method combined with "thiol-ene" click reaction. The prepared monolithic column had good stability and permeability, large specific surface, and showed excellent selectivity towards chemotherapeutic anthracyclines of doxorubicin and epirubicin. In addition, the enantiomers of doxorubicin and epirubicin can be easily separated by aptamer-based affinity monolithic capillary liquid chromatography. Furthermore, doxorubicin and epirubicin spiked in serum and urine were also successfully determined, which suggested that the complex biological matrix had a negligible effect on the detection of doxorubicin and epirubicin. Finally, we quantified the concentration of epirubicin in the serum of breast cancer patients treated with epirubicin by intravenous injection. The developed analytical method is cost-effective and rapid, and biological samples can be directly analyzed without any tedious sample pretreatment, which is extremely useful for monitoring medicines in serum and urine for pharmacokinetic studies.

  15. Separation and Analysis of Organic Acids in Food by Capillary Silica Monolithic Column%毛细管硅胶整体柱分离分析食品中有机酸

    Institute of Scientific and Technical Information of China (English)

    高文惠; 杨桂君; 贾英民

    2012-01-01

    A capillary electrochromatographic method for the separation and analysis of organic acids in food was proposed using a capillary silica monolithic column.Optimization of experimental parameters that influence separation efficiency was carried out.A capillary silica monolithic C18 column was prepared in our lab for the separation of organic acids using a mobile phase(pH 5.2) consisting of 150 mmol/L sodium dihydrogen phosphate-60 mmol/L borax buffer solution with a final concentration of 5:2 in the mixture and 0.5 mmol/L cetyl trimethyl ammonium bromide.Other experimental conditions were as follows: voltage-6 kV;injection time 10 s;column temperature 25 ℃;and detection wavelength 200 nm.Results showed that the linear range was 10–1000 μg/mL for oxalic acid and fumaric acid,20–500 μg/mL for succinic acid,15–1000 μg/mL for tartaric acid and citric acid.The average recovery rates for the organic acids were between 89.8% and 101.1%,with a relative standard deviation(RSD) less than or equal to 6.23%(n = 5).The detection limits of the proposed methods were between 3.0 and 7.5 μg/mL.In conclusion,capillary silica monolithic column is inexpensive,stable to heat and organic solvents,and repeatedly usable.Capillary electrochromatography with capillary silica monolithic column allows simple,rapid and effective separation and analysis of organic acids in food.%建立应用毛细管硅胶整体柱采用毛细管电色谱法分离分析食品中有机酸的方法。对影响毛细管电色谱分离效率的条件进行优化,色谱柱为本实验室制作的毛细管硅胶整体C18柱(100μm×40cm)、电压-6kV、进样时间10s、紫外检测波长200nm,流动相为150mmol/L磷酸二氢钠-60mmol/L硼砂缓冲溶液(浓度比为5:2)和0.5mmol/L十六烷基三甲基溴化铵,pH7.5、25℃。结果表明:草酸和富马酸的线性范围为10~1000μg/mL,丁二酸线性范围20~500μg/mL,酒石酸和柠檬酸的线性范围为15~1000μg

  16. Surface crystallization of amorphous fused silica during electron cyclotron resonance plasma etching%非晶熔石英表面等离子体刻蚀过程中的表面晶化研究

    Institute of Scientific and Technical Information of China (English)

    王锋; 吴卫东; 蒋晓东; 唐永建

    2012-01-01

    本工作采用电子回旋共振(ECR)低压等离子体刻蚀技术,刻蚀非晶熔石英表面.Ar/CF_4为反应气体刻蚀后再经O等离子体钝化,非晶熔石英表面出现晶化现象.晶化层约几百纳米厚.Ar/CF_4在ECR的电磁场作用下产生F离子与C离子,F离子使熔石英表面的Si-O共价键断裂,并释放出O离子.C离了与O离子迅速键合生成CO_2,而被断键的Si原子与四个F原子键合生成气态SiF4.熔石英原始表面被去除的同时,在新的表面留下大量不饱和Si原子.不饱和Si原子在高温条件下被O等离子钝化,形成结晶态α方石英.%After low pressure fluorine plasma ecthing and oxygen ion passivation,a crystallized layer composed of SiO_2 nano-crystal grains is observed in an amorphous fused silica surface.The depth of crystallized layer is at least several hundreds nanometers.Fluorine and carbon ion are generated from Ar/CF_4 by the method of electron cyclotron resonance(ECR).F ion breaks Si-O band of initial silica surface layer and releases O ion.Carbon ion combines with oxygen ion,and turns into CO_2,and SiF_4 is generated from fluorine and silicon.After initial surface layer is removed,unsaturated Si atom remains.Si dangling bond recombines with new O ion and then creates crystallizedα-cristobalite nano-crystal grains under a high temperature.

  17. Determination of vanillin in vanilla perfumes and air by capillary electrophoresis.

    Science.gov (United States)

    Minematsu, Saaya; Xuan, Guang-Shan; Wu, Xing-Zheng

    2013-12-01

    The present study investigated capillary electrophoretic detection of vanillin in vanilla perfume and air. An UV-absorbance detector was used in a home-made capillary electrophoretic instrument. A fused silica capillary (outer diameter: 364 μm, inner diameter: 50 μm) was used as a separation capillary, and a high electric voltage (20 kV) was applied across the two ends of the capillary. Total length of the capillary was 70 cm, and the effective length was 55 cm. Experimental results showed that the vanillin peak was detected at about 600, 450, and 500 seconds when pH of running buffers in CE were 7.2, 9.3, and 11.5, respectively. The peak area of vanillin was proportional to its concentration in the range of 0-10(-2) mol/L. The detection limit was about 10(-5) mol/L. Vanillin concentration in a 1% vanilla perfume sample was determined to be about 3×10(-4) mol/L, agreed well with that obtained by a HPLC method. Furthermore, determination of vanillin in air by combination of CE and active carbon adsorption method was investigated. Copyright © 2013 The Research Centre for Eco-Environmental Sciences, Chinese Academy of Sciences. Published by Elsevier B.V. All rights reserved.

  18. 航天器舷窗玻璃超高速撞击损伤与M/OD撞击风险评估%Hypervelocity impact damage of fused silica glass and M/OD impact risk assessment of spacecraft windshield

    Institute of Scientific and Technical Information of China (English)

    庞贺伟; 龚自正; 张文兵; 杨继运; 童靖宇

    2007-01-01

    用北京卫星环境工程研究所的18mm口径二级轻气炮(TLGG)和20 J激光驱动微小飞片装置(LDFF-20)对用作航天器舷窗玻璃的熔融石英玻璃的超高速撞击损伤特性进行了实验研究和分析.其中,TLGG发射的球形铝弹丸直径分别为1 mm和3 mm,速度2~6.5 km/s;LDFF-20发射的圆柱形飞片厚度7 μm,直径1 mm,速度1~8.3 km/s.撞击结果为:对12 mm厚的熔融石英玻璃,直径为3mm的弹丸甚至在2.8 km/s的低速下就将其穿透,而直径为1 mm的弹丸在6.5km/s的高速下没有穿透,这说明弹丸直径对撞击损伤特性有很强的影响;LDFF-20发射的微小飞片的撞击仅在玻璃表面产生很浅的凹坑,没有裂纹产生,但微小飞片的累积撞击损伤明显地降低了玻璃的透光性.实验初步获得了侵彻深度PC、侵彻直径D1与弹丸撞击速度Vp、弹丸质量Mp之间的经验关系.依据实验结果和目前的微流星体/空间碎片(M/OD)环境工程模型,建议对于高度为400 km、轨道倾角42°、寿命为3年的典型航天器,其舷窗玻璃的临界安全(非穿透)厚度至少为12mm.%Hypervelocity impact experiments were conducted on fused silica glass to obtain the damage characteristics and to build a damage model using Ly12 aluminum spheres of diameters 1 mm and 3 mm launched by the two-stage-light-gas gun of up to 6.5 km/s, and the small aluminum flyer of 1 mm in diameter and 7 μm in thickness launched by a laser-driven flyer facility of up to 8.3 km/s, developed by Beijing Institute of Spacecraft Environment (BISEE). The empirical damage equations were obtained to approximately predict the penetration depth (PC) and its diameter (D1) as a function of impact parameters (projectile velocityVp, mass Mp). For the Ly12 A1 projectile of 3 mm diameter sphere, the glass was perforated thoroughly even at a low impact velocity of 2.80 km/s. This means that the projectile diameter plays a major role with respect to the impact damage. The damage

  19. 1.2W laser amplification at 1427nm on the 4Fsub>3/2sub> to 4Isub>13/2sub> spectral line in an Nd3+ doped fused silica optical fiber.

    Science.gov (United States)

    Dawson, Jay W; Pax, Paul H; Allen, Graham S; Drachenberg, Derrek R; Khitrov, Victor V; Schenkel, Nick; Messerly, Michael J

    2016-12-12

    A 9.3dB improvement in optical gain and a 100x improvement in total optical power over prior published experimental results from the 4Fsub>3/2sub> to 4Isub>13/2sub> transition in an Nd3+ doped fused silica optical fiber is demonstrated. This is enabled via an optical fiber waveguide design that creates high spectral attenuation in the 1050-1120nm-wavelength range, a continuous spectral filter for the primary 4Fsub>3/2sub> to 4Isub>11/2sub> optical transition. A maximum output power at 1427nm of 1.2W was attained for 43mW coupled seed laser power and 22.2W of coupled pump diode laser power at 880nm a net optical gain of 14.5dB. Reducing the coupled seed laser power to 2.5mW enabled the system to attain 19.3dB of gain for 16.5W of coupled pump power. Four issues limited results; non-optimal seed laser wavelength, amplified spontaneous emission on the 4Fsub>3/2sub> to 4Isub>9/2sub> optical transition, low absorption of pump light from the cladding and high spectral attenuation in the 1350-1450nm range. Future fibers that mitigate these issues should lead to significant improvements in the efficiency of the laser amplifier, though the shorter wavelength region of the transition from 1310nm to >1350nm is still expected to be limited by excited state absorption.

  20. Capillary Hemangioma

    Science.gov (United States)

    ... Frequently Asked Questions Español Condiciones Chinese Conditions Capillary Hemangioma En Español Read in Chinese What is a capillary hemangioma? A capillary hemangioma (“strawberry” birthmark) is a benign ( ...

  1. The Advanced Virgo monolithic fused silica suspension

    Energy Technology Data Exchange (ETDEWEB)

    Aisa, D.; Aisa, S.; Campeggi, C.; Colombini, M. [University of Perugia and INFN Perugia (Italy); Conte, A. [University of Roma Sapienza and INFN Roma (Italy); Farnesini, L. [University of Perugia and INFN Perugia (Italy); Majorana, E.; Mezzani, F. [University of Roma Sapienza and INFN Roma (Italy); Montani, M. [University of Urbino and INFN Firenze (Italy); Naticchioni, L.; Perciballi, M. [University of Roma Sapienza and INFN Roma (Italy); Piergiovanni, F. [University of Urbino and INFN Firenze (Italy); Piluso, A. [University of Perugia and INFN Perugia (Italy); Puppo, P., E-mail: paola.puppo@roma1.infn.it [University of Roma Sapienza and INFN Roma (Italy); Rapagnani, P. [University of Roma Sapienza and INFN Roma (Italy); Travasso, F. [University of Perugia and INFN Perugia (Italy); Vicerè, A. [University of Urbino and INFN Firenze (Italy); Vocca, H. [University of Perugia and INFN Perugia (Italy)

    2016-07-11

    The detection of gravitational waves is one of the most challenging prospects faced by experimental physicists. Suspension thermal noise is an important noise source at operating frequencies between approximately 10 and 30 Hz, and represents a limit to the sensitivity of the ground based interferometric gravitational wave detectors. Its effects can be reduced by minimizing the losses and by optimizing the geometry of the suspension fiber as well as its attachment system. In this proceeding we will describe the mirrors double stage monolithic suspension system to be used in the Advanced Virgo (AdV) detector. We also present the results of the thermal noise study, performed with the help of a finite elements model, taking into account the precise geometry of the fibers attachment systems on the suspension elements. We shall demonstrate the suitability of this suspension for installation in AdV. - Highlights: • Suspension system design for the test masses of the gravitational wave detectors. • Finite element model studies. • Suspension thermal noise studies.

  2. Preparation and evaluation of micro and meso porous silica monoliths with embedded carbon nanoparticles for the extraction of non-polar compounds from waters.

    Science.gov (United States)

    Fresco-Cala, Beatriz; Cárdenas, Soledad; Valcárcel, Miguel

    2016-10-14

    A novel hybrid micro and meso porous silica monolith with embedded carbon nanoparticles (Si-CNPs monolith) was prepared inside a fused silica capillary (3cm in length) and used as a sorbent for solid-phase microextraction. The hybrid monolithic capillary was synthetized by hydrolysis and polycondensation of a mixture of tetraethoxysilane (TEOS), ethanol, and three different carbon nanoparticles such as carboxylated single-walled carbon nanotubes (c-SWCNTs), carboxylated multi-walled carbon nanotubes (c-MWCNTs), and oxidized single-walled carbon nanohorns (o-SWNHs) via a two-step catalytic sol-gel process. Compared with silica monolith without carbon nanoparticles, the developed monolithic capillary column exhibited a higher extraction efficiency towards the analytes which can be ascribed to the presence of the carbon nanoparticles. In this regard, the best performance was achieved for silica monolith with embedded c-MWCNTs. The resulted monolithic capillaries were also characterized by scanning electron microscopy (SEM), elemental analysis and nitrogen intrusion porosimetry. Variables affecting to the preparation of the sorbent phase including three different carbon nanoparticles and extraction parameters were studied in depth using polycyclic aromatic hydrocarbons (PAHs) as target analytes. Gas chromatography-mass spectrometry was selected as instrumental technique. Detection limits range from 0.1 to 0.3μgL(-1), and the inter-extraction units precision (expressed as relative standard deviation) is between 5.9 and 14.4%.

  3. Study on the Interaction between Strychnine and Bovine Serum Albumin by Capillary Electrophoretic Frontal Analysis

    Institute of Scientific and Technical Information of China (English)

    2005-01-01

    The protein binding constant, binding sites of the Strychnos alkaloid-strychnine and bovine serum albumin (BSA) was determined by capillary electrophoretic frontal analysis (CE-FA)for the first time. The experiment was carried out in a polyacrylamide-coated fused silica capillary (48.4 cm×50 μm i.d., 38.1 cm effective length) with 20 mmol/L citrate/MES buffer (pH 6.0, ionic strength 0.17). The applied voltage was 12 kV and detection wavelength was set at 257nm. The plateau height of the peak was employed to determine the unbound concentration of drug in BSA equilibrated sample solution based on the external drug standard in the absence of protein. The present method provides a convenient, accurate technique for the early stage of drug screening.

  4. Chiral separation of benzothiazole derivatives of amino acids using capillary zone electrophoresis.

    Science.gov (United States)

    Nováková, Zuzana; Pejchal, Vladimír; Fischer, Jan; Česla, Petr

    2017-02-01

    A method for the separation of enantiomers of leucine and phenylalanine benzothiazole derivatives as potential antimicrobial agents was developed using capillary zone electrophoresis with a dual cyclodextrin (CD) system. The best resolution of enantiomers was achieved in 100 mmol/L phosphate background electrolyte (pH 3.5) with the dual CD system consisting of 10 mmol/L of β-CD with 10 mmol/L of 2-hydroxypropyl-β-cyclodextrin for leucine derivative and 10 mmol/L of 2-hydroxypropyl-γ-cyclodextrin for phenylalanine derivative, respectively. Under the optimal conditions, the highest enantioresolution of 1.25 was achieved in a noncoated-fused silica capillary at 17°C and 24 kV applied voltage.

  5. Effect of polyamines on the separation of ovalbumin glycoforms by capillary electrophoresis.

    Science.gov (United States)

    Legaz, M E; Pedrosa, M M

    1996-01-05

    The successful separation of ovalbumin (M(r) 45,000; pI 4.7) glycoforms by capillary electrophoresis in an uncoated fused-silica capillary with different buffer additives is reported. The optimum conditions for obtaining the resolution of glycoforms were 25 mM borate (pH 9.0) containing 0.87 mM spermidine or 0.14 mM spermine. The effects of different concentrations of putrescine, cadaverine, spermidine, spermine and some monoamines or diamines are compared in terms of selectivity factors of ovalbumin peaks. Addition of sodium dodecyl sulfate at a concentration below the critical micelle concentration increased the resolution between the three main peaks of ovalbumin but did not permit their microheterogeneity to be expressed.

  6. Pressure evolution during HBC fuse operation

    Energy Technology Data Exchange (ETDEWEB)

    Rochette, D; Bussiere, W [Laboratoire Arc Electrique et Plasmas Thermiques (LAEPT)-CNRS UMR 6069, Universite Blaise Pascal, 24 Avenue des Landais, F 63177 Aubiere Cedex (France)

    2004-05-01

    The purpose of this paper is to describe the influence of the silica sand grains on pressure during the energy release in a high breaking capacity (HBC) fuse. During the HBC fuse operation, the pressure evolution is the result of two opposite trends: the pressure increase due to the interaction of the silica plasma with the surrounding granular sand, and the pressure decrease due to the propagation of the pressure waves toward the porous medium. Due to the complex phenomena occurring during the current extinction by a fuse, two kinds of pressure are distinguished: the pressure inside the silica plasma and the pressure in the silica sand. From the simulations we show that the Forchheimer flow resistance is stronger than the Darcy flow resistance once the electric power is over 30% of the maximum value. A comparison of the calculated and measured pressures is made at various positions from the fuse element axis. Two different pressures are obtained experimentally: the pressure P{sub SAND} exerted on the sand grains due to the plasma pressure, and the pressure P{sub GAS} of the gas flowing through the interstices of the silica sand. We show that the experimental and calculated trends are similar and they both depend on the electric power level and the silica sand mean granulometry. The maximum pressures are observed at the same time as the maximum electric power levels. The ratio P{sub SAND}/P{sub GAS} is about 8 with P{sub GAS} values not exceeding 1.5 x 10{sup 5} Pa.

  7. Fabrication of High Performance Microlenses for an Integrated Capillary Channel Electrochromatograph with Fluorescence Detection

    Energy Technology Data Exchange (ETDEWEB)

    Wendt, J.R.; Warren, M.E.; Sweatt, W.C.; Bailey, C.G.; Matzke, C.M.; Arnold, D.W.; Allerman, A.A.; Carter, T.R.; Asbill, R.E.; Samora, S.

    1999-07-07

    We describe the microfabrication of an extremely compact optical system as a key element in an integrated capillary channel electrochromatograph with fluorescence detection. The optical system consists of a vertical cavity surface-emitting laser (VCSEL), two high performance microlenses and a commercial photodetector. The microlenses are multilevel diffractive optics patterned by electron beam lithography and etched by reactive ion etching in fused silica. The design uses substrate-mode propagation within the fused silica substrate. Two generations of optical subsystems are described. The first generation design has a 6 mm optical length and is integrated directly onto the capillary channel-containing substrate. The second generation design separates the optical system onto its own substrate module and the optical path length is further compressed to 3.5 mm. The first generation design has been tested using direct fluorescence detection with a 750 nm VCSEL pumping a 10{sup {minus}4}M solution of CY-7 dye. The observed signal-to-noise ratio of better than 100:1 demonstrates that the background signal from scattered pump light is low despite the compact size of the optical system and is adequate for system sensitivity requirements.

  8. Semipermanent capillary coatings in mixed organic-water solvents for CE.

    Science.gov (United States)

    Diress, Abebaw G; Yassine, Mahmoud M; Lucy, Charles A

    2007-04-01

    This report describes the creation of semipermanent capillary coatings that are compatible with organic-water solvent systems in CE. The coatings are created by simply rinsing the fused-silica capillary with long double-chain cationic surfactants, such as dimethyl-ditetradecyl ammonium bromide (2C(14)DAB), dihexadecyldimethyl ammonium bromide (2C(16)DAB), and dimethyldioctadecyl ammonium bromide (2C(18)DAB). These surfactants generate semipermanent bilayer coatings on the capillary surface, which display a high degree of stability in buffers containing up to 60% v/v of organic solvents, such as methanol and ACN. The coating stability increases with increasing hydrophobicity of the surfactant, i.e., with increasing chain length. For instance, the EOF changes by only 1.2% in a 2C(18)DAB-coated capillary after 130 capillary volumes of rinsing with 60% v/v methanol containing buffer. The bilayer coatings allow separations to be performed without the need to regenerate the coating between runs or to maintain the EOF modifier in the run buffer. Rapid separations (organic solvent content is adjusted.

  9. Hybrid phospholipid bilayer coatings for separations of cationic proteins in capillary zone electrophoresis.

    Science.gov (United States)

    Gallagher, Elyssia S; Adem, Seid M; Bright, Leonard K; Calderon, Isen A C; Mansfield, Elisabeth; Aspinwall, Craig A

    2014-04-01

    Protein separations in CZE suffer from nonspecific adsorption of analytes to the capillary surface. Semipermanent phospholipid bilayers have been used to minimize adsorption, but must be regenerated regularly to ensure reproducibility. We investigated the formation, characterization, and use of hybrid phospholipid bilayers (HPBs) as more stable biosurfactant capillary coatings for CZE protein separations. HPBs are formed by covalently modifying a support with a hydrophobic monolayer onto which a self-assembled lipid monolayer is deposited. Monolayers prepared in capillaries using 3-cyanopropyldimethylchlorosilane (CPDCS) or n-octyldimethylchlorosilane (ODCS) yielded hydrophobic surfaces with lowered surface free energies of 6.0 ± 0.3 or 0.2 ± 0.1 mJ m(-2) , respectively, compared to 17 ± 1 mJ m(-2) for bare silica capillaries. HPBs were formed by subsequently fusing vesicles comprised of 1,2-dilauroyl-sn-glycero-3-phosphocholine or 1,2-dioleoyl-sn-glycero-3-phosphocholine to CPDCS- or ODCS-modified capillaries. The resultant HPB coatings shielded the capillary surface and yielded reduced electroosmotic mobility (1.3-1.9 × 10(-4) cm(2) V(-1) s(-1) ) compared to CPDCS- and ODCS-modified or bare capillaries (3.6 ± 0.2 × 10(-4) cm(2) V(-1) s(-1) , 4.8 ± 0.4 × 10(-4) cm(2) V(-1) s(-1) , and 6.0 ± 0.2 × 10(-4) cm(2) V(-1) s(-1) , respectively), with increased stability compared to phospholipid bilayer coatings. HPB-coated capillaries yielded reproducible protein migration times (RSD ≤ 3.6%, n ≥ 6) with separation efficiencies as high as 200 000 plates/m.

  10. Attempt to run urinary protein electrophoresis using capillary technique.

    Science.gov (United States)

    Falcone, Michele

    2014-10-01

    The study of urinary protein has a predominant place in the diagnosis of kidney disease. The most common technique is agarose gel electrophoresis (AGE). For several years, the technique of choice applied to the analysis of serum proteins has been CE, a system that uses capillary fused silica, subjected to high voltage to separate and measure serum proteins. The purpose of this paper was to perform capillary electrophoresis on urinary proteins which, at present, are not interpretable due to the many nonspecific peaks visible when using gel electrophoresis. In order to carry out our research, we used a capillary V8 analyzer together with an agarose gel system from the same company. AGE was taken as the reference method, for which urine was used without any pretreatment. For the V8 system, urine was subjected to purification on granular-activated carbon and then inserted into the V8 analyzer, selecting a program suitable for liquids with low protein content. We examined 19 urine samples collected over 24 hrs from both hospitalized and external patients with different types of proteinuria plus a serum diluted 1/61 considered as a control to recognize the bands. Both methods showed the same protein fractions and classified the proteinuria in a similar way.

  11. Analysis of roller pen inks by capillary zone electrophoresis

    Institute of Scientific and Technical Information of China (English)

    ZHAO Pengcheng; WANG Yanji; XU Yuanyuan; YAO Lijuan

    2007-01-01

    The analysis of roller pen inks has become more and more important in fraudulent document examination because of the extensive use of roller pens in financial documents.Capillary electrophoresis with powerful resolution was applied for the analysis of roller pen inks.The experiment focused on the optimization of the separation of the extract from commercially available roller pen entries.A better separation electropherogram was obtained when a 20 mM borate buffer at pH 8.5 and a fused silica capillary with an inner diameter of 100 μm with a total length of 47 (40 cm to the detector window)were used.Five inks from roller pens of different manufacturers and countries were analyzed,and their electropherograms showed that most patterns are distinctly different from each other.Capillary with inner diameter of 100 μm increased the intensity of determination;therefore,color dyes were identified in the visible range and were able to provide more information for comparing types of roller pen inks.

  12. Intrinsic advantages of packed capillaries over narrow-bore columns in very high-pressure gradient liquid chromatography.

    Science.gov (United States)

    Gritti, Fabrice; McDonald, Thomas; Gilar, Martin

    2016-06-17

    250μm×100mm fused silica glass capillaries were packed with 1.8μm high-strength silica (HSS) fully porous particles. They were prepared without bulky stainless steel endfittings and metal frits, which both generate significant sample dispersion. The isocratic efficiencies and gradient peak capacities of these prototype capillary columns were measured for small molecules (n-alkanophenones) using a home-made ultra-low dispersive micro-HPLC instrument. Their resolution power was compared to that of standard 2.1mm×100mm very high-pressure liquid chromatography (vHPLC) narrow-bore columns packed with the same particles. The results show that, for the same column efficiency (25000 plates) and gradient steepness (0.04min(-1)), the peak capacity of the 250μm i.d. capillary columns is systematically 15-20% higher than that of the 2.1mm i.d. narrow-bore columns. A validated model of gradient chromatography enabled one to predict accurately the observed peak capacities of the capillary columns for non-linear solvation strength retention behavior and under isothermal conditions. Thermodynamics applied to the eluent quantified the temperature difference for the thermal gradients in both capillary and narrow-bore columns. Experimental data revealed that the gradient peak capacity is more affected by viscous heating than the column efficiency. Unlike across 2.1mm i.d. columns, the changes in eluent composition across the 250μm i.d. columns during the gradient is rapidly relaxed by transverse dispersion. The combination of (1) the absence of viscous heating and (2) the high uniformity of the eluent composition across the diameter of capillary columns explains the intrinsic advantage of capillary over narrow-bore columns in gradient vHPLC.

  13. Screening for urinary amphetamine and analogs by capillary electrophoretic immunoassays and confirmation by capillary electrophoresis with on-column multiwavelength absorbance detection.

    Science.gov (United States)

    Ramseier, A; Caslavska, J; Thormann, W

    1998-11-01

    This paper characterizes competitive binding, electrokinetic capillary-based immunoassays for screening of urinary amphetamine (A) and analogs using reagents which were commercialized for a fluorescence polarization immunoassay (FPIA). After incubation of 25 microL urine with the reactants, a small aliquot of the mixture is applied onto a fused-silica capillary and unbound fluorescein-labeled tracer compounds are monitored by capillary electrophoresis with on-column laser-induced fluorescence detection. Configurations in presence and absence of micelles were investigated and found to be capable of recognizing urinary D-(+)-amphetamine at concentrations > about 80 ng/mL. Similar responses were obtained for racemic methamphetamine (MA) and 3,4-methylenedioxymethamphetamine (MDMA). The electrokinetic immunoassay data suggest that the FPIA reagent kit includes two immunoassay systems (two antibodies and two tracer molecules), one that recognizes MA and MDMA, and one that is geared towards monitoring of A. For confirmation analysis of urinary amphetamines and ephedrines, capillary electrophoresis in a pH 9.2 buffer and multiwavelength UV detection was employed. The suitability of the electrokinetic methods for screening and confirmation is demonstrated via analysis of patient and external quality control urines.

  14. Separation of selected peptides by capillary electroendoosmotic chromatography using 3 microns reversed-phase bonded silica and mixed-mode phases.

    Science.gov (United States)

    Walhagen, K; Unger, K K; Olsson, A M; Hearn, M T

    1999-08-20

    The retention behaviour and selectivity of selected basic, neutral and acidic peptides have been studied by capillary electroendoosmotic chromatography (CEC) with Hypersil C8, C18, Hypersil mixed-mode, and Spherisorb C18/SCX columns, 250 (335) mm x 100 microns, packed with 3 microns particles, and eluted with mobile phases composed of acetonitrile-triethylamine-phosphoric acid (TEAP) at pH 3.0 using a Hewlett-Packard Model HP3DCE capillary electrophoresis system. The selected peptides were desmopressin (D), two analogues (A and B) of desmopressin, oxytocin (O) and carbetocin (C). The peptides eluted either before or after the electroendoosmotic flow (EOF) marker, depending on the concentration of acetonitrile used and the buffer ionic strength. The retention and selectivity of these peptides under CEC conditions were compared to their behaviour in free zone capillary electrophoresis (CZE), where the separation mode was based on the electrophoretic migration of the analytes due to their charge and Stokes radius properties. In addition, their retention behaviour in RP-HPLC was also examined. As a result, it can be concluded that the elution process of this group of synthetic peptides in CEC with a TEAP buffer at pH 3.0 is mediated by a combination of both electrophoretic migration processes and retention mechanisms involving hydrophobic as well as silanophilic interactions. This CEC method when operated with these 3 microns reversed-phase and mixed-mode sorbents with peptides is thus a hybrid of two well-known analytical methods, namely CZE and RP-HPLC. However, the retention behaviour and selectivity of the selected peptides differs significantly in the CEC mode compared to the RP-HPLC or CZE modes. Therefore this CEC method with these peptides represents an orthogonal analytical separation procedure that is complimentary to both of these alternative techniques.

  15. Capillary sample

    Science.gov (United States)

    ... several times a day using capillary blood sampling. Disadvantages to capillary blood sampling include: Only a limited ... do not constitute endorsements of those other sites. Copyright 1997-2017, A.D.A.M., Inc. Duplication ...

  16. Simultaneous detection of genetically modified organisms by multiplex ligation-dependent genome amplification and capillary gel electrophoresis with laser-induced fluorescence.

    Science.gov (United States)

    García-Cañas, Virginia; Mondello, Monica; Cifuentes, Alejandro

    2010-07-01

    In this work, an innovative method useful to simultaneously analyze multiple genetically modified organisms is described. The developed method consists in the combination of multiplex ligation-dependent genome dependent amplification (MLGA) with CGE and LIF detection using bare-fused silica capillaries. The MLGA process is based on oligonucleotide constructs, formed by a universal sequence (vector) and long specific oligonucleotides (selectors) that facilitate the circularization of specific DNA target regions. Subsequently, the circularized target sequences are simultaneously amplified with the same couple of primers and analyzed by CGE-LIF using a bare-fused silica capillary and a run electrolyte containing 2-hydroxyethyl cellulose acting as both sieving matrix and dynamic capillary coating. CGE-LIF is shown to be very useful and informative for optimizing MLGA parameters such as annealing temperature, number of ligation cycles, and selector probes concentration. We demonstrate the specificity of the method in detecting the presence of transgenic DNA in certified reference and raw commercial samples. The method developed is sensitive and allows the simultaneous detection in a single run of percentages of transgenic maize as low as 1% of GA21, 1% of MON863, and 1% of MON810 in maize samples with signal-to-noise ratios for the corresponding DNA peaks of 15, 12, and 26, respectively. These results demonstrate, to our knowledge for the first time, the great possibilities of MLGA techniques for genetically modified organisms analysis.

  17. DNA Sequencing Using capillary Electrophoresis

    Energy Technology Data Exchange (ETDEWEB)

    Dr. Barry Karger

    2011-05-09

    The overall goal of this program was to develop capillary electrophoresis as the tool to be used to sequence for the first time the Human Genome. Our program was part of the Human Genome Project. In this work, we were highly successful and the replaceable polymer we developed, linear polyacrylamide, was used by the DOE sequencing lab in California to sequence a significant portion of the human genome using the MegaBase multiple capillary array electrophoresis instrument. In this final report, we summarize our efforts and success. We began our work by separating by capillary electrophoresis double strand oligonucleotides using cross-linked polyacrylamide gels in fused silica capillaries. This work showed the potential of the methodology. However, preparation of such cross-linked gel capillaries was difficult with poor reproducibility, and even more important, the columns were not very stable. We improved stability by using non-cross linked linear polyacrylamide. Here, the entangled linear chains could move when osmotic pressure (e.g. sample injection) was imposed on the polymer matrix. This relaxation of the polymer dissipated the stress in the column. Our next advance was to use significantly lower concentrations of the linear polyacrylamide that the polymer could be automatically blown out after each run and replaced with fresh linear polymer solution. In this way, a new column was available for each analytical run. Finally, while testing many linear polymers, we selected linear polyacrylamide as the best matrix as it was the most hydrophilic polymer available. Under our DOE program, we demonstrated initially the success of the linear polyacrylamide to separate double strand DNA. We note that the method is used even today to assay purity of double stranded DNA fragments. Our focus, of course, was on the separation of single stranded DNA for sequencing purposes. In one paper, we demonstrated the success of our approach in sequencing up to 500 bases. Other

  18. Simultaneous determination of berberine,matrine and oxymatrine in traditional Chinese medicines by using nonaqueous capillary electrophoresis

    Institute of Scientific and Technical Information of China (English)

    2010-01-01

    A rapid method for the simultaneous determination of berberine(BBR),matrine(MT)and oxymatrine(OMT)by nonaqueous capillary electrophoresis(NACE)was developed.Optimum separation of the analytes was obtained on a 50cm×50μm i.d.fused-silica capillary using a non-aqueous buffer system of 70mM ammonium acetate,7.0% acetic acid and 10% acetonitrile at 25kV and 20℃.The relative standard deviations(R.S.D.)of the migration times and peak areas of the three active components were 0.06%-0.20% and 0.12%-3.41% for berber...

  19. Measuring circular dichroism in a capillary cell using the b23 synchrotron radiation CD beamline at diamond light source.

    Science.gov (United States)

    Jávorfi, Tamás; Hussain, Rohanah; Myatt, Daniel; Siligardi, Giuliano

    2010-01-01

    Synchrotron radiation circular dichroism (SRCD) is a well-established method in structural biology. The first UV-VIS beamline dedicated to circular dichroism at Diamond Light Source, a third generation synchrotron facility in South Oxfordshire, has recently become operational and it is now available for the user community. Herein we present an important application of SRCD: the CD measurement of protein solutions in fused silica rectangular capillary cells. This was achieved without the use of any lens between the photoelastic modulator and the photomultiplier tube detectors by exploiting the high photon flux of the collimated beam that can be as little as half a millimeter squared. Measures to minimize or eliminate vacuum-UV protein denaturation effects are discussed. The CD spectra measured in capillaries is a proof of principle to address CD measurements in microdevice systems using the new B23 SRCD beamline.

  20. Improving sensitivity in simultaneous determination of copper carboxylates by nonaqueous capillary electrophoresis.

    Science.gov (United States)

    Laamanen, Pirkko-Leena; Blanco, Eva; Cela, Rafael; Matilainen, Rose

    2006-03-31

    A new method of nonaqueous capillary electrophoresis (NACE) with UV spectrophotometric detection was developed and optimized for the simultaneous determination of seven carboxylates (trans-1,2-diaminocyclohexane-N,N,N',N'-tetraacetic acid (CDTA), diethylenetriaminepentaacetic acid (DTPA), ethylenediaminetetraacetic acid (EDTA), N-(2-hydroxyethyl)ethylenediamine-N,N',N'-triacetic acid (HEDTA), nitrilotriacetic acid (NTA), 1,3-diaminopropane-N,N,N',N'-tetraacetic acid (PDTA) and triethylenetetraaminehexaacetic acid (TTHA)) as copper complexes. The method development was carried out by using a fused silica capillary. Background electrolyte (BGE) was optimized and the best separation achieved by using 30mmolL(-1) potassium bromide in N-methylformamide (NMF) at apparent pH (pH(app)) 10.2. A voltage of +30kV and direct UV detection at 280nm were used in all measurements. Large-volume sample stacking using the electroosmotic flow pump (LVSEP) was tested in addition to basic capillary electrophoresis (CE) and observed to improve the separation of the analyte zones in the capillary. All the peaks in the electropherograms were properly separated, the calibration plots gave excellent correlation coefficients (R(2)>or=0.994) and all seven copper carboxylate complexes were detected in less than 20min using both the basic measurements and the large-volume sample stacking method. The new NACE method was tested with lake water and proved to be reliable.

  1. Highly efficient capillary columns packed with superficially porous particles via sequential column packing.

    Science.gov (United States)

    Treadway, James W; Wyndham, Kevin D; Jorgenson, James W

    2015-11-27

    Highly efficient capillary columns packed with superficially porous particles were created for use in ultrahigh pressure liquid chromatography. Superficially porous particles around 1.5μm in diameter were packed into fused silica capillary columns with 30, 50, and 75μm internal diameters. To create the columns, several capillary columns were serially packed from the same slurry, with packing progress plots being generated to follow the packing of each column. Characterization of these columns using hydroquinone yielded calculated minimum reduced plate heights as low as 1.24 for the most efficient 30μm internal diameter column, corresponding to over 500,000plates/m. At least one highly efficient column (minimum reduced plate height less than 2) was created for all three of the investigated column inner diameters, with the smallest diameter columns having the highest efficiency. This study proves that highly efficient capillary columns can be created using superficially porous particles and shows the efficiency potential of these particles.

  2. Polydopamine assisted fabrication of titanium oxide nanoparticles modified column for proteins separation by capillary electrochromatography.

    Science.gov (United States)

    Zhang, Yamin; Wang, Wentao; Ma, Xiangdong; Jia, Li

    2016-11-01

    Development of a simple method for preparation of stable open tubular (OT) columns for proteins separation by capillary electrochromatography is still challenging. In this work, the titanium oxide (TiO2) nanoparticles coated OT column was successfully prepared for separation of proteins by capillary electrochromatography. The polydopamine (PDA) film was first formed in the inner surface of a fused-silica capillary by the self-polymerization of dopamine under alkaline conditions. Then the TiO2 coating was deposited onto the surface of pre-modified capillary with PDA by a liquid phase deposition process. The plentifully active hydroxyl groups in PDA coating can chelate with Ti(4+) to boost the nucleation and growth of TiO2 film. The as-prepared TiO2 coated OT column was characterized by scanning electron microscopy and measurement of electroosmotic flow. Furthermore, the influence of liquid phase deposition time on the TiO2 coating was investigated. The TiO2 coated OT column was used for successful separation of two variants of β-lactoglobulin and eight glycoisoforms of ovalbumin. The column demonstrated good repeatability and stability. The relative standard deviations of migration times of proteins representing run-to-run, day-to-day, and column-to-column were less than 3.7%. Moreover, the application of the column was verified by successful separation of acidic proteins in egg white. Copyright © 2016 Elsevier Inc. All rights reserved.

  3. Separation and determination of basic dyes formulated in hair care products by capillary electrophoresis.

    Science.gov (United States)

    Masukawa, Yoshinori

    2006-03-03

    A capillary electrophoretic (CE) method for analyzing five basic dyes (Basic Red 76, Basic Brown 16, Basic Yellow 57, Basic Brown 17 and Basic Blue 99) sold under the trade name Arianor, which are commonly used in hair care products, has been established. A buffer of 100 mM acetic acid-ammonium acetate (50:50) containing 90% (v/v) methanol was employed in a fused-silica capillary of 40.0 cm x 50 microm I.D. with a bubble cell arrangement. Washing the capillary end immediately after injection was effective in preventing peak tailing of the basic dyes, which was due to their adsorption onto the outer wall of the capillary during the injection. Under these optimized conditions, acceptable results for reproducibility, limit of detection and quantitation, and linearity were obtained for the five authentic dyes tested. The recoveries of five authentic basic dyes spiked to three commercial hair care products also provided with acceptable results. This optimized CE method is useful for the analysis of mixed basic dyes in hair care products.

  4. Capillary Condensation, Freezing, and Melting in Silica Nanopores: A Sorption Isotherm and Scanning Calorimetry Study on Nitrogen in Mesoporous SBA-15

    CERN Document Server

    Moerz, Sebastian T; Huber, Patrick; 10.1103/PhysRevB.85.075403

    2012-01-01

    Condensation, melting and freezing of nitrogen in a powder of mesoporous silica grains (SBA-15) has been studied by combined volumetric sorption isotherm and scanning calorimetry measurements. Within the mean field model of Saam and Cole for vapor condensation in cylindrical pores a liquid nitrogen sorption isotherm is well described by a bimodal pore radius distribution. It encompasses a narrow peak centered at 3.3 nm, typical of tubular mesopores, and a significantly broader peak characteristic of micropores, located at 1 nm. The material condensed in the micropores as well as the first two adsorbed monolayers in the mesopores do not exhibit any caloric anomaly. The solidification and melting transformation affects only the pore condensate beyond approx. the second monolayer of the mesopores. Here, interfacial melting leads to a single peak in the specific heat measurements. Homogeneous and heterogeneous freezing along with a delayering transition for partial fillings of the mesopores result in a caloric fr...

  5. Capillary rise of water in hydrophilic nanopores

    CERN Document Server

    Gruener, Simon; Wallacher, Dirk; Kityk, Andriy V; Huber, Patrick; 10.1103/PhysRevE.79.067301

    2009-01-01

    We report on the capillary rise of water in three-dimensional networks of hydrophilic silica pores with 3.5nm and 5nm mean radii, respectively (porous Vycor monoliths). We find classical square root of time Lucas-Washburn laws for the imbibition dynamics over the entire capillary rise times of up to 16h investigated. Provided we assume two preadsorbed strongly bound layers of water molecules resting at the silica walls, which corresponds to a negative velocity slip length of -0.5nm for water flow in silica nanopores, we can describe the filling process by a retained fluidity and capillarity of water in the pore center. This anticipated partitioning in two dynamic components reflects the structural-thermodynamic partitioning in strongly silica bound water layers and capillary condensed water in the pore center which is documented by sorption isotherm measurements.

  6. High Throughput Sample Preparation and Analysis for DNA Sequencing, PCR and Combinatorial Screening of Catalysis Based on Capillary Array Technique

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Yonghua [Iowa State Univ., Ames, IA (United States)

    2000-01-01

    Sample preparation has been one of the major bottlenecks for many high throughput analyses. The purpose of this research was to develop new sample preparation and integration approach for DNA sequencing, PCR based DNA analysis and combinatorial screening of homogeneous catalysis based on multiplexed capillary electrophoresis with laser induced fluorescence or imaging UV absorption detection. The author first introduced a method to integrate the front-end tasks to DNA capillary-array sequencers. protocols for directly sequencing the plasmids from a single bacterial colony in fused-silica capillaries were developed. After the colony was picked, lysis was accomplished in situ in the plastic sample tube using either a thermocycler or heating block. Upon heating, the plasmids were released while chromsomal DNA and membrane proteins were denatured and precipitated to the bottom of the tube. After adding enzyme and Sanger reagents, the resulting solution was aspirated into the reaction capillaries by a syringe pump, and cycle sequencing was initiated. No deleterious effect upon the reaction efficiency, the on-line purification system, or the capillary electrophoresis separation was observed, even though the crude lysate was used as the template. Multiplexed on-line DNA sequencing data from 8 parallel channels allowed base calling up to 620 bp with an accuracy of 98%. The entire system can be automatically regenerated for repeated operation. For PCR based DNA analysis, they demonstrated that capillary electrophoresis with UV detection can be used for DNA analysis starting from clinical sample without purification. After PCR reaction using cheek cell, blood or HIV-1 gag DNA, the reaction mixtures was injected into the capillary either on-line or off-line by base stacking. The protocol was also applied to capillary array electrophoresis. The use of cheaper detection, and the elimination of purification of DNA sample before or after PCR reaction, will make this approach an

  7. High Throughput Sample Preparation and Analysis for DNA Sequencing, PCR and Combinatorial Screening of Catalysis Based on Capillary Array Technique

    Energy Technology Data Exchange (ETDEWEB)

    Yonghua Zhang

    2002-05-27

    Sample preparation has been one of the major bottlenecks for many high throughput analyses. The purpose of this research was to develop new sample preparation and integration approach for DNA sequencing, PCR based DNA analysis and combinatorial screening of homogeneous catalysis based on multiplexed capillary electrophoresis with laser induced fluorescence or imaging UV absorption detection. The author first introduced a method to integrate the front-end tasks to DNA capillary-array sequencers. protocols for directly sequencing the plasmids from a single bacterial colony in fused-silica capillaries were developed. After the colony was picked, lysis was accomplished in situ in the plastic sample tube using either a thermocycler or heating block. Upon heating, the plasmids were released while chromsomal DNA and membrane proteins were denatured and precipitated to the bottom of the tube. After adding enzyme and Sanger reagents, the resulting solution was aspirated into the reaction capillaries by a syringe pump, and cycle sequencing was initiated. No deleterious effect upon the reaction efficiency, the on-line purification system, or the capillary electrophoresis separation was observed, even though the crude lysate was used as the template. Multiplexed on-line DNA sequencing data from 8 parallel channels allowed base calling up to 620 bp with an accuracy of 98%. The entire system can be automatically regenerated for repeated operation. For PCR based DNA analysis, they demonstrated that capillary electrophoresis with UV detection can be used for DNA analysis starting from clinical sample without purification. After PCR reaction using cheek cell, blood or HIV-1 gag DNA, the reaction mixtures was injected into the capillary either on-line or off-line by base stacking. The protocol was also applied to capillary array electrophoresis. The use of cheaper detection, and the elimination of purification of DNA sample before or after PCR reaction, will make this approach an

  8. Solvent-resistant sol-gel polydimethyldiphenylsiloxane coating for on-line hyphenation of capillary microextraction with high-performance liquid chromatography.

    Science.gov (United States)

    Segro, Scott S; Malik, Abdul

    2008-09-26

    A sol-gel polydimethyldiphenylsiloxane (PDMDPS) coating was developed for capillary microextraction on-line hyphenated with high-performance liquid chromatography (HPLC). This coating was created using methyltrimethoxysilane (MTMS) as the sol-gel precursor and di-hydroxy-terminated PDMDPS as the sol-gel active polymer. The methyl and phenyl groups on the sol-gel active polymer and the methyl groups on the sol-gel precursor ultimately turned into pendant groups providing the ability to extract non-polar analytes. A 40-cm segment of 0.25 mm I.D. fused silica capillary containing the sol-gel PDMDPS coating was installed as an external sampling loop in an HPLC injection port. Aqueous samples containing polycyclic aromatic hydrocarbons (PAHs), aromatic compounds, ketones, and aldehydes were passed through this capillary wherein the analytes were extracted by the sol-gel coating. The extracted analytes were then transferred to the HPLC column using isocratic or gradient elution with an acetonitrile/water mobile phase. This capillary demonstrated excellent extraction capability for non-polar (e.g., polycyclic aromatic hydrocarbons and aromatic compounds) as well as moderately polar compounds, such as aromatic amines, ketones, and aldehydes. The test results indicate that PDMDPS can be successfully immobilized into a sol-gel network and that the resulting solvent-resistant sol-gel organic-inorganic hybrid coating can be effectively used for on-line hyphenation of capillary microextraction with high-performance liquid chromatography. The test results also indicate that the sol-gel PDMDPS coated capillary is resistant to high-temperature solvents, making it suitable for applications in high-temperature HPLC. To the best of our knowledge, this is the first report on the creation of a silica-based sol-gel PDMDPS coating used in capillary microextraction on-line hyphenated to HPLC.

  9. Capillary condensation, freezing, and melting in silica nanopores: A sorption isotherm and scanning calorimetry study on nitrogen in mesoporous SBA-15

    Science.gov (United States)

    Moerz, Sebastian T.; Knorr, Klaus; Huber, Patrick

    2012-02-01

    Condensation, melting, and freezing of nitrogen in a powder of mesoporous silica grains (SBA-15) has been studied by combined volumetric sorption isotherm and scanning calorimetry measurements. Within the mean-field model of Saam and Cole for vapor condensation in cylindrical pores, a liquid nitrogen sorption isotherm is well described by a bimodal pore radius distribution. It encompasses a narrow peak centered at 3.3 nm, typical of tubular mesopores, and a significantly broader peak characteristic of micropores, located at 1 nm. The material condensed in the micropores as well as the first two adsorbed monolayers in the mesopores do not exhibit any caloric anomaly. The solidification and melting transformation affects only the pore condensate beyond approximately the second monolayer of the mesopores. Here, interfacial melting leads to a single peak in the specific-heat measurements. Homogeneous and heterogeneous freezing along with a delayering transition for partial fillings of the mesopores result in a caloric freezing anomaly similarly complex and dependent on the thermal history to that observed for argon in SBA-15. The axial propagation of the crystallization in pore space is more effective in the case of nitrogen than previously observed for argon, which we attribute to differences in the crystalline textures of the pore solids.

  10. Determination of acidity constants of enolisable compounds by capillary electrophoresis.

    Science.gov (United States)

    Mofaddel, N; Bar, N; Villemin, D; Desbène, P L

    2004-10-01

    Research on the structure-activity relationships of molecules with acidic carbon atoms led us to undertake a feasibility study on the determination of their acidity constants by capillary electrophoresis (CE). The studied molecules had diverse structures and were tetronic acid, acetylacetone, diethylmalonate, Meldrum's acid, 3-methylrhodanine, nitroacetic acid ethyl ester, pyrimidine-2,4,6-trione, 3-oxo-3-phenylpropionic acid ethyl ester, 1-phenylbutan-1,3-dione, 5,5-dimethylcyclohexan-1,3-dione and homophthalic anhydride. The p Ka range explored by CE was therefore very large (from 3 to 12) and p Ka values near 12 were evaluated by mathematical extrapolations. The analyses were carried out in CZE mode using a fused silica capillary grafted (or not) with hexadimethrine. Owing to the electrophoretic behaviour of these compounds according to the pH, their acidity constants could be evaluated and appeared in perfect agreement with the literature data obtained, a few decades ago, by means of potentiometry, spectrometry or conductimetry. The p Ka of homophthalic anhydride and 3-methylrhodanine were evaluated for the first time.

  11. Monolithic molecularly imprinted polymeric capillary columns for isolation of aflatoxins.

    Science.gov (United States)

    Szumski, Michał; Grzywiński, Damian; Prus, Wojciech; Buszewski, Bogusław

    2014-10-17

    Monolithic molecularly imprinted polymers extraction columns have been prepared in fused-silica capillaries by UV or thermal polymerization in a two-step process. First, a poly-(trimethylolpropane trimethacrylate) (polyTRIM) core monolith was synthesized either by UV or thermal polymerization. Then it was grafted with the mixture of methacrylic acid (MAA) as a functional monomer, ethylene dimethacrylate (EDMA) as a cross-linking agent, 5,7-dimethoxycoumarin (DMC) as an aflatoxin-mimicking template, toluene as a porogen solvent and 2,2-azobis-(2-methylpropionitrile) (AIBN) as an initiator of the polymerization reaction. Different thermal condition of the photografting and different concentrations of the grafting mixture were tested during polymerization. The extraction capillary columns were evaluated in the terms of their hydrodynamic and chromatographic properties. Retention coefficients for aflatoxin B1 and DMC were used for assessment of the selectivity and imprinting factor. The obtained results indicate that the temperature of photografting and concentration of the grafting mixture are key parameters that determine the quality of the prepared MIPs. From the MIP columns characterized by the highest permeability the column of the highest imprinting factor was applied for isolation of aflatoxins B1, B2, G1 and G2 from the model aqueous sample followed by on-line chromatographic separation. The process was performed using a micro-MISPE-microLC-LIF system of a novel design, which allowed for detection of the eluates from the sample preparation part as well as from the chromatographic separation.

  12. Study of the electroosmotic flow as a means to propel the mobile phase in capillary electrochromatography in view of further miniaturization of capillary electrochromatography systems.

    Science.gov (United States)

    Szekely, Laszlo; Freitag, Ruth

    2005-05-01

    In this paper, we investigate the phenomenon of electroosmosis as a means to propel a mobile phase, in particular in view of an application in microfluidic systems, which are characterized by significantly smaller volumes of the reservoirs and the separation channels compared to conventional instrumentation. In the microfluidic chip, pH changes due to water electrolysis quickly showed an effect on the electroosmotic flow (EOF), which could be counteracted by either regularly exchanging or buffering the mobile phase. Surface treatment was of no effect in regard to EOF stabilization in empty channels but may have an influence in channels filled with a charged monolith. In fused-silica capillaries the EOF was generally found to decrease from 'naked' to surface-treated to monolith-filled capillaries. The EOF tended to be higher when an organic solvent (acetonitrile) was added to the mobile phase and could be further increased by substituting the water with equal amounts of methanol. In addition, the hydrostatic pressure exerted by the EOF was investigated. In a microfluidic chip with empty (cross-)channels such an effect could be responsible for a redirection of the flow. In capillaries partially filled with a noncharged (non-EOF-generating) monolith, a linear relationship could be established between the EOF created in the empty section of the capillary (apparent mobility) and the length of the monolith (backpressure). In capillaries partially filled with a charged (EOF-producing) monolith, flow inhomogeneities must be expected as a consequence of a superimposition of hydrodynamic pressure and EOF as mobile phase driving force.

  13. Sealed silica pressure ampoules for crystal growth

    Science.gov (United States)

    Holland, L. R.

    1984-01-01

    The properties of vitreous silica and the mechanics of thick walled pressure vessels are reviewed with regard to the construction of sealed silica crucibles such as are used in the growth of mercury-cadmium telluride crystals. Data from destructive rupture tests are reported, failure modes discussed, and recommendations for design given. Ordinary commercial clear vitreous silica from flame fused quartz can withstand a surface stress of 20 MPa or more in this application.

  14. Preparation and Characterization of Gold Nanoparticle-Modified Silica Monolith for Capillary Electrochromatography%金纳米粒子修饰毛细管硅胶整体柱的制备及其电色谱性能研究

    Institute of Scientific and Technical Information of China (English)

    叶芳贵; 陆俊宇; 王圆; 张爱珠; 田建袅; 赵书林

    2011-01-01

    通过毛细管硅胶整体柱表面修饰十八烷基硫醇金纳米粒子,制备了一种新型毛细管电色谱固定相.制备金纳米粒子修饰整体柱时,采用溶胶-凝胶法制备毛细管硅胶整体柱,并在其表面化学修饰3-巯基丙基三甲氧基硅烷;通过巯基基团固载金纳米粒子于整体柱上,再共价键合十八烷基硫醇于金纳米粒子表面.以甲苯为探针,对理论塔板高度与流动相线速度之间的关系进行了考察,其最小理论塔板高度约为7.8 μm.考察了操作条件如流动相中的有机改性剂和缓冲溶液pH值对金纳米粒子修饰毛细管整体柱电渗流的影响,并与相应的毛细管硅胶整体柱(Silica)进行比较.以烷基苯同系物为模型化合物,评价了Silica、巯基 (Silica-SH)和十八烷基(Silica-GNPs-C18) 3种整体柱电色谱性能;还考察了烷基苯同系物在Silica-GNPs-C18上的保留行为.结果表明,其保留机理是基于典型的反相作用.另外,在甲醇含量为15%的流动相条件下,Silica-GNPs-C18还可实现4 种极性苯酚类物质的基线分离.%A novel silica monolithic stationary phase functionalized with octadecanethiol gold nanoparticles was prepared for capillary electrochromatography (CEC). The bare monolithic silica column was prepared by a sol-gel process and has been chemically modified with 3-mercaptopropyl-trimethoxysilane, followed by immobilization of gold nanoparticles and modification by octadecanethiol. The relationship between plot of plate height and the linear velocity on gold nanoparticle-modified silica monolith was investigated, and a minimum plate height of about 7.8 μm for toluene was obtained.The electroosmotic flow characteristics of the gold nanoparticle-modified silica monolith and bare silica monolith (Silica) were studied by varying the percentage of organic modifier in buffer and buffer pH.To evaluate the column performance, hydrophobic alkylbenzenes as model compounds were tested on the

  15. Functional Use Database (FUse)

    Data.gov (United States)

    U.S. Environmental Protection Agency — There are five different files for this dataset: 1. A dataset listing the reported functional uses of chemicals (FUse) 2. All 729 ToxPrint descriptors obtained from...

  16. Automation and integration of polymerase chain reaction with capillary electrophoresis for high throughput genotyping and disease diagnosis

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, N.

    1999-02-12

    Genotyping is to detect specific loci in the human genome. These loci provide important information for forensic testing, construction of genetic linkage maps, gene related disease diagnosis and pharmacogenetic research. Genotyping is becoming more and more popular after these loci can be easily amplified by polymerase chain reaction (PCR). Capillary electrophoresis has its unique advantages for DNA analysis due to its fast heat dissipation and ease of automation. Four projects are described in which genotyping is performed by capillary electrophoresis emphasizing different aspects. First, the author demonstrates a principle to determine the genotype based on capillary electrophoresis system. VNTR polymorphism in the human D1S80 locus was studied. Second, the separation of four short tandem repeat (STR) loci vWF, THO1, TPOX and CSF1PO (CTTv) by using poly(ethylene oxide) (PEO) was studied in achieving high resolution and preventing rehybridization of the DNA fragments. Separation under denaturing, non-denaturing conditions and at elevated temperature was discussed. Third, a 250 {micro}m i.d., 365 {micro}m o.d. fused silica capillary was used as the microreactor for PCR. Fourth, direct PCR from blood was studied to simplify the sample preparation for genotyping to minimum.

  17. Application of a low impedance contactless conductometric detector for the determination of inorganic cations in capillary monolithic column chromatography.

    Science.gov (United States)

    Shen, Dazhong; Li, Dongdong; Yang, Xiuwen; Zhu, Yan; Dong, Jianfeng; Kang, Qi

    2011-03-15

    Poly(glycidyl methacrylate) cation exchange monolithic column was prepared in fused-silica capillaries of 320 μm i.d. by thermally initiated radical polymerization and utilized in capillary ion chromatography. With 15 mM methanesulfonic acid as the mobile phase, the separations of a mixture of inorganic cations (Li(+), Na(+), NH(4)(+), K(+)) was tested by using a capacitively coupled contactless conductivity detector (C(4)D) and a low impedance C(4)D (LIC(4)D). The LIC(4)D is the series combination of a C(4)D and a quartz crystal resonator. At the resonant frequency of the series combination, the capacitor impedance from capillary wall was offset by the inductance impedance from the quartz crystal resonator. A minimum impedance was obtained in the impedance-frequency curve of the combination. The responses of the C(4)D and LIC(4)D were analyzed based on an equivalent circuit model. It was shown that the sensitivity of the C(4)D to the change in analyte concentration is rather poor due to the high ratio of the impedance from the capillary wall capacitor to the solution impedance. The LIC(4)D has the similar sensitivity as a contact conductivity detector but a much smaller cell volume. The on-column detection model was realized by LiC(4)D without preparation of optical detection window in monolithic column.

  18. Prepared polymethacrylate-based monoliths for the separation of cations by non-suppressed capillary ion chromatography.

    Science.gov (United States)

    Li, Jing; Zhu, Yan

    2014-01-01

    This paper describes a novel analytical system for non-suppressed capillary ion chromatography. Methacrylate monolithic columns were prepared from silanized fused-silica capillaries of 320 µm i.d. by in situ polymerization of glycidyl methacrylate and ethylene dimethacrylate in the presence of 1,4-butanediol, 1-propanol and water as the porogen solvents. The introduction of cation-exchange sites was achieved by sulfonating the matrix with sodium sulfite to produce total cation-exchange capacities in the range of 45-105 μequiv/mL for a 25 cm column. The conditions (concentrations of sodium sulfite solution, reacting time and modified flow rate) of sulfonation were optimized. The hydrodynamic and chromatographic performances were estimated. Coupled with a conductivity detector, a capillary ion chromatography system was set up with the prepared column. Finally, the resultant column was used for the separations of five common univalent cations (Li(+), Na(+), NH4(+), K(+) and Cs(+)) using methanesulfonic acid as the eluent and four divalent cations (Mg(2+), Ca(2+), Sr(2+) and Ba(2+)) by non-suppressed capillary ion chromatography; the chromatographic parameters were further researched.

  19. ESI-MS compatible permanent coating of glass surfaces using poly(ethylene glycol)-terminated alkoxysilanes for capillary zone electrophoretic protein separations.

    Science.gov (United States)

    Razunguzwa, Trust T; Warrier, Manoj; Timperman, Aaron T

    2006-07-01

    Thin poly(ethylene glycol) silane (PEG-silane) coatings formed from N-(triethoxysilyl propyl)-O-poly(ethylene oxide) urethane with different chain lengths of poly(ethylene glycol) (MW 750 and 4000-5000) are used to modify glass microfluidic channels and fused-silica capillaries for electrophoretic separations of proteins. These coatings combine three important properties, which make them favorable for proteomic analyses including reduction of protein adsorption, compatibility with mass spectrometry due to their stability, and the ability to control the magnitude of electroosmotic flow (EOF). The coatings have been successfully used in microfluidic chips and fused-silica capillaries for separation of protein sample mixtures under low EOF conditions. The long-chain and mixed PEG-silane coatings suppress electroosmotic flow by more than 90%, whereas the short-chain PEG silane suppresses EOF by 65-75% at pH values of 3-9. The long-chain and mixed PEG-silane coatings are suitable for low EOF applications or for cases where negative effects of EOF are to be minimized. Efficient separations of unlabeled basic proteins at low pH and FITC-labeled proteins at high pH were achieved, as well as excellent stability for at least 200 electrophoretic runs. Additionally, these covalent coatings produce no detectable background ions in ESI-MS, making them compatible with on-line mass spectrometry.

  20. Thiol-yne Click Adamantane Monolithic Stationary Phase for Capillary Electrochromatography

    Institute of Scientific and Technical Information of China (English)

    Dao, Thi Thu Hien; Guerrouache, Mohamed; Carbonnier, Benjamin

    2012-01-01

    A porous crosslinked organic polymer based on N-acryloxysuccinimide (NAS) and ethylene dimethacrylate (EDMA) was prepared inside 75 μm i.d. fused silica capillary as functionalizable monolithic stationary phase for electrochromatographic applications. Succinimide groups on the monolith surface provide reactive sites able to re- act readily through standard electrophile-nucleophile chemistry. Propargylamine was used to prepare alkyne func- tionalized poly(NAS-co-EDMA). Onto this thiol-reactive polymer surface was grafted adamantane units via a photochemically-driven addition reaction. Chemical characterization was performed in situ after each synthetic step by means of Raman spectroscopy and grafting kinetics was investigated to ensure quantitative grafting of 1-adamantanethiol. The as-designed monolithic stationary phase exhibited typical reversed-phase separation mechanism as evidenced by the linear increase of the logarithm of retention factor of neutral aromatic solutes with the increase of the aqueous buffer content in the mobile phase.

  1. Simultaneous determination of caffeine, paracetamol, and ibuprofen in pharmaceutical formulations by high-performance liquid chromatography with UV detection and by capillary electrophoresis with conductivity detection.

    Science.gov (United States)

    Cunha, Rafael R; Chaves, Sandro C; Ribeiro, Michelle M A C; Torres, Lívia M F C; Muñoz, Rodrigo A A; Dos Santos, Wallans T P; Richter, Eduardo M

    2015-05-01

    Paracetamol, caffeine and ibuprofen are found in over-the-counter pharmaceutical formulations. In this work, we propose two new methods for simultaneous determination of paracetamol, caffeine and ibuprofen in pharmaceutical formulations. One method is based on high-performance liquid chromatography with diode-array detection and the other on capillary electrophoresis with capacitively coupled contactless conductivity detection. The separation by high-performance liquid chromatography with diode-array detection was achieved on a C18 column (250×4.6 mm(2), 5 μm) with a gradient mobile phase comprising 20-100% acetonitrile in 40 mmol L(-1) phosphate buffer pH 7.0. The separation by capillary electrophoresis with capacitively coupled contactless conductivity detection was achieved on a fused-silica capillary (40 cm length, 50 μm i.d.) using 10 mmol L(-1) 3,4-dimethoxycinnamate and 10 mmol L(-1) β-alanine with pH adjustment to 10.4 with lithium hydroxide as background electrolyte. The determination of all three pharmaceuticals was carried out in 9.6 min by liquid chromatography and in 2.2 min by capillary electrophoresis. Detection limits for caffeine, paracetamol and ibuprofen were 4.4, 0.7, and 3.4 μmol L(-1) by liquid chromatography and 39, 32, and 49 μmol L(-1) by capillary electrophoresis, respectively. Recovery values for spiked samples were between 92-107% for both proposed methods.

  2. On-column micro gas chromatography detection with capillary-based optical ring resonators.

    Science.gov (United States)

    Shopova, Siyka I; White, Ian M; Sun, Yuze; Zhu, Hongying; Fan, Xudong; Frye-Mason, Greg; Thompson, Aaron; Ja, Shiou-jyh

    2008-03-15

    We developed a novel on-column micro gas chromatography (microGC) detector using capillary based optical ring resonators (CBORRs). The CBORR is a thin-walled fused silica capillary with an inner diameter ranging from a few tens to a few hundreds of micrometers. The interior surface of the CBORR is coated with a layer of stationary phase for gas separation. The circular cross section of the CBORR forms a ring resonator and supports whispering gallery modes (WGMs) that circulate along the ring resonator circumference hundreds of times. The evanescent field extends into the core and is sensitive to the refractive index change induced by the interaction between the gas sample and the stationary phase. The WGM can be excited and monitored at any location along the CBORR by placing a tapered optical fiber against the CBORR, thus enabling on-column real-time detection. Rapid separation of both polar and nonpolar samples was demonstrated with subsecond detection speed. Theoretical work was also established to explain the CBORR detection mechanism. While low-nanogram detection limits are observed in these preliminary tests, many methods for improvements are under investigation. The CBORR is directly compatible with traditional capillary GC columns without any dead volumes. Therefore, the CBORR-based muGC is a very promising technology platform for rapid, sensitive, and portable analytical devices.

  3. Validated Method for the Determination of Piroxicam by Capillary Zone Electrophoresis and Its Application to Tablets

    Directory of Open Access Journals (Sweden)

    Arın Gül Dal

    2014-01-01

    piroxicam in tablets. The separation of piroxicam was conducted in a fused-silica capillary by using 10 mM borate buffer (pH 9.0 containing 10% (v/v methanol as background electrolyte. The optimum conditions determined were 25 kV for separation voltage and 1 s for injection time. Analysis was carried out with UV detection at 204 nm. Naproxen sodium was used as an internal standard. The method was linear over the range of 0.23–28.79 µg/mL. The accuracy and precision were found to be satisfied within the acceptable limits (<2%. The LOD and LOQ were found to be 0.07 and 0.19 µg/mL, respectively. The method described here was applied to tablet dosage forms and the content of a tablet was found in the limits of USP-24 suggestions. To compare the results of capillary electrophoretic method, UV spectrophotometric method was developed and the difference between two methods was found to be insignificant. The capillary zone electrophoretic method developed in this study is rapid, simple, and suitable for routine analysis of piroxicam in pharmaceutical tablets.

  4. Separation and determination of cefotaxime enantiomers in injections by capillary zone electrophoresis.

    Science.gov (United States)

    Wang, Rong; Jia, Zheng-Ping; Fan, Jun-Jie; Ma, Jun; Hua, Xie; Zhang, Qiang; Wang, Juan

    2009-03-01

    Cefotaxime enantiomers have specific effects on Gram-negative bacteria. For quality control of cefotaxime it was necessary to establish a method for enantioseparation by capillary zone electrophoresis (CZE) using cyclodextrin (CD) as a chiral selector. The effects of various parameters on enantioseparation were studied. A fused silica capillary (40 cm effective length x 75 microm ID) was used. The cefotaxime enantiomers were separated on the baseline under conditions of 0.5 mmol/L CM-beta-CD, 75 mmol/L NaH2PO4 buffer at pH 7.0 using UV detection at 280 nm. Applied voltage and capillary temperature were 20 kV and 25 degrees C, respectively. Under these conditions for enantioseparation, linear calibration curves were obtained in the range 2 approximately 160 microg/mL. The limit of detection for both isomers was less than 0.5 microg/mL. The method was used for analysis of pharmaceutical preparations (dosage forms) of cefotaxime from various factories. A simple and specific CZE method was successfully demonstrated for the separation of cefotaxime enantiomers. The enantioseparation method should be established and this method should be used to control the quality of cefotaxime.

  5. Pore capillary pressure and saturation of methane hydrate bearing sediments

    Institute of Scientific and Technical Information of China (English)

    SUN Shicai; LIU Changling; YE Yuguang; LIU Yufeng

    2014-01-01

    To better understand the relationship between the pore capillary pressure and hydrate saturation in sedi-ments, a new method was proposed. First, the phase equilibria of methane hydrate in fine-grained silica sands were measured. As to the equilibrium data, the pore capillary pressure and saturation of methane hydrate were calculated. The results showed that the phase equilibria of methane hydrates in fine-grained silica sands changed due to the depressed activity of pore water caused by the surface group and negatively charged characteristic of silica particles as well as the capillary pressure in small pores together. The capil-lary pressure increased with the increase of methane hydrate saturation due to the decrease of the available pore space. However, the capillary-saturation relationship could not yet be described quantitatively because of the stochastic habit of hydrate growth.

  6. [The novel copolymer coated capillary columns of electrophoresis and their applications to separation of proteins].

    Science.gov (United States)

    Lu, G; Gao, D; Gu, J; Fu, R; Li, F; Zhang, H

    1999-01-01

    The copolymer of acrylonitrile, methyl acrylate, hydroxy ethyl acrylate (ZB-004), the copolymer of acrylonitrile, methyl acrylate, hydroxy ethyl acrylate, acrylamide (ZB-014) and the copolymer of acrylonitrile, hydroxy ethyl acrylate (ZB-016) were coated on the inner surface of fused-silica capillaries by just filling the capillary with solutions containing these copolymers followed by flushing the capillary with nitrogen. The physically adsorbed layer can reduce both protein adsorption and electroosmotic flow in the pH range of 3-5. Electroosmotic flow decreased by raising the concentrations of the copolymers. Separation performance of ZB-004 layer is better than those of other two layers due to its low hydrophilicity, but with higher pH values, appreciable peak deformation and increase in electroosmosis were observed. The intra day and inter day migration reproducibility were investigated in terms of relative standard deviation (RSD) with four basic proteins at pH 4.0. The RSDs of the intra day migration times were less than 2%. The RSDs of the inter day migration times were less than 4%. At pH 5.0, the RSDs of the migration times in two ZB-004-coated capillaries made on two different days were less than 1%. Separation efficiencies of four basic proteins in a ZB-004-coated capillary which stored in a buffer (pH 4.0) for fifteen days after being used for 14 days decreased 15%. These coatings were stable and exhibited reproducible separations from intra day, inter day and inter column under acidic conditions.

  7. Polymer-coated fibrous materials as the stationary phase in packed capillary gas chromatography.

    Science.gov (United States)

    Saito, Yoshihiro; Tahara, Ai; Imaizumi, Motohiro; Takeichi, Tsutomu; Wada, Hiroo; Jinno, Kiyokatsu

    2003-10-15

    Synthetic polymer filaments have been introduced as the support material in packed capillary gas chromatography (GC). The filaments of the heat-resistant polymers, Zylon, Kevlar, Nomex, and Technora, were longitudinally packed into a short fused-silica capillary, followed by the conventional coating process for open-tubular GC columns. The separation of several test mixtures such as n-alkylbenzenes and n-alkanes was carried out with these polymer-coated fiber-packed capillary columns. With the coating by various polymeric materials on the surface of these filaments, the retentivity was significantly improved over the parent fiber-packed column (without polymer coating) as well as a conventional open-tubular capillary of the same length. The results demonstrated a good combination of Zylon as the support and poly(dimethylsiloxane)-based materials as the coating liquid-phase for the successful GC separation of n-alkanes and polycyclic aromatic hydrocarbons (PAHs), while successful applications for other separations such as poly(ethylene glycol) coating for the separation of alcohols were also obtained. From the results it has been suggested that the selectivity of the fiber-packed column could be tuned by selecting different coating materials, indicating the promising possibility for a novel usage of fine fibrous polymers as the support material that can be combined with newly synthesized coating materials specially designed for particular separations. Taking advantage of good thermal stability of the fibers, the column temperature could be elevated to higher than 350 degrees C with the combination of a short metallic capillary.

  8. Experimental study and simulation of fused silica damage initiation by laser pulse irradiation; Etude experimentale et modelisation de l'initiation de l'endommagement de la silice sous irradiation laser impulsionnelle

    Energy Technology Data Exchange (ETDEWEB)

    Bonneau, F.; Combis, J.L.; Vierne, J. [CEA Bruyeres-le-Chatel, Dept. de Physique Theorique et Appliquee, 91 (France)] [and others

    2002-07-01

    In order to resolve problems concerning the understanding and the control of laser-induced damage of silica optical elements, a collaboration between the CEA (CESTA/DLP, DIF/DPTA, and Grenoble/LETI) and different university laboratories has been undertaken. Ultra-pure silica 'model' samples, seeded with gold nano-particles whose diameter does not exceed 5 nm, were made at the LASIM in Lyon. The aim in using these samples is to observe the mechanism of damage initiation that can be attributed to inclusions of nano-metric site. This report presents the different steps encountered during this study: making the samples, the laser-induced damage tests performed at the CESTA, and the 'Nomarski' and 'atomic force' microscope observations of this damage carried out at the Fresnel Institute in Marseille. These samples were also used for a series of experiments using a time-of-flight mass spectrometer at ANL near Chicago. This installation is of great interest because it enables us to combine the laser irradiation of the sample with the chemical identification of material ejected by the sample. A precise evaluation of the quantity of gold atoms emitted during irradiation can thus be obtained from the experimental results. The experimental data is then interpreted, and in particular, compared to, numerical simulations obtained with the DELPOR program. A very encouraging result is the existence of a pre-damage phase at very low fluences that is not detectable by classical optical devices. The experimental means developed for such 'model' samples should be transposable to the analysis of industrial glasses. (authors)

  9. 用于高效液相色谱和开管毛细管电色谱的氢化硅胶分离材料%Hydride-Based Separation Materials for High Performance Liquid Chromatography and Open Tubular Capillary Electrochromatography

    Institute of Scientific and Technical Information of China (English)

    PESEK Joseph J; MATYSKA Maria T

    2005-01-01

    Silica hydride is a recent development in chromatographic support materials for high performance liquid chromatography (HPLC) where hydride groups replace 95% of the silanols on the surface. This conversion changes many of the fundamental properties of the material as well as the bonded stationary phases that are the result of further chemical modification of the hydride surface. Some unique chromatographic properties of hydride-based phases are described as well as some general application areas where these bonded materials may be used in preference to or have advantages not available from typical stationary phases. The fabrication, properties and applications of etched chemically modified capillaries for electrophoretic analysis are also reviewed. It is shown that the etching process creates a surface that is fundamentally different than a bare fused silica capillary. The new surface matrix produces unique electroosmotic flow properties and is more compatible with basic and biological compounds. After chemical modification of the surface, the bonded organic moiety (stationary phase) contributes to the control of migration of solutes in the capillary. Both electrophoretic and chromatographic processes take place in the etched chemically modified capillaries leading to a variety of experimental variables that can be used to optimize separations. A number of examples of separations on these capillaries are described.

  10. Germania-based, sol-gel hybrid organic-inorganic coatings for capillary microextraction and gas chromatography.

    Science.gov (United States)

    Fang, Li; Kulkarni, Sameer; Alhooshani, Khalid; Malik, Abdul

    2007-12-15

    Germania-based, sol-gel hybrid organic-inorganic coatings were developed for capillary microextraction and gas chromatography (GC). Being an isostructural analogue of SiO2, GeO2 is compatible with the silica network. Because of this similarity, germania-based materials possess great potential for being used in the areas of chromatographic separation and sample preparation. These possibilities, however, remain practically unexplored. To our knowledge, this is the first instance that a germania-based hybrid sol-gel material is used as a sorbent in analytical sample preparation or chromatographic separation. Tetramethoxygermane was used as a precursor to create a sol-gel network via hydrolytic polycondensation reactions performed within a fused-silica capillary. The growing sol-gel germania network was simultaneously reacted with an organic ligand that contained sol-gel-active sites in its chemical structure. Three different sol-gel-active ligands were used: (a) hydroxy-terminated poly(dimethylsiloxane), (b) hydroxy-terminated poly(dimethyldiphenylsiloxane), and (c) 3-aminopropyltrimethoxysilane. Sol-gel germania-coated capillaries of desired polarity and extraction selectivity were prepared by using an appropriately selected sol-gel-active ligand in the sol solution. These capillaries were further used to extract trace concentrations of polycyclic aromatic hydrocarbons, aldehydes, ketones, alcohols, phenols, and free fatty acids from aqueous samples. The extracted solutes were further analyzed by GC-FID. The new germania-based coatings showed excellent stability under harsh operation conditions involving extreme pH values, high temperatures, and aggressive solvents. Our preliminary results also indicate that sol-gel hybrid germania coatings have the potential to offer great analytical performance as GC stationary phases.

  11. Capillary origami

    OpenAIRE

    Py, Charlotte; Reverdy, Paul; Doppler, L.; J. Bico; Roman, B.; Baroud, Charles,

    2007-01-01

    International audience; The hairs of a wet dog rushing out from a pond assemble into bundles; this is a common example of the effect of capillary forces on flexible structures. From a practical point of the deformation and adhesion of compliant structures induced by interfacial forces may lead to disastrous effects in mechanical microsystems.

  12. Heterogeneous integration of gallium nitride light-emitting diodes on diamond and silica by transfer printing.

    Science.gov (United States)

    Trindade, A J; Guilhabert, B; Xie, E Y; Ferreira, R; McKendry, J J D; Zhu, D; Laurand, N; Gu, E; Wallis, D J; Watson, I M; Humphreys, C J; Dawson, M D

    2015-04-06

    We report the transfer printing of blue-emitting micron-scale light-emitting diodes (micro-LEDs) onto fused silica and diamond substrates without the use of intermediary adhesion layers. A consistent Van der Waals bond was achieved via liquid capillary action, despite curvature of the LED membranes following release from their native silicon growth substrates. The excellence of diamond as a heat-spreader allowed the printed membrane LEDs to achieve optical power output density of 10 W/cm(2) when operated at a current density of 254 A/cm(2). This high-current-density operation enabled optical data transmission from the LEDs at 400 Mbit/s.

  13. Effect of Joule heating on efficiency and performance for microchip-based and capillary-based electrophoretic separation systems: a closer look.

    Science.gov (United States)

    Petersen, Nickolaj J; Nikolajsen, Rikke P H; Mogensen, Klaus B; Kutter, Jörg P

    2004-01-01

    An attempt is made to revisit the main theoretical considerations concerning temperature effects ("Joule heating") in electro-driven separation systems, in particular lab-on-a-chip systems. Measurements of efficiencies in microfabricated devices under different Joule heating conditions are evaluated and compared to both theoretical models and measurements performed on conventional capillary systems. The widely accepted notion that planar microdevices are less susceptible to Joule heating effects is largely confirmed. The heat dissipation from a nonthermostatically controlled glass microdevice was found to be comparable to that from a liquid-cooled-fused silica capillary. Using typically dimensioned glass and glass/silicon microdevices, the experimental results indicate that 5-10 times higher electric field strengths can be applied than on conventional capillaries, before detrimental effects on the separation efficiency occur. The main influence of Joule heating on efficiency is via the establishment of a radial temperature profile across the lumen of the capillary or channel. An overall temperature increase of the buffer solution has only little influence on the quality of the separation. Still, active temperature control (cooling, thermostatting) can help prevent boiling of the buffer and increase the reproducibility of the results.

  14. Graphene/poly(ethylene-co-vinyl acetate) composite electrode fabricated by melt compounding for capillary electrophoretic determination of flavones in Cacumen platycladi.

    Science.gov (United States)

    Sheng, Shijun; Liu, Shuang; Zhang, Luyan; Chen, Gang

    2013-02-01

    In this report, a graphene/poly(ethylene-co-vinyl acetate) composite electrode was fabricated by melt compounding for the amperometric detection of capillary electrophoresis. The composite electrode was fabricated by packing a mixture of graphene and melted poly(ethylene-co-vinyl acetate) in a piece of fused silica capillary under heat. The structure of the composite was investigated by scanning electron microscopy and Fourier transform infrared spectroscopy. The results indicated that graphene sheets were well dispersed in the composite to form an interconnected conducting network. The performance of this unique graphene-based detector has been demonstrated by separating and detecting rutin, quercitrin, kaempferol, and quercetin in Cacumen platycladi in combination with capillary electrophoresis. The four flavones have been well separated within 9 min in a 50-cm-long capillary at a separation voltage of 12 kV using a 50 mM sodium borate buffer (pH 9.2). The graphene-based detector offered significantly lower operating potentials, substantially enhanced signal-to-noise characteristics, lower expense of operation, high resistance to surface fouling, and enhanced stability. It showed long-term stability and repeatability with relative standard deviations of <5% for the peak current (n = 15).

  15. Reproducible preparation of nanospray tips for capillary electrophoresis coupled to mass spectrometry using 3D printed grinding device.

    Science.gov (United States)

    Tycova, Anna; Prikryl, Jan; Foret, Frantisek

    2016-04-01

    The use of high quality fused silica capillary nanospray tips is critical for obtaining reliable and reproducible electrospray/MS data; however, reproducible laboratory preparation of such tips is a challenging task. In this work, we report on the design and construction of low-cost grinding device assembled from 3D printed and commercially easily available components. Detailed description and characterization of the grinding device is complemented by freely accessible files in stl and skp format allowing easy laboratory replication of the device. The process of sharpening is aimed at achieving maximal symmetricity, surface smoothness and repeatability of the conus shape. Moreover, the presented grinding device brings possibility to fabricate the nanospray tips of desired dimensions regardless of the commercial availability. On several samples of biological nature (reserpine, rabbit plasma, and the mixture of three aminoacids), performance of fabricated tips is shown on CE coupled to MS analysis. The special interest is paid to the effect of tip sharpness.

  16. Capillary electrophoresis of heparin and other glycosaminoglycans using a polyamine running electrolyte

    Energy Technology Data Exchange (ETDEWEB)

    Loegel, Thomas N.; Trombley, John D.; Taylor, Richard T. [Department of Chemistry and Biochemistry, Miami University, Oxford, OH 45056 (United States); Danielson, Neil D., E-mail: danielnd@muohio.edu [Department of Chemistry and Biochemistry, Miami University, Oxford, OH 45056 (United States)

    2012-11-13

    Highlights: Black-Right-Pointing-Pointer Ethylenediamine is likely acting as an ion-pairing agent. Black-Right-Pointing-Pointer Oversulfated chondroitin sulfate is last peak instead of first peak. Black-Right-Pointing-Pointer There is about a factor of five improved detectability with a 12.5 min analysis time. Black-Right-Pointing-Pointer Use of a 50 {mu}m ID capillary is possible. - Abstract: This study involves the use of polyamines as potential resolving agents for the capillary electrophoresis (CE) of glycosaminoglycans (GAGs), specifically heparin, dermatan sulfate, chondroitin sulfate, over-sulfated chondroitin sulfate (OSCS), and hyaluronan. All of the compounds can be separated from each other with the exception of chondroitin sulfate and hyaluronan. Using optimization software, the final run conditions are found to be 200 mM ethylenediamine and 45.5 mM phosphate as the electrolyte with -14 V applied across a 50 {mu}m ID Multiplication-Sign 24.5 cm fused silica capillary at 15 Degree-Sign C. The ion migration order, with OSCS as the last instead of the first peak, is in contrast to previous reports using either a high molarity TRIS or lithium phosphate run buffer with narrower bore capillaries. Total analysis time is 12. 5 min and the relative standard deviation of the heparin migration time is about 2.5% (n = 5). The interaction mechanism between selected polyamines and heparin is explored using conductivity measurements in addition to CE experiments to show that an ion-pairing mechanism is likely.

  17. Analysis of Proteins, Protein Complexes, and Organellar Proteomes Using Sheathless Capillary Zone Electrophoresis - Native Mass Spectrometry

    Science.gov (United States)

    Belov, Arseniy M.; Viner, Rosa; Santos, Marcia R.; Horn, David M.; Bern, Marshall; Karger, Barry L.; Ivanov, Alexander R.

    2017-09-01

    Native mass spectrometry (MS) is a rapidly advancing field in the analysis of proteins, protein complexes, and macromolecular species of various types. The majority of native MS experiments reported to-date has been conducted using direct infusion of purified analytes into a mass spectrometer. In this study, capillary zone electrophoresis (CZE) was coupled online to Orbitrap mass spectrometers using a commercial sheathless interface to enable high-performance separation, identification, and structural characterization of limited amounts of purified proteins and protein complexes, the latter with preserved non-covalent associations under native conditions. The performance of both bare-fused silica and polyacrylamide-coated capillaries was assessed using mixtures of protein standards known to form non-covalent protein-protein and protein-ligand complexes. High-efficiency separation of native complexes is demonstrated using both capillary types, while the polyacrylamide neutral-coated capillary showed better reproducibility and higher efficiency for more complex samples. The platform was then evaluated for the determination of monoclonal antibody aggregation and for analysis of proteomes of limited complexity using a ribosomal isolate from E. coli. Native CZE-MS, using accurate single stage and tandem-MS measurements, enabled identification of proteoforms and non-covalent complexes at femtomole levels. This study demonstrates that native CZE-MS can serve as an orthogonal and complementary technique to conventional native MS methodologies with the advantages of low sample consumption, minimal sample processing and losses, and high throughput and sensitivity. This study presents a novel platform for analysis of ribosomes and other macromolecular complexes and organelles, with the potential for discovery of novel structural features defining cellular phenotypes (e.g., specialized ribosomes). [Figure not available: see fulltext.

  18. Capillary zone electrophoresis for determination of vildagliptin (a DPP-4 inhibitor) in pharmaceutical formulation and comparative study with HPLC.

    Science.gov (United States)

    Barden, A T; Piccoli, B L; Volpato, N M; Schapoval, E E S; Steppe, M

    2014-02-01

    A stability-indicating capillary zone electrophoresis (CZE) method was validated for the determination of vildagliptin (VLG) in pharmaceutical dosage forms using ranitidine hydrochloride (RH) as internal standard. The CZE method was carried out in a fused silica capillary (64.5 cm total length and 56.0 cm effective length, 50 microm i.d.) by applying a potential of 25 kV (positive polarity), hydrodynamic injection by 50 mbar for 5 s and the temperature of the capillary cartridge was 25 degreesC. The selected background electrolyte (BGE) consisted of 25 mM potassium phosphate (pH 8.0) with UV/PDA detection at 207 nm. The electrophoretic separation was obtained within 6 min and was linear in the range of 50-200 microg/mL (r= 0.9994). The specificity and the stability-indicating capability were demonstrated through degradation studies, which also showed that there was no interference of the formulation excipients. The method was validated in accordance to ICH guidelines acceptance criteria for specificity, linearity, precision, accuracy, robustness and system suitability. The proposed method was compared with HPLC method previously validated for this drug, and statistical analysis showed no significant difference between the methods.

  19. Determination of arbutin and bergenin in Bergeniae Rhizoma by capillary electrophoresis with a carbon nanotube-epoxy composite electrode.

    Science.gov (United States)

    Zhang, Luyan; Zhang, Wei; Chen, Gang

    2015-11-10

    This report describes the fabrication and the application of a novel carbon nanotube (CNT)-epoxy composite electrode as a sensitive amperometric detector for the capillary electrophoresis (CE). The composite electrode was fabricated on the basis of the in situ polycondensation of a mixture of CNTs and 1,2-ethanediamine-containing bisphenol A epoxy resin in the inner bore of a piece of fused silica capillary under heat. It was coupled with CE for the separation and detection of arbutin and bergenin in Bergeniae Rhizoma, a traditional Chinese medicine, to demonstrate its feasibility and performance. The two phenolic constituents were well separated within 10min in a 45cm capillary length at a separation voltage of 12kV using a 50mM borate buffer (pH 9.2). The CNT-based detector offered higher sensitivity, significantly lower operating potential, satisfactory resistance to surface fouling, and lower expense of operation, indicating great promise for a wide range of analytical applications. It showed long-term stability and reproducibility with relative standard deviations of less than 5% for the peak current (n=15).

  20. Dual-channel capillary electrophoresis for simultaneous determination of cations and anions.

    Science.gov (United States)

    Opekar, František; Tůma, Petr

    2016-05-13

    An original electrophoresis apparatus for simultaneous rapid determination of cations and anions has been designed and tested. The separation part of the apparatus consists of two identical fused-silica capillaries, each with a length of 10.5cm and inner diameter of 25μm. The injection space is formed by the crossing of four channels in a plexiglass cross-piece. The capillaries pass through two opposing channels and their injection ends are located opposite one another at a distance of approx. 0.5mm in the centre of the crossing point. The exit ends of the capillaries are placed in vessels containing the background electrolyte in which are immersed the electrodes of a high-voltage source. Contactless conductivity detectors with semi-cylindrical electrodes are located 2cm from the exit ends of the capillaries. The injection part of the apparatus consists of two piezoelectric micro-pumps bringing the solution through another channel in the cross-piece to the injection ends of the capillary. During the injection, the sample is brought through one of them and is injected electrokinetically for a defined time. Then the sample zone is forced out of the injection space by a stream of background electrolyte from the second micro-pump. The timing of the injection process is computer-controlled. Thus the equipment can be considered to constitute electrophoresis in one capillary with injection into its centre. The use of short capillaries and miniature micro-pumps without other mechanical components enabled the construction of the apparatus on a board with dimensions of 20×25cm. The proposed equipment was used to test simultaneous separation of a mixture of cations and anions, NH4(+), K(+), Ca(2+), Mg(2+), Sr(2+), Ba(2+), Cl(-), NO3(-), SO4(2-), ClO3(-) and F(-), in BGE with composition 500mM HAc+20mM Tris+2mM 18-crown-6 (pH 3.3). Baseline separation of all the components was achieved in time less than 1min. Quantification of the content of nitrate nitrogen (determined as

  1. POLYMER-COATED FIBROUS MATERIALS AS THE STATIONARY PHASE IN PACKED CAPILLARY GAS CHROMATOGRAPHY AND THE APPLICATIONS FOR SAMPLE PREPARATION IN ENVIRONMENTAL ANALYSIS%聚合物涂层纤维材料为固定相填充毛细管气相色谱及其在样品预处理中的应用

    Institute of Scientific and Technical Information of China (English)

    SAITOYoshihiro; JINNOKiyokatsu

    2003-01-01

    Fibrous polymers having an excellent heat-resistance were successfully introduced as the stationary phase in capillary gas chromatography (GC) and the basic separation performance has been investigated. Poly(p-phenylene-26-benzobisoxazole); Zylon, fibers were selected as the stationary phase taking into account the chemical structure, heat resistance, solvent resistance and the physical strength. About 330 filaments of the polymer were packed longitudinally into fused-silica capillaries of 0.32 mm i.d., and the GC separation of several test mixtures, such as n-alkylbenzenes and n-alkanes was carried out with these fiber-packed capillary columns. From the results it has been demonstrated that the fiber-packed capillary columns have a great potential as the separation media for volatile compounds. Polymer coating onto the surface of the packed-filaments has been also studied, and the results clearly showed that the retentivity was significantly improved over a conventional capillary columns of the same length and that the selectivity can be tuned by selecting different types of coating materials selected for the purposes. The applications of polymer-coated fiber-packed capillary as a miniaturized sample preparation device was also investigated for the analysis of environmental pollutants in river water samples.

  2. Polydopamine-supported immobilization of covalent-organic framework-5 in capillary as stationary phase for electrochromatographic separation.

    Science.gov (United States)

    Bao, Tao; Tang, Pingxiu; Kong, Deying; Mao, Zhenkun; Chen, Zilin

    2016-05-06

    Covalent-organic frameworks (COFs) are attractive materials for their fascinating properties, such as rigid structures, exceptional thermal stabilities, low densities, and permanent porosity with specific surface areas, which indicate potential for application in chromatography similar to related metal-organic frameworks (MOFs). However, the utilization of COFs in analytical chemistry is far behind as compared to that of the MOFs due to the challenging work of their immobilization. Here, we have successfully demonstrated the growth of the boron COF-5 on the inner wall of the fused silica capillary by a developed polydopamine-supported method. Combined with the layer-by-layer strategy, multilayer COF-5-coated capillary was obtained. The formation of COF-5 on polydopamine-coated substrate has been confirmed by scanning electron microscopy, Fourier transform infrared spectroscopy, X-ray diffraction. A novel stationary phase of COF-5 was developed on the basis of successful growth of COF-5 on polydopamine for open-tubular capillary electrochromatography (OT-CEC). Baseline separation of neutral, acidic and basic analytes was achieved on multilayer COF-5-coated capillary column. The fabricated capillary columns showed high column efficiency (154,060 plates/m for methylbenzene), excellent stability and repeatability. The precision (relative standard deviation (RSD), n=3) of retention time, peak height, and peak area for tested neutral compounds were in the range of 1.2-1.3%, 1.8-4.2%, and 0.9-2.4%, respectively. To the best of our knowledge, it was the first demonstration that COF-5 was developed as a novel stationary phase. Copyright © 2016 Elsevier B.V. All rights reserved.

  3. Simultaneous Determination of FOur Arsenic Additives in Animal Feed by Capillary Electrophoresis

    Institute of Scientific and Technical Information of China (English)

    BaoguoSun; MiroslavMacka; 等

    2002-01-01

    Four additives,[4-hydroxy-3-nitrophenylarsonic acid(Roxarsone),4-nitrophenylarsonic acid(4-NPAA),phenylarsonic acid (PAA) and p-aminophenylarsonic acid (p-ASA)] in chicken feed were simultaneously determinated by capillary zone electrophoresis(CZE) with on -line UV-detection.Based on our previous research,the sample extraction,cleanup and detection condition were discussed and optimised,Analytes were extracted with acidic 20% acetonitrile and the cleaned up with C18 SPE before the detection.20mM Carbonate buffer at pH10 was used as electrolyte,A fused silica capillary(48.5cm x75um),18kV working voltage and 200nm detection wavelength were applied for CE detection.Acetonitrile functioned as a modifier to reduce the conductivity of the sample soulution during the CE separation.The sensityvity of the method is sufficient for the routine inspection of Roxarsone in animal feed,The recoveries for all analytes were reasonably good but the precision of the method was poorer than HPLC.

  4. Capillary electrophoresis micro X-ray fluorescence: a tool for benchtop elemental analysis.

    Science.gov (United States)

    Miller, Thomasin C; Joseph, Martha R; Havrilla, George J; Lewis, Cris; Majidi, Vahid

    2003-05-01

    A new tool was developed for separation and elemental detection by interfacing a simple capillary electrophoresis (CE) apparatus, constructed using a thin-walled fused-silica capillary, with a benchtop energy-dispersive micro X-ray fluorescence (MXRF) system. X-ray excitation and detection of the separated analytes was done using an EDAX Eagle II micro X-ray fluorescence system equipped with a polycapillary Rh target excitation source and a SiLi detector. It was demonstrated that this prototype system could be used for the separation and detection of species containing two different metals from one another, specifically Cu and Co. Free Co could also be separated from Co bound to cyanocobalamin (vitamin B-12). Two organic compounds were also separated from one another, a large biological protein, ferritin, from a small biological organic, cyanocobalamin. Preliminary average detection limits obtained on this system were on the order of 10(-)(4) M and compared favorably to those reported for the similar technique of CE-synchrotron XRF. CEMXRF allows for nondestructive, simultaneous, on-line, benchtop elemental analysis for chemical speciation applications.

  5. Stereospecific micellar electrokinetic chromatography assay of methionine sulfoxide reductase activity employing a multiple layer coated capillary.

    Science.gov (United States)

    Zhu, Qingfu; El-Mergawy, Rabab G; Heinemann, Stefan H; Schönherr, Roland; Jáč, Pavel; Scriba, Gerhard K E

    2013-09-01

    A micellar electrokinetic chromatography method for the analysis of the l-methionine sulfoxide diastereomers employing a successive multiple ionic-polymer layer coated fused-silica capillary was developed and validated in order to investigate the stereospecificity of methionine sulfoxide reductases. The capillary coating consisted of a first layer of hexadimethrine and a second layer of dextran sulfate providing a stable strong cathodic EOF and consequently highly repeatable analyte migration times. The methionine sulfoxide diastereomers, methionine as product as well as β-alanine as internal standard were derivatized by dabsyl chloride and separated using a 35 mM sodium phosphate buffer, pH 8.0, containing 25 mM SDS as BGE and a separation voltage of 25 kV. The method was validated in the range of 0.15-2.0 mM with respect to linearity and precision. The LODs of the analytes ranged between 0.04 and 0.10 mM. The assay was subsequently applied to determine the stereospecificity of methionine sulfoxide reductases as well as the enzyme kinetics of human methionine sulfoxide reductase A. Monitoring the decrease of the l-methionine-(S)-sulfoxide Km = 411.8 ± 33.8 μM and Vmax = 307.5 ± 10.8 μM/min were determined.

  6. A robust method for iodine status determination in epidemiological studies by capillary electrophoresis.

    Science.gov (United States)

    de Macedo, Adriana Nori; Teo, Koon; Mente, Andrew; McQueen, Matthew J; Zeidler, Johannes; Poirier, Paul; Lear, Scott A; Wielgosz, Andy; Britz-McKibbin, Philip

    2014-10-21

    Iodine deficiency is the most common preventable cause of intellectual disabilities in children. Global health initiatives to ensure optimum nutrition thus require continuous monitoring of population-wide iodine intake as determined by urinary excretion of iodide. Current methods to analyze urinary iodide are limited by complicated sample pretreatment, costly infrastructure, and/or poor selectivity, posing restrictions to large-scale epidemiological studies. We describe a simple yet selective method to analyze iodide in volume-restricted human urine specimens stored in biorepositories by capillary electrophoresis (CE) with UV detection. Excellent selectivity is achieved when using an acidic background electrolyte in conjunction with dynamic complexation via α-cyclodextrin in an unmodified fused-silica capillary under reversed polarity. Sample self-stacking is developed as a novel online sample preconcentration method to boost sensitivity with submicromolar detection limits for iodide (S/N ≈ 3, 0.06 μM) directly in urine. This assay also allows for simultaneous analysis of environmental iodide uptake inhibitors, including thiocyanate and nitrate. Rigorous method validation confirmed good linearity (R(2) = 0.9998), dynamic range (0.20 to 4.0 μM), accuracy (average recovery of 93% at three concentration levels) and precision for reliable iodide determination in pooled urine specimens over 29 days of analysis (RSD = 11%, n = 87).

  7. Rapid and high resolution capillary supercritical fluid chromatography (SFC) and SFC/MS of trichothecene mycotoxins.

    Science.gov (United States)

    Smith, R D; Udseth, H R; Wright, B W

    1985-05-01

    The potential application of capillary column supercritical fluid chromatography (SFC) and SFC/mass spectrometry (SFC/MS) for the separation and analysis of mycotoxins of the trichothecene group was examined. Trichothecenes present significant analytical problems for both gas and liquid chromatography with a major difficulty for the latter being the lack of sufficiently sensitive and selective detectors. Supercritical carbon dioxide mobile phases at temperatures up to 100 degrees C were used with deactivated fused silica columns coated with crosslinked stationary phases. Separations were obtained under pressure ramped conditions using long (15 m) 50-micron i.d. columns for several trichothecenes (diacetoxyscirpenol, deoxynivalenol, and T-2 toxin) and related higher molecular weight macrocyclic (roridin and verrucarin) trichothecenes. In addition, new rapid pressure programming techniques with short (less than 2m) 25- to 50-micron i.d. capillary columns were used to obtain fast separations in as little as 1 min. SFC/MS with ammonia chemical ionization provided high selectivity and sensitive detection (with approximately 1-pg detection limits) for trichothecene mixtures. The extension to complex sample matrices is discussed and the application of selective MS/MS detection is demonstrated.

  8. Quantitative analysis of synthetic dyes in lipstick by micellar electrokinetic capillary chromatography.

    Science.gov (United States)

    Desiderio, C; Marra, C; Fanali, S

    1998-06-01

    The separation of synthetic dyes, used as color additives in cosmetics, by micellar electrokinetic capillary chromatography (MEKC) is described in this study. The separation of seven dyes, namely eosine, erythrosine, cyanosine, rhodamine B, orange II, chromotrope FB and tartrazine has been achieved in about 3 min in an untreated fused silica capillary containing as background electrolyte a 25 mM tetraborate/phosphate buffer, pH 8.0, and 30 mM sodium dodecyl sulfate. The electrophoretic method exhibits precision and relatively high sensitivity. A detection limit (LOD, signal/noise = 3) in the range of 5-7.5 X 10(-7) M of standard compounds was recorded. Intra-day repeatability of all the studied dye determinations (8 runs) gave the following results (limit values), % standard deviation: 0.24-1.54% for migration time, 0.99-1.24% for corrected peak areas, 0.99-1.24% for corrected peak area ratio (analyte/internal standard) and 1.56-2.74% for peak areas. The optimized method was successfully applied to the analysis of a lipstick sample where eosine and cyanosine were present.

  9. Capillary electrophoresis in the evaluation of ischemic injury: simultaneous determination of purine compounds and glutathione.

    Science.gov (United States)

    Carlucci, F; Tabucchi, A; Biagioli, B; Sani, G; Lisi, G; Maccherini, M; Rosi, F; Marinello, E

    2000-05-01

    An understanding of tissue energy metabolism and antioxidant status is of major interest in the field of organ preservation for transplantation. Nucleotide and glutathione are indicators of cell damage occurring during ischemia and reperfusion. A high performance capillary electrophoresis (HPCE) method with UV detection (185 nm) for the simultaneous analysis of intracellular free ribonucleotides, nucleosides, bases and glutathione (oxidized and reduced form) in myocardial tissues is described. The method does not involve thiol derivatization. The separations were carried out in an uncoated fused-silica capillary, 60 cm long, 52.5 cm to detector, 75 microm ID, with 20 mM Na-borate buffer, pH 10.00, at 20 kV voltage and reading at 185 nm. Injection was hydrostatic for 12 s and total analysis time was 20 min. The technique enables optimum separation of all the compounds examined and has a resolution similar to that of HPLC analysis, with the advantage of fast simultaneous measurement of cell nucleotide metabolism and redox state, not possible with HPLC.

  10. Analysis of red inks by micellar electrokinetic capillary chromatography with laser-induced fluorescence detection.

    Science.gov (United States)

    Król, Małgorzata; Gondko, Klaudia; Kula, Agnieszka; Kościelniak, Paweł

    2016-01-01

    A combination of MEKC with a--highly sensitive but not commonly used--LIF detector was tested regarding the possibility of differentiation of red inks. The separation process was conducted in a fused silica capillary (id 50 μm, 60/50 cm total/effective length) in BGE consisting of 40 mM sodium borate, 20 mM SDS and 10% v/v ACN with 30 kV applied. The optimized temperature of storage and capillary was 10 and 25°C, respectively. The samples were prepared using 20 dots (ø 0.5 mm), extracted in 35 μL BGE and diluted with 30 μL of water. The proposed method showed excellent repeatability and reproducibility (RSD (tm ) < 0.8 and < 2.5%, respectively). It was applied to group identification and differentiation of different brands, models, and batches of red printing, stamp, and pen inks. It was demonstrated that differentiation can be performed effectively on the basis of migration times and ratios of peak areas. The high efficiency of the developed method was indicated by discriminating power ranging from 87.3 to 98.8%, for stamp and pen inks, respectively. The results showed that the proposed procedure can be valuable for an objective examination of the red parts of questioned documents.

  11. Analysis of anionic metallized azo and formazan dyes by capillary electrophoresis-mass spectrometry.

    Science.gov (United States)

    Poiger, T; Richardson, S D; Baughman, G L

    2000-07-21

    Capillary electrophoresis-mass spectrometry was applied to the separation of several anionic dyes containing copper(II), chromium(III), or cobalt(III) as part of the dye molecule. The dyes were separated using a 110 cm x 50 microm uncoated fused-silica capillary and a 5 mM ammonium acetate buffer (pH 9) containing 40% acetonitrile. Excellent separation efficiencies (N = 500,000 plates/column) and low detection limits of 20-50 pg (selected ion monitoring, S/N = 10) were achieved. Mass spectra were acquired at different cone voltages. At low cone voltages (low collision energies), sensitivity was maximized and the mass spectra contained only signals of the (multiply charged) molecular ions and low levels of sodium ion and proton adducts. At higher cone voltages, the 2:1 (ligand:metal) chromium and cobalt dyes showed losses of one of the two dye ligands, accompanied by a reduction of the metal. The copper dyes showed signals due to loss of SO2 and SO3-, but no release of metal. Azo cleavage, otherwise typical of azo dyes, was not observed with the metallized dyes.

  12. Determination of ibuprofen and flurbiprofen in pharmaceuticals by capillary zone electrophoresis.

    Science.gov (United States)

    Hamoudová, Rafifa; Pospísilová, Marie

    2006-06-16

    Capillary zone electrophoresis with spectrophotometric detection was used for the determination of ibuprofen (IB) and flurbiprofen (FL) in pharmaceuticals. The separation was carried out in a fused silica capillary (60 cm x 100 microm i.d. effective length 45 cm) at 30 kV with UV detection at 232 nm. The optimized background electrolyte was 20mM N-(2-acetamido)-2-aminoethanesulfonic acid (ACES) with 20mM imidazole and 10mM alpha-cyclodextrin of pH 7.3. 2-Naphthoxyacetic acid was used as internal standard. A single analysis took less than 5 min. Rectilinear calibration ranges were 2-500 mg l(-1) for IB and 1-60 mg l(-1) for FL. The relative standard deviations (R.S.D.) values (n=6) were 1.53% for IB and 1.29% for FL (for 200 mg l(-1) IB and 10 mg l(-1) FL). This validated method has been successfully applied for the routine analysis of 10 commercially available pharmaceutical preparations (syrup, tablets, cream and gel).

  13. Sol-gel methyl coating in capillary microextraction hyphenated on-line with high-performance liquid chromatography Counterintuitive extraction behavior for polar analytes.

    Science.gov (United States)

    Segro, Scott S; Malik, Abdul

    2008-07-18

    A sol-gel coating with anchored methyl groups was developed for capillary microextraction hyphenated on-line with high-performance liquid chromatography (HPLC). This was accomplished by using methyltrimethoxysilane as the sol-gel precursor. The methyl group on the sol-gel precursor ultimately turned into a pendant group on the created sol-gel coating and was primarily responsible for the extraction of nonpolar analytes. A 40-cm segment of 0.25mm I.D. fused silica capillary containing the sol-gel methyl coating on the inner surface was installed as a sampling loop in an HPLC injection port. The analytes were extracted by the coating when an aqueous sample containing the analytes was passed through this capillary. The extracted analytes were then transferred to the HPLC column using isocratic elution with an acetonitrile/water mobile phase. This capillary demonstrated excellent extraction capability for polycyclic aromatic hydrocarbons and ketones. Unexpectedly, this coating also provided good extraction for polar analytes, including aromatic phenols, alcohols, and amines. Considering the fact that the methyl group is nonpolar in nature, such an extraction behavior of sol-gel methyl coating toward polar analytes is counterintuitive. Thus, sol-gel sorbents with short alkyl side chains have the potential to offer a polymer-free alternative to traditional sol-gel capillary microextraction (CME) media commonly prepared with the use of polymers in the sol solution. Elimination of polymers from the sol-gel coating solution is conducive to improving thermal stability and solvent tolerance of the created sol-gel extracting phase. This also makes the preparation of sol-gel coatings facile and cost-effective. Possessing excellent solvent stability, such sol-gel coatings offer the opportunity for effective on-line hyphenation of capillary microextraction with HPLC and other liquid-phase separation techniques that employ organo-aqueous mobile phases.

  14. Polymethacrylate monolithic and hybrid particle-monolithic columns for reversed-phase and hydrophilic interaction capillary liquid chromatography.

    Science.gov (United States)

    Jandera, Pavel; Urban, Jirí; Skeríková, Veronika; Langmaier, Pavel; Kubícková, Romana; Planeta, Josef

    2010-01-01

    We prepared hybrid particle-monolithic polymethacrylate columns for micro-HPLC by in situ polymerization in fused silica capillaries pre-packed with 3-5microm C(18) and aminopropyl silica bonded particles, using polymerization mixtures based on laurylmethacrylate-ethylene dimethacrylate (co)polymers for the reversed-phase (RP) mode and [2-(methacryloyloxy)ethyl]-dimethyl-(3-sulfopropyl) zwitterionic (co)polymers for the hydrophilic interaction (HILIC) mode. The hybrid particle-monolithic columns showed reduced porosity and hold-up volumes, approximately 2-2.5 times lower in comparison to the pure monolithic columns prepared in the whole volume of empty capillaries. The elution volumes of sample compounds are also generally lower in comparison to packed or pure monolithic columns. The efficiency and permeability of the hybrid columns are intermediate in between the properties of the reference pure monolithic and particle-packed columns. The chemistries of the embedded solid particles and of the interparticle monolithic moiety in the hybrid capillary columns contribute to the retention to various degrees, affecting the selectivity of separation. Some hybrid columns provided improved separations of proteins in comparison to the reference particle-packed columns in the reversed-phase mode. Zwitterionic hybrid particle-monolithic columns show dual mode retention HILIC/RP behaviour depending on the composition of the mobile phase and allow separations of polar compounds such as phenolic acids in the HILIC mode at lower concentrations of acetonitrile and, often in shorter analysis time in comparison to particle-packed and full-volume monolithic columns.

  15. Capillary electrophoresis for the assay of fixed-dose combination tablets of artesunate and amodiaquine

    Directory of Open Access Journals (Sweden)

    Amin N’Cho

    2012-05-01

    Full Text Available Abstract Background Quality control of drugs in formulations is still a major challenge in developing countries. For the quality control of artesunate and amodiaquine tablets in fixed-dose combination, only liquid chromatographic methods have been proposed in the literature. There are no capillary electrophoretic methods reported for the determination of these active substances, although this technique presents several advantages over liquid chromatography (long lifetime, low price of the capillary, low volumes of electrolyte consumption in addition to simplicity. In this paper, a reliable capillary electrophoresis method has been developed and validated for the quality control of these drugs in commercial fixed-dose combination tablets. Methods Artesunate and amodiaquine hydrochloride in bilayer tablets were determined by micellar electrokinetic capillary chromatography (MEKC. Analytes were extracted from tablets by sonication with a solvent mixture phosphate buffer pH 7.0-acetonitrile containing benzoic acid as internal standard. Separation was carried out on Beckman capillary electrophoresis system equipped with fused silica capillary, 30 cm long (20 cm to detector × 50 μm internal diameter, using a 25 mM borate buffer pH 9.2 containing 30 mM sodium dodecyl sulfate as background electrolyte, a 500 V cm−1 electric field and a detection wavelength of 214 nm. Results Artesunate, amodiaquine and benzoic acid were separated in 6 min. The method was found to be reliable with respect to specificity,linearity of the calibration line (r2 > 0.995, recovery from synthetic tablets (in the range 98–102%, repeatability (RSD 2–3%, n = 7 analytical procedures. Application to four batches of commercial formulations with different dosages gave content in good agreement with the declared content. Conclusion The MEKC method proposed is reliable for the determination of artesunate and amodiaquine hydrochloride in fixed

  16. Sol-gel approach to in situ creation of high pH-resistant surface-bonded organic-inorganic hybrid zirconia coating for capillary microextraction (in-tube SPME).

    Science.gov (United States)

    Alhooshani, Khalid; Kim, Tae-Young; Kabir, Abuzar; Malik, Abdul

    2005-01-07

    A novel zirconia-based hybrid organic-inorganic sol-gel coating was developed for capillary microextraction (CME) (in-tube SPME). High degree of chemical inertness inherent in zirconia makes it very difficult to covalently bind a suitable organic ligand to its surface. In the present work, this problem was addressed from a sol-gel chemistry point of view. Principles of sol-gel chemistry were employed to chemically bind a hydroxy-terminated silicone polymer (polydimethyldiphenylsiloxane, PDMDPS) to a sol-gel zirconia network in the course of its evolution from a highly reactive alkoxide precursor undergoing controlled hydrolytic polycondensation reactions. A fused silica capillary was filled with a properly designed sol solution to allow for the sol-gel reactions to take place within the capillary for a predetermined period of time (typically 15-30 min). In the course of this process, a layer of the evolving hybrid organic-inorganic sol-gel polymer got chemically anchored to the silanol groups on the capillary inner walls via condensation reaction. At the end of this in-capillary residence time, the unbonded part of the sol solution was expelled from the capillary under helium pressure, leaving behind a chemically bonded sol-gel zirconia-PDMDPS coating on the inner walls. Polycyclic aromatic hydrocarbons, ketones, and aldehydes were efficiently extracted and preconcentrated from dilute aqueous samples using sol-gel zirconia-PDMDPS coated capillaries followed by thermal desorption and GC analysis of the extracted solutes. The newly developed sol-gel hybrid zirconia coatings demonstrated excellent pH stability, and retained the extraction characteristics intact even after continuous rinsing with a 0.1 M NaOH solution for 24 h. To our knowledge, this is the first report on the use of a sol-gel zirconia-based hybrid organic-inorganic coating as an extraction medium in solid phase microextraction (SPME).

  17. Fluorescent polymer coated capillaries as optofluidic refractometric sensors.

    Science.gov (United States)

    Rowland, Kristopher J; François, Alexandre; Hoffmann, Peter; Monro, Tanya M

    2013-05-06

    A capillary microresonator platform for refractometric sensing is demonstrated by coating the interior of thick-walled silica capillaries with a sub-wavelength layer of high refractive index, dye-doped polymer. No intermediate processing, such as etching or tapering, of the capillary is required. Side illumination and detection of the polymer layer reveals a fluorescence spectrum that is periodically modulated by whispering gallery mode resonances within the layer. Using a Fourier technique to calculate the spectral resonance shifts, the fabricated capillary resonators exhibited refractometric sensitivities up to approximately 30 nm/RIU upon flowing aqueous glucose through them. These sensors could be readily integrated with existing biological and chemical separation platforms such as capillary electrophoresis and gas chromatography where such thick walled capillaries are routinely used with polymer coatings. A review of the modelling required to calculate whispering gallery eigenmodes of such inverted cylindrical resonators is also presented.

  18. Capillary electrophoresis procedure for the simultaneous analysis and stoichiometry determination of a drug and its counter-ion by using dual-opposite end injection and contactless conductivity detection: application to labetalol hydrochloride.

    Science.gov (United States)

    Nehmé, Reine; Lascaux, Adrien; Delépée, Raphaël; Claude, Bérengère; Morin, Philippe

    2010-03-24

    In this work, a capillary electrophoresis (CE) procedure was developed for the simultaneous determination of a pharmaceutical drug and its counter-ion, namely labetalol hydrochloride. For this purpose, an uncoated fused-silica capillary, a low conductivity background electrolyte (BGE) and a capacitively coupled contactless conductivity detector (C(4)D) were employed. This detection system is highly sensitive and enables detection of inorganic as well as organic ions unlike with direct UV detection. Moreover, to be able to simultaneously analyze the cationic drug (labetalol(+)) and its anionic counter-ion (Cl(-)) in the same electrophoretic run without the need of a coated capillary, a dual-opposite end injection was performed. In this technique, the sample is hydrodynamically injected into both ends of the capillary. This method is simple and easy to perform since the different injection steps are automated by the CE software. This novel CE-C(4)D procedure with dual-opposite end injection has been successfully validated and applied for the analysis of chloride content in an adrenergic antagonist (labetalol hydrochloride). Thus, the hereby developed method has been shown to enable fast (analysis time<10 min), precise (repeatability of migration times<0.7% and of corrected-peak areas < 3.3%; n=6) and rugged analyses for the simultaneous determination of a pharmaceutical drug and its counter-ion. Copyright 2010 Elsevier B.V. All rights reserved.

  19. Combining ligation reaction and capillary gel electrophoresis to obtain reliable long DNA probes.

    Science.gov (United States)

    García-Cañas, Virginia; Mondello, Monica; Cifuentes, Alejandro

    2011-05-01

    New DNA amplification methods are continuously developed for sensitive detection and quantification of specific DNA target sequences for, e.g. clinical, environmental or food applications. These new applications often require the use of long DNA oligonucleotides as probes for target sequences hybridization. Depending on the molecular technique, the length of DNA probes ranges from 40 to 450 nucleotides, solid-phase chemical synthesis being the strategy generally used for their production. However, the fidelity of chemical synthesis of DNA decreases for larger DNA probes. Defects in the oligonucleotide sequence result in the loss of hybridization efficiency, affecting the sensitivity and selectivity of the amplification method. In this work, an enzymatic procedure has been developed as an alternative to solid-phase chemical synthesis for the production of long oligonucleotides. The enzymatic procedure for probe production was based on ligation of short DNA sequences. Long DNA probes were obtained from smaller oligonucleotides together with a short sequence that acts as bridge stabilizing the molecular complex for DNA ligation. The ligation reactions were monitored by capillary gel electrophoresis with laser-induced fluorescence detection (CGE-LIF) using a bare fused-silica capillary. The capillary gel electrophoresis-LIF method demonstrated to be very useful and informative for the characterization of the ligation reaction, providing important information about the nature of some impurities, as well as for the fine optimization of the ligation conditions (i.e. ligation cycles, oligonucleotide and enzyme concentration). As a result, the yield and quality of the ligation product were highly improved. The in-lab prepared DNA probes were used in a novel multiplex ligation-dependent genome amplification (MLGA) method for the detection of genetically modified maize in samples. The great possibilities of the whole approach were demonstrated by the specific and sensitive

  20. Interactions of helquats with chiral acidic aromatic analytes investigated by partial-filling affinity capillary electrophoresis.

    Science.gov (United States)

    Růžička, Martin; Koval, Dušan; Vávra, Jan; Reyes-Gutiérrez, Paul E; Teplý, Filip; Kašička, Václav

    2016-10-07

    Noncovalent molecular interactions between helquats, a new class of dicationic helical extended diquats, and several chiral acidic aromatic drugs and catalysts have been investigated using partial-filling affinity capillary electrophoresis (PF-ACE). Helquats dissolved at 1mM concentration in the aqueous background electrolyte (40mM Tris, 20mM acetic acid, pH 8.1) were introduced as ligand zones of variable length (0-130mm) into the hydroxypropylcellulose coated fused silica capillary whereas 0.1mM solutions of negatively charged chiral drugs or catalysts (warfarin, ibuprofen, mandelic acid, etodolac, binaphthyl phosphate and 11 other acidic aromatic compounds) were applied as a short analyte zone at the injection capillary end. After application of electric field, analyte and ligand migrated against each other and in case of their interactions, migration time of the analyte was increasing with increasing length of the ligand zone. From the tested compounds, only isomers of those exhibiting helical chirality and/or possessing conjugated aromatic systems were enantioselectively separated through their differential interactions with helquats. Some compounds with conjugated aromatic groups interacted with helquats moderately strongly but non-enantiospecifically. Small compounds with single benzene ring exhibited no or very weak non-enantiospecific interactions. PF-ACE method allowed to determine binding constants of the analyte-helquat complexes from the changes of migration times of the analytes. Binding constants of the weakest complexes of the analytes with helquats were less than 50L/mol, whereas binding constants of the strongest complexes were in the range 1 000-1 400L/mol.

  1. The distribution of subsurface damage in fused silica

    Energy Technology Data Exchange (ETDEWEB)

    Miller, P E; Suratwala, T I; Wong, L L; Feit, M D; Menapace, J A; Davis, P J; Steele, R A

    2005-11-21

    Managing subsurface damage during the shaping process and removing subsurface damage during the polishing process is essential in the production of low damage density optical components, such as those required for use on high peak power lasers. Removal of subsurface damage, during the polishing process, requires polishing to a depth which is greater than the depth of the residual cracks present following the shaping process. To successfully manage, and ultimately remove subsurface damage, understanding the distribution and character of fractures in the subsurface region introduced during fabrication process is important. We have characterized the depth and morphology of subsurface fractures present following fixed abrasive and loose abrasive grinding processes. At shallow depths lateral cracks and an overlapping series of trailing indentation fractures were found to be present. At greater depths, subsurface damage consists of a series of trailing indentation fractures. The area density of trailing fractures changes as a function of depth, however the length and shape of individual cracks remain nearly constant for a given grinding process. We have developed and applied a model to interpret the depth and crack length distributions of subsurface surface damage in terms of key variables including abrasive size and load.

  2. Measurement of nitrosodimethylamine by capillary gas chromatography-mass spectrometry with the /sup 15/N-labelled compound as an internal standard

    Energy Technology Data Exchange (ETDEWEB)

    Kosaka, H.; Uozumi, M.; Nakajima, T.

    1984-01-01

    Artifactual formation of N-nitrosodimethylamine during the extraction procedure from aminopyrine and nitrite was examined. The use of the basic pH condition was the most effective in preventing artifactual formation. Sulfamic acid or ascorbic acid was partially effective in preventing artifactual formation. Since significant losses of volatile N-nitrosodimethylamine occur during the extraction and concentration steps, N-nitrosodimethylamine was analyzed by combined gas chromatography mass spectrometry with /sup 15/N-nitrosodimethylamine as an internal standard. The use of a fused silica capillary column enabled us to obtain a fine separation of the chromatogram. This methodology was applied to our model experiment, which was performed to locate the formation of N-nitrosodimethylamine when a rabbit was exposed to NO/sub 2/ after the administration of aminopyrine. SO/sub 3/ inhaled together with NO/sub 2/ was found to increase the nitrosation.

  3. Leukocytes in capillary flow.

    Science.gov (United States)

    Schmid-Schönbein, G W; Lee, J

    1995-01-01

    During disease, the flow of blood cells through the capillary network is one of the most perilous events in the microcirculation. Capillary distensibility, cytoplasmic activity of endothelial cells, red cells and leukocytes play an important role in capillary perfusion. Occlusion of capillaries is one of the early signs of vascular failure and is encountered in many different conditions and organs. Adhesion of leukocytes to the endothelium via expression of membrane adhesion molecules leads to microvascular entrapment with capillary occlusion.

  4. Silica Nephropathy

    Directory of Open Access Journals (Sweden)

    N Ghahramani

    2010-06-01

    Full Text Available Occupational exposure to heavy metals, organic solvents and silica is associated with a variety of renal manifestations. Improved understanding of occupational renal disease provides insight into environmental renal disease, improving knowledge of disease pathogenesis. Silica (SiO2 is an abundant mineral found in sand, rock, and soil. Workers exposed to silica include sandblasters, miners, quarry workers, masons, ceramic workers and glass manufacturers. New cases of silicosis per year have been estimated in the US to be 3600–7300. Exposure to silica has been associated with tubulointerstitial disease, immune-mediated multisystem disease, chronic kidney disease and end-stage renal disease. A rare syndrome of painful, nodular skin lesions has been described in dialysis patients with excessive levels of silicon. Balkan endemic nephropathy is postulated to be due to chronic intoxication with drinking water polluted by silicates released during soil erosion. The mechanism of silica nephrotoxicity is thought to be through direct nephrotoxicity, as well as silica-induced autoimmune diseases such as scleroderma and systemic lupus erythematosus. The renal histopathology varies from focal to crescentic and necrotizing glomerulonephritis with aneurysm formation suggestive of polyarteritis nodosa. The treatment for silica nephrotoxicity is non-specific and depends on the mechanism and stage of the disease. It is quite clear that further research is needed, particularly to elucidate the pathogenesis of silica nephropathy. Considering the importance of diagnosing exposure-related renal disease at early stages, it is imperative to obtain a thorough occupational history in all patients with renal disease, with particular emphasis on exposure to silica, heavy metals, and solvents.

  5. Simultaneous determination of the beta-blocker atenolol and several complementary antihypertensive agents in pharmaceutical formulations and urine by capillary zone electrophoresis.

    Science.gov (United States)

    Maguregui, M I; Jiménez, R M; Alonso, R M

    1998-10-01

    A simple capillary zone electrophoresis method is developed for the quantitation of the beta-blocker atenolol and the complementary antihypertensive agents bendroflumethiazide, amiloride, and hydrochlorothiazide in human urine samples. The electrophoretic separation is performed using a 78-cm x 75-micron-i.d. (70-cm effective length) fused-silica capillary. A borate buffer (pH 9) is used as running electrolyte. The sample is hydrostatically introduced for 20 s, and the running voltage is 25 kV at the injector end of the capillary. The analysis of urine samples requires the optimization of solid-phase extraction methods, achieving recoveries > or = 61% for all the drugs and good separation from the urine matrix. The method is successfully applied to the determination of these compounds in pharmaceutical formulations and in urine samples collected after the intake of Neatenol Diu (100 mg atenolol-5 mg bendroflumethiazide) and Kalten (50 mg atenolol-25 mg hydrochlorothiazide-2.5 mg amiloride). The method is validated in terms of reproducibility, linearity, and accuracy.

  6. Determination of pyruvate and lactate as potential biomarkers of embryo viability in assisted reproduction by capillary electrophoresis with contactless conductivity detection.

    Science.gov (United States)

    Mádr, Aleš; Celá, Andrea; Klejdus, Bořivoj; Pelcová, Marta; Crha, Igor; Žáková, Jana; Glatz, Zdeněk

    2015-06-01

    Human-assisted reproduction is increasing in importance due to the constantly rising number of couples suffering from infertility issue. A key step in in vitro fertilization is the proper assessment of embryo viability in order to select the embryo with the highest likelihood of resulting in a pregnancy. This study proposes a method based on CE with contactless conductivity detection for the determination of pyruvate and lactate in spent culture media used in human-assisted reproduction. A fused-silica capillary of 64.0 cm total length and 50 μm inner diameter was used. The inner capillary wall was modified by the coating of successive layers of the ionic polymers polybrene and dextran sulfate to reverse EOF. The BGE was composed of 10 mM MES/lithium hydroxide, pH 6.50. The sample was injected by pressure 50 mbar for 18 s, separation voltage was set to -24 kV, and capillary temperature to 15°C. The presented method requires only 2 μL of the culture medium, with LODs for pyruvate and lactate of 0.03 and 0.02 μM, respectively. The results demonstrated the method's suitability for the analysis of spent culture media to support embryo viability assessment by light microscopy, providing information about key metabolites of the energy metabolism of a developing embryo.

  7. Simultaneous determination of six toxic alkaloids in human plasma and urine using capillary zone electrophoresis coupled to time-of-flight mass spectrometry.

    Science.gov (United States)

    Yu, Zhuhong; Wu, Zhongping; Gong, Feijun; Wong, Rong; Liang, Chen; Zhang, Yurong; Yu, Yunqiu

    2012-10-01

    A novel capillary zone electrophoresis separation coupled to electro spray ionization time-of-flight mass spectrometry method was developed for the simultaneous analysis of six toxic alkaloids: brucine, strychnine, atropine sulfate, anisodamine hydrobromide, scopolamine hydrobromide and anisodine hydrobromide in human plasma and urine. To obtain optimal sensitivity, a solid-phase extraction method using Oasis MCX cartridges (1 mL, 30 mg; Waters, USA) for the pretreatment of samples was used. All compounds were separated by capillary zone electrophoresis at 25 kV within 12 min in an uncoated fused-silica capillary of 75 μm id × 100 cm and were detected by time-of-flight mass spectrometry. This method was validated with regard to precision, accuracy, sensitivity, linear range, limit of detection (LOD), and limit of quantification (LOQ). In the plasma and urine samples, the linear calibration curves were obtained over the range of 0.50-100 ng/mL. The LOD and LOQ were 0.2-0.5 ng/mL and 0.5-1.0 ng/mL, respectively. The intra- and interday precision was better than 12% and 13%, respectively. Electrophoretic peaks could be identified by mass analysis.

  8. On-line immunoaffinity solid-phase extraction capillary electrophoresis mass spectrometry for the analysis of large biomolecules: a preliminary report.

    Science.gov (United States)

    Medina-Casanellas, Silvia; Benavente, Fernando; Giménez, Estela; Barbosa, José; Sanz-Nebot, Victoria

    2014-08-01

    The analysis of large biomolecules by on-line immunoaffinity solid-phase extraction capillary electrophoresis mass spectrometry (IA-SPE-CE-MS) remains unexplored because of the complex issues that need to be addressed. In this preliminary study, we used the human glycoprotein transferrin (Tf) as a model of a large biomolecule. First, we established by CE-UV a novel method compatible with IA-SPE-CE-MS, based on the use of a fused silica capillary coated with an anionic derivative of polyacrylamide (UltraTrol(TM) Dynamic Pre-Coat High Normal, HN) to prevent protein adsorption. The methodology allowed the detection of the most abundant Tf sialoforms. Repeatability studies demonstrated high stability of the coated capillaries, which was required for on-line immunoextraction and MS detection. IA-SPE-CE-UV and IA-SPE-CE-MS methods were optimized for the analysis of Tf standards and human serum samples using a laboratory-made IA sorbent. Three peaks corresponding to Tf were detected with UV detection when on-line immunoextraction was applied to the standards. The use of MS detection, however, reduced the resolution of the electrophoretic separation. Finally, we demonstrated that it was possible to detect Tf in human serum samples, after off-line serum sample de-salting by centrifugal filtration.

  9. Determination of anions using monolithic capillary column ion chromatography with end-to-end differential contactless conductometric detectors under resonance approach.

    Science.gov (United States)

    Zhang, Zhenli; Li, Dongdong; Liu, Xueyong; Subhani, Qamar; Zhu, Yan; Kang, Qi; Shen, Dazhong

    2012-06-21

    An end-to-end differential measurement approach with capacitively coupled contactless conductivity detection (C(4)D) was applied to anion-exchange monolithic capillary column ion chromatography. The column was prepared by thermally initiated radical polymerization of poly(glycidyl methacrylate) in a fused-silica capillary of 320 μm i.d. and modified by quaternary ammonium latex surface coating. Two C(4)Ds were placed near both ends of the capillary column and the output difference between them was measured. With 15 mM potassium hydrogen phthalate used as the eluent, good separation of a mixture of inorganic anions (F(-), Cl(-), NO(2)(-), NO(3)(-)) was achieved. The detection limits of conventional C(4)D are 1.6, 0.28, 0.53, and 0.47 mg L(-1) for F(-), Cl(-), NO(2)(-), and NO(3)(-), respectively. To further enhance the sensitivity, the capacitive impedance from C(4)D was neutralized by an inductive impedance from a piezoelectric resonator. An increase in sensitivity by a factor of 7-8 was achieved in the resonating C(4)D in comparison with the conventional C(4)D. The detection limits of the resonating C(4)D are 0.23, 0.041, 0.065, and 0.059 mg L(-1) for F(-), Cl(-), NO(2)(-), and NO(3)(-), respectively. The response of the resonating C(4)D was analyzed based on an equivalent circuit model.

  10. Infrared spectra of silica polymorphs

    Science.gov (United States)

    Koike, C.; Noguchi, R.; Chihara, H.; Suto, H.; Ohtaka, O.; Imai, Y.; Matsumoto, T.; Tsuchiyama, A.

    The existence of silica within several debris disks has been suggested. We investigate the annealing conditions of α-cristobalite, and further prepare various types of silica, including α-cristobalite, α-quartz, coesite, stishovite, and fused quartz, which are natural, synthetic or commercial samples. We compare the results to previous studies and find that α-cristobalite synthesized at higher temperature than annealed silica. The interesting result of features similar to those of forsterite should be highlighted, where αcristobalite and coesite showed similar peaks at 16, 33, and 69 μm as forsterite. The 69 μm band for αcristobalite is especially very broad and strong, and shifts largely to a shorter wavelengths under cooling to low temperatures. The band for coesite, however, is very sharp, and shifts only a small amount to longer wavelengths under cooling to low temperatures. The peak positions of 16 and 69-μm band due to α-cristobalite can become index for temperature of silica dust. We discuss the possibility of silica detection around debris disks.

  11. Protein attachment onto silica surfaces--a survey of molecular fundamentals, resulting effects and novel preventive strategies in CE.

    Science.gov (United States)

    Stutz, Hanno

    2009-06-01

    This review addresses the fundamentals governing the adsorption of individual protein molecules onto the surface of fused-silica capillaries, the protein aggregation to adsorbate clusters and their final accretion to monolayers with subsequent stratification to protein multilayers. The attention in CE protein separation has primarily been focused on (i) tuning the BGE including the buffer type, ionic strength, pH and additives, (ii) tailored post-rinse procedures to detach adhered protein residues and (iii) the optimization of capillary wall shielding in order to reduce protein attachment. Improvements in protein separation as well as related adverse effects are mainly discussed on the basis of parameters known to become deteriorated in case of protein adhesion, e.g. repeatability of the EOF and of migration times, peak width, theoretical plate numbers, resolution and asymmetry factor. However, knowledge of the molecular principles controlling protein adsorption onto silica surfaces is indispensable for separation optimization. Furthermore, it facilitates troubleshooting and the interpretation of undesired concomitant phenomena. This review comprehensively discusses protein adsorption models derived from surface chemistry primarily in terms of their relevance for CE, clearly showing that the adsorption process in its complexity is only partially revealed by models, which address single or binary protein solutions. In a further section theoretical concepts and surface models are related to surface phenomena encountered in CE. The final part of the review surveys recent concepts for prevention of protein adhesion, thereby addressing capillary treatment, favorable buffer types, dynamic and adhesive semi-permanent coating strategies covering the literature from 2000-2008.

  12. [Separation of cefoperazone and its S-isomer and other related substances by micellar electrokinetic capillary chromatography].

    Science.gov (United States)

    Zhang, Huiwen; Hu, Changqin; Xu, Mingzhe; Li, Yaping; Hang, Taijun

    2007-09-01

    The separation of cefoperazone, its S-isomer, impurity A and other unknown related substances by micellar electrokinetic capillary chromatography (MECC) using sodium dodecyl sulphate (SDS) as the micellar phase was investigated. The effects of pH, concentration of phosphate buffer solution, SDS micelle concentration, methanol volume fraction, applied voltage and temperature on the separation were studied. It was found that the migration of these compounds was affected by these factors, especially by pH of the solution. The elution, as well as the migration time and separation efficiency of cefoperazone, its S-isomer, impurity A and other related substances changed with the acidity of the solution. The optimized separation conditions consisted of a running buffer of 70 mmol/L sodium phosphate buffer, at pH 6.5, containing 100 mmol/L SDS, with an applied voltage of 15 kV and a temperature of 25 degrees C. An uncoated fused-silica capillary of 51.0 cm x 75 microm (42.5 cm of effective length) was used. The sample was injected into the column by pressure (5 kPa) for 5 s. The detection wavelength was set at 254 nm. Twenty-eight impurities in cefoperazone sodium could be detected. Cefoperazone sodium and the degradation products could be separated well. The method was applied to separate and determine cefoperazone and its related substances successfully.

  13. Rapid "one-pot" preparation of polymeric monolith via photo-initiated thiol-acrylate polymerization for capillary liquid chromatography.

    Science.gov (United States)

    Bai, Jingyao; Wang, Hongwei; Ou, Junjie; Liu, Zhongshan; Shen, Yehua; Zou, Hanfa

    2016-06-21

    A facile approach was exploited for fast preparation of polymer-based monoliths in UV-transparent fused-silica capillaries via "one-pot" photo-initiated thiol-acrylate polymerization reaction of dipentaerythritolpenta-/hexaacrylate (DPEPA) and 1-octadecanethiol (ODT) in the presence of porogenic solvents (1-butanol and ethylene glycol). Due to relative insensitivity of oxygen inhibition in thiol-ene free-radical polymerization, the polymerization could be performed within 5 min. The effects of composition of prepolymerization solution on the morphology and permeability of poly(ODT-co-DPEPA) monoliths were investigated in detail by adjusting the content of monomer and binary porogen ratio. The physical properties of poly(ODT-co-DPEPA) monoliths were characterized by Fourier transform infrared spectroscopy (FT-IR), mercury intrusion porosimetry (MIP) and nitrogen adsorption/desorption measurement. The evaluation of chromatographic performance was carried out by capillary liquid chromatography (cLC). The results indicated that the poly(ODT-co-DPEPA) monolith was homogeneous and permeable, and also possessed a typical reversed-phase retention mechanism in cLC with high efficiency (∼75,000 N m(-1)) for separation of alkylbenzenes. Eventually, the further separation of tryptic digest of proteins by cLC tandem mass spectrometry (cLC-MS/MS) demonstrated its potential in the analysis of biological samples.

  14. Analysis of active alkaloids in the Menispermaceae family by nonaqueous capillary electrophoresis-ion trap mass spectrometry.

    Science.gov (United States)

    Chen, Qinhua; Zhang, Juan; Zhang, Wenpeng; Chen, Zilin

    2013-01-01

    A nonaqueous CE-IT MS with a nanospray ionization interface method was developed for the identification and quantification of tetrandrine (TET), fangchinoline (FAN), and sinomenine (SIN) using berberine as internal standard. The TET, FAN, and SIN standard solutions were directly infused into IT-MS for collecting MS(1-3) spectra. The major fragment ions of analytes were confirmed and possible main cleavage pathways of fragment ions were studied. A bare fused-silica capillary was used for separation of the analytes. A sheath liquid (50% aqueous methanol containing 0.2% acetic acid) to the capillary effluent with a nanoelectrospray ionization interface was added. Separation buffer comprised 80 mM solution of ammonium acetate, in a mixture of 70% methanol, 20% ACN, and 10% water, which also contained 1% acetic acid. The CE-MS method was validated for linearity, sensitivity, accuracy, and precision, and then used to determine the content of the above components. The detection limits of TET, FAN, and SIN are 0.05, 0.08, and 0.15 μg/mL, respectively. The precision was no more than 4.67% and the mean recovery of the analytes were 95.36-99.24%. This method was successfully applied to determine TET, FAN, and SIN in real samples radix Stephaniae tetrandrae and rhizomes of Menispermum dauricum.

  15. [Rapid determination of lactose, sucrose, glucose and fructose in foods by capillary zone electrophoresis with indirect ultraviolet detection].

    Science.gov (United States)

    Zhang, Huanhuan; Li, Jiang; Zhao, Shan; Ding, Xiaojing; Wang, Zhi

    2015-08-01

    A new and rapid method for the simultaneous determination of lactose, sucrose, glucose and fructose by capillary zone electrophoresis ( CZE) with indirect ultraviolet detection was developed. The separation was completed with an uncoated fused-silica capillary with 30.2 cm of total length (effective length of 20 cm) x 50 µm. The separation buffer consisted of 4 mmol/L potassium sorbate, 10 mmol/L sodium phosphate, 30 mmol/L NaOH (pH 12. 56) and 0. 5 mmol/L hexadecytrimethylammonium bromide (CTAB). The separation was performed at a voltage of -8 kV with the ultraviolet detection at 254 nm. The analysis of the four carbohydrates was completed within 10 min. The limits of detection (S/N= 3) for lactose, sucrose, glucose and fructose were 50, 75, 25 and 25 mg/L, and the limits of quantification (S/N = 10) were 150, 225, 75 and 75 mg/L, respectively. The average recoveries for the four carbohydrates were in the range of 87.0%-107.0% with the relative standard deviations of 1.2%-4.7%. No organic solvent was consumed throughout the whole process of the analysis. The method was used for the analysis of nine food samples and a quality control sample. The results demonstrated that the method is simple, rapid, accurate, and suitable for the routine analysis of the four carbohydrates in food samples.

  16. Separation and determination of strychnine and brucine in Strychnos nux-vomica L. and its preparation by nonaqueous capillary electrophoresis.

    Science.gov (United States)

    Li, Yuqin; He, Xiaojun; Qi, Shengda; Gao, Wenhua; Chen, Xingguo; Hu, Zhide

    2006-05-03

    An easy, rapid method for simultaneous determination of strychnine and brucine in Strychnos nux-vomica L. and its preparation was developed by nonaqueous capillary electrophoresis (NACE) without pretreatment for the first time. Optimum separation was achieved with a fused-silica capillary column (50 cmx75 microm i.d.) and a running buffer containing 30 mM ammonium acetate, 1.0% acetic acid and 15% acetonitrile (ACN) in methanol medium. The applied voltage was 30.0 kV. The analytes were detected by UV at 214 nm. The effects of concentration of ammonium acetate, acetic acid and organic modifier on electrophoretic behavior of the analytes were studied. The established method with sophoridine as internal standard was linear in the range of 5-1000 mg/mL for both strychnine and brucine. The extracts of Strychnos nux-vomica and its preparation could be directly injected for determination with recoveries ranging from 94.5 to 104%.

  17. Application of maltodextrin as chiral selector in capillary electrophoresis for quantification of amlodipine enantiomers in commercial tablets.

    Science.gov (United States)

    Nojavan, Saeed; Pourmoslemi, Shabnam; Behdad, Hamideh; Fakhari, Ali Reza; Mohammadi, Ali

    2014-08-01

    Maltodextrin was investigated as a chiral selector in capillary electrophoresis (CE) analysis of amlodipine (AM) enantiomers. For development of a stereoselective CE method, various effective parameters on the enantioseparation were optimized. The best results were achieved on an uncoated fused silica capillary at 20 °C using phosphate buffer (100 mM, pH 4) containing 10% w/v maltodextrin (dextrose equivalent value 4-7). The UV detector was set at 214 nm and a constant voltage of 20 kV was applied. The range of quantitation was 2.5-250 µg/mL (R(2)  > 0.999) for both enantiomers. Intra- (n = 5) and interday (n = 3) relative standard deviation (RSD) values were less than 7%. The limits of quantitation and detection were 1.7 µg/mL and 0.52 µg/mL, respectively. Recoveries of R(+) and S(-) enantiomers from tablet matrix were 97.2% and 97.8%, respectively. The method was applied for the quantification of AM enantiomers in commercial tablets. Also, the enantioseparation capability of heparin was evaluated and the results showed that heparin did not have any chiral selector activity in this study.

  18. Enantiomeric separation of 13 new amphetamine-like designer drugs by capillary electrophoresis, using modified-B-cyclodextrins.

    Science.gov (United States)

    Burrai, Lucia; Nieddu, Maria; Pirisi, Maria Antonietta; Carta, Antonio; Briguglio, Irene; Boatto, Gianpiero

    2013-10-01

    An easy-to-prepare chiral CE method for the enantiomeric separation of 13 new amphetamine-like designer drugs, using CDs as chiral selectors, was developed. Sulfated-β-CD was found to be the best chiral selector among the three used (sulfated-β-CD, caroboxymethyl-β-CD, dimethyl-β-CD). The separation of the analytes was achieved in a fused-silica gel capillary at 20 °C using an applied voltage of +25 kV. The optimized background electrolyte consisted of 63.5 mM H3 PO4 and 46.9 mM NaOH in water. Several electrophoretic parameters such as CD type, CD concentration (1 - 40 mg/mL), buffer pH (2.6, 3.6, 5.0, 6.0), length of the capillary (70 - 40 cm total length), amount of the organic solvent (methanol and acetonitrile) were investigated and optimized.

  19. Separation of oxalate, formate and glycolate in human body fluid samples by capillary electrophoresis with contactless conductometric detection.

    Science.gov (United States)

    Kubáň, Petr; Ďurč, Pavol; Bittová, Miroslava; Foret, František

    2014-01-17

    A new method for rapid determination of toxic metabolites after methanol and ethylene glycol intoxication - oxalate, formate and glycolate in various body fluid samples (blood serum, saliva, urine, exhaled breath condensate) by capillary electrophoresis with contactless conductometric detection was developed. A selective separation of the three target analytes from other constituents present in the analyzed biological matrices was achieved in less than 6min in a fused silica capillary of 25μm I.D. using an electrolyte comprising 50mM l-histidine and 50mM 2-(N-morpholino)ethanesulfonic acid at pH 6.1. The only sample preparation was dilution with deionized water. The limits of detection were 0.4, 0.6 and 1.3μM and limits of quantitation 1.3, 1.9 and 4.2μM for oxalate, formate and glycolate, respectively. The method provides a simple and rapid diagnostic test in suspected intoxication and is able to distinguish the ingested liquid, based on its metabolite trace. The method presents a fast screening tool that can be applicable in clinical practice.

  20. Separation and determination of four active anthraquinones in Chinese herbal preparations by flow injection-capillary electrophoresis.

    Science.gov (United States)

    Liu, Lihong; Fan, Liuyin; Chen, Hongli; Chen, Xingguo; Hu, Zhide

    2005-08-01

    A simple, rapid, and accurate method for the separation and determination of physcion, chrysophanol, aloe-emodin, and emodin in Rhubarb, Juemingzi, and Chinese herbal preparations was developed by combination of flow injection-capillary zone electrophoresis for the first time. The analysis was carried out using an unmodified fused-silica capillary (75 mm x 50 microm ID x 375 microm OD, effective separation length of 48 mm) and direct ultraviolet detection at 254 nm. By a series of optimization, the sample solvent consisted of NaOH (100 mmol/L) and ACN (1:1 v/v), and a running buffer composed of 15 mmol/L sodium borate - 12.5 mmol/L sodium dihydrogen phosphate - 42% v/v ACN (pH 10.1) was applied for the separation of the four anthraquinones. The separation was rapid and highly reproducible, with complete resolution of all four compounds within 6 min. The sample throughput rate could reach up to 12 per h. The repeatability (defined as relative standard deviation) was 4.45, 4.44, 4.34, 0.61% with peak height evaluation and 1.62, 0.89, 2.49, 2.19% with peak area evaluation for physcion, chrysophanol, aloe-emodin, and emodin, respectively.

  1. Sol-gel immobilized short-chain poly(ethylene glycol) coating for capillary microextraction of underivatized polar analytes.

    Science.gov (United States)

    Kulkarni, Sameer; Shearrow, Anne M; Malik, Abdul

    2007-12-07

    Sol-gel coating with covalently bonded low-molecular-weight (MWsol-gel chemistry proved effective in the immobilization of low-molecular-weight PEGs thanks to the formation of chemical bonds between the organic-inorganic hybrid sol-gel PEG coating and the fused silica capillary inner surface. This chemical anchorage provided excellent thermal and solvent stability to the created sol-gel PEG coating as is evidenced by its high upper limit of allowable conditioning temperature (340 degrees C) and its practically identical performance before and after rinsing with various solvents. The prepared sol-gel PEG coating provided simultaneous extraction of moderately polar and highly polar analytes from aqueous samples without requiring derivatization, pH adjustment or salting-out procedures. Detection limits on the order of nanogram per liter (ng/L) were achieved in CME-GC-flame ionization detection experiments designed for the preconcentration and trace analysis of both highly polar and moderately polar compounds extracted directly from aqueous media using sol-gel short-chain PEG coated microextraction capillaries.

  2. Analysis of the anti-Parkinson drug pramipexole in human urine by capillary electrophoresis with laser-induced fluorescence detection.

    Science.gov (United States)

    Musenga, Alessandro; Kenndler, Ernst; Morganti, Emanuele; Rasi, Fabrizio; Raggi, Maria Augusta

    2008-09-19

    A sensitive method based on capillary electrophoresis with laser-induced fluorescence detection has been developed for the analysis of the non-ergoline dopamine agonist pramipexole in human urine. Separation was carried out in uncoated fused silica capillaries (75microm internal diameter, 75.0 and 60.0cm total and effective length, respectively), with a background electrolyte composed of borate buffer (50mM, pH 10.3), tetrabutylammonium bromide (30mM), and acetone (15%, v/v). Applying a 20kV voltage, the electrophoretic run is completed within 12min. A sample pre-treatment procedure based on liquid/liquid extraction with ethyl acetate, followed by derivatisation of pramipexole with fluorescein isothiocyanate at pH 9, allows the complete removal of biological interferences, with extraction yields always higher than 94.5%. Method validation gave good linearity (r(2)=0.9992) in the 25.0-1000ngmL(-1) range; limit of detection and limit of quantitation were 10.0 and 25.0ngmL(-1), respectively; precision was 90.0. The method was applied to the analysis of urine samples from patients undergoing therapy with pramipexole.

  3. Electrophoretic analysis of biomarkers using capillary modification with gold nanoparticles embedded in a polycation and boron doped diamond electrode.

    Science.gov (United States)

    Zhou, Lin; Glennon, Jeremy D; Luong, John H T

    2010-08-15

    Field-amplified sample stacking using a fused silica capillary coated with gold nanoparticles (AuNPs) embedded in poly(diallyl dimethylammonium) chloride (PDDA) has been investigated for the electrophoretic separation of indoxyl sulfate, homovanillic acid (HVA), and vanillylmandelic acid (VMA). AuNPs (27 nm) exhibit ionic and hydrophobic interactions, as well as hydrogen bonding with the PDDA network to form a stable layer on the internal wall of the capillary. This approach reverses electro-osmotic flow allowing for fast migration of the analytes while retarding other endogenous compounds including ascorbic acid, uric acid, catecholamines, and indoleamines. Notably, the two closely related biomarkers of clinical significance, HVA and VMA, displayed differential interaction with PDDA-AuNPs which enabled the separation of this pair. The detection limit of the three analytes obtained by using a boron doped diamond electrode was approximately 75 nM, which was significantly below their normal physiological levels in biological fluids. This combined separation and detection scheme was applied to the direct analysis of these analytes and other interfering chemicals including uric and ascorbic acids in urine samples without off-line sample treatment or preconcentration.

  4. Fused-Polished Fiber Couplers

    Institute of Scientific and Technical Information of China (English)

    Sien; Chi; Shiao-Min; Tseng

    2003-01-01

    We report on fused-polished fiber couplers with a new fabrication method. This structure so fabricated is promising while achieving high-performance all-fiber WDM devices. Potential advantages and prospects of our works are presented.

  5. Ultra-high-stability, pH-resistant sol-gel titania poly(tetrahydrofuran) coating for capillary microextraction on-line coupled to high-performance liquid chromatography.

    Science.gov (United States)

    Segro, Scott S; Cabezas, Yaniel; Malik, Abdul

    2009-05-15

    A sol-gel titania poly(tetrahydrofuran) (poly-THF) coating was developed for capillary microextraction hyphenated on-line with high-performance liquid chromatography (HPLC). Poly-THF was covalently bonded to the sol-gel titania network which, in turn, became chemically anchored to the inner surface of a 0.25mm I.D. fused silica capillary. For sample preconcentration, a 38-cm segment of the sol-gel titania poly-THF coated capillary was installed on an HPLC injection port as a sampling loop. Aqueous samples containing a variety of analytes were passed through the capillary and, during this process, the analytes were extracted by the sol-gel titania poly-THF coating on the inner surface of the capillary. Using isocratic and gradient elution with acetonitrile/water mobile phases, the extracted analytes were desorbed into the on-line coupled HPLC column for separation and UV detection. The sol-gel titania poly-THF coating was especially efficient in extracting polar analytes, such as underivatized phenols, alcohols, amines, and aromatic carboxylic acids. In addition, this coating was capable of extracting moderately polar and nonpolar analytes, such as ketones and polycyclic aromatic hydrocarbons. The sol-gel titania poly-THF coated capillary was also able to extract polypeptides at pH values near their respective isoelectric points. Extraction of these compounds can be important for environmental and biomedical applications. The observed extraction behavior can be attributed to the polar and nonpolar moieties in the poly-THF structure. This coating was found to be stable under extremely low and high pH conditions-even after 18h of exposure to 1M HCl (pH approximately 0.0) and 1M NaOH (pH approximately 14.0).

  6. Capillary rise dynamics of liquid hydrocarbons in mesoporous silica as explored by gravimetry, optical and neutron imaging: Nano-rheology and determination of pore size distributions from the shape of imbibition fronts

    CERN Document Server

    Gruener, Simon; Schillinger, Burkhard; Egelhaaf, Stefan U; Huber, Patrick

    2015-01-01

    We present gravimetrical, optical, and neutron imaging measurements of the capillarity-driven infiltration of mesoporous silica glass by hydrocarbons. Square-root-of-time Lucas-Washburn invasion kinetics are found for linear alkanes from n-decane (C10) to n-hexacontane (C60) and for squalane, a branched alkane, in porous Vycor with 6.5 nm or 10 nm pore diameter, respectively. Humidity-dependent experiments allow us to study the influence on the imbibition kinetics of water layers adsorbed on the pore walls. Except for the longest molecule studied, C60, the invasion kinetics can be described by bulk fluidity and bulk capillarity, provided we assume a sticking, pore-wall adsorbed boundary layer, i.e. a monolayer of water covered by a monolayer of flat-laying hydrocarbons. For C60, however, an enhanced imbibition speed compared to the value expected in the bulk is found. This suggests the onset of velocity slippage at the silica walls or a reduced shear viscosity due to the transition towards a polymer-like flow...

  7. Thermal fatigue of electrical fuses

    Directory of Open Access Journals (Sweden)

    Gelet Jean-Louis

    2014-06-01

    Full Text Available Electric Fuses have to respect different national or international standards such as IEC (International Electro-technical Commission 269. These standards define the characteristics of the fuses and describe the tests to be run in order to check fuse's ability to take up their main functions, i.e. current-conduction and operation under overloads and short-circuits. But fuses never carry current neither operate under standardized conditions. For example, rated current is evaluated under specified ambient temperature, without cooling air-flow, and with 1 meter-long connection-cables on both sides. In the field, temperature can reach up 80∘C, with or without air-flow and connection-parts are much more shorter. An issue is that current is never constant, often being cyclingly applied; equipments are frequently in use during the day and stopped in the night. ON-time and OFF-time generate alternative heating, then alternative stresses leading to thermal fatigue. MERSEN run many tests along the years, allowing to develop a method for choosing right fuses for each application. As a result, fuses don't melt unexpectedly in the field, but the method is supposed to be conservative and does not permit to get a better understanding of the phenomena neither an improvement of the products. The paper presents some specific ageing-tests run on conductive elements and tries to establish a correspondence between these tests and others carried out on complete fuses. Tests have been run on silver and copper, but their principle could be interesting for any structural material, especially because it underlines crack-opening.

  8. Direct comparison of capillary electrophoresis and capillary liquid chromatography hyphenated to collision-cell inductively coupled plasma mass spectrometry for the investigation of Cd-, Cu- and Zn-containing metalloproteins.

    Science.gov (United States)

    Montes-Bayon, Maria; Pröfrock, Daniel; Sanz-Medel, Alfredo; Prange, Andreas

    2006-05-05

    Capillary liquid chromatography (cLC) and capillary electrophoresis (CE) have been critically compared for the separation of metalloproteins when using collision-cell inductively coupled plasma mass spectrometry (ICP-CC-MS) as detection system. For cLC separation, the selected column was a C8 (0.3 mm I.D.) and the separation conditions involved a gradient up to 80% methanol in 10mM ammonium acetate buffer (pH 7.4). The low flow rate used (3 microL min(-1)) permitted the utilization of a high methanol content maintaining the sensitivity along the whole chromatographic run. For this purpose, a new low-flow interface has been developed based on a total consumption nebulizer. Similarly, CE has been studied as separation technique using a 75 microm I.D. fused silica capillary and a running buffer of 20 mM Tris-HNO3 (pH 7.4) and working at 30 kV. Metallothionein (mixture of MT-I and -II) and superoxide dismutase (SOD) have been used as protein models in order to evaluate the separation/detection capabilities using the same injection volumes in both systems (20 nL). For both hybrid systems, separation parameters such as retention factor, numbers of theoretical plates, tailing factor and resolution have been critically compared. Also, the analytical performance characteristics of both hybrid systems have been evaluated and tested by analyzing the Cu-, Zn-species present in red blood cell extracts in order to explore more adequate separation methodology for the analysis of metalloproteins in complex matrices.

  9. Performance and characteristics of a high pressure, high temperature capillary cell with facile construction for operando x-ray absorption spectroscopy.

    Science.gov (United States)

    Bansode, Atul; Guilera, Gemma; Cuartero, Vera; Simonelli, Laura; Avila, Marta; Urakawa, Atsushi

    2014-08-01

    We demonstrate the use of commercially available fused silica capillary and fittings to construct a cell for operando X-ray absorption spectroscopy (XAS) for the study of heterogeneously catalyzed reactions under high pressure (up to 200 bars) and high temperature (up to 280 °C) conditions. As the first demonstration, the cell was used for CO2 hydrogenation reaction to examine the state of copper in a conventional Cu/ZnO/Al2O3 methanol synthesis catalyst. The active copper component of the catalyst was shown to remain in the metallic state under supercritical reaction conditions, at 200 bars and up to 260 °C. With the coiled heating system around the capillary, one can easily change the length of the capillary and control the amount of catalyst under investigation. With precise control of reactant(s) flow, the cell can mimic and serve as a conventional fixed-bed micro-reactor system to obtain reliable catalytic data. This high comparability of the reaction performance of the cell and laboratory reactors is crucial to gain insights into the nature of actual active sites under technologically relevant reaction conditions. The large length of the capillary can cause its bending upon heating when it is only fixed at both ends because of the thermal expansion. The degree of the bending can vary depending on the heating mode, and solutions to this problem are also presented. Furthermore, the cell is suitable for Raman studies, nowadays available at several beamlines for combined measurements. A concise study of CO2 phase behavior by Raman spectroscopy is presented to demonstrate a potential of the cell for combined XAS-Raman studies.

  10. Efficient sample clean-up and online preconcentration for sensitive determination of melamine in milk samples by capillary electrophoresis with contactless conductivity detection.

    Science.gov (United States)

    Ji, Yan-ling; Chen, Xiao-wei; Zhang, Zhu-bao; Li, Jing; Xie, Tian-yao

    2014-10-01

    Based on an efficient sample clean-up and field-amplified sample injection online preconcentration technique in capillary electrophoresis with contactless conductivity detection, a new analytical method for the sensitive determination of melamine in milk samples was established. In order to remove the complex matrix interference, which resulted in a serious problem during field-amplified sample injection, liquid-liquid extraction was utilized. As a result, liquid-liquid extraction provides excellent sample clean-up efficiency when ethyl acetate was used as organic extraction by adjusting the pH of the sample solution to 9.5. Both inorganic salts and biological macromolecules are effectively removed by liquid-liquid extraction. The sample clean-up procedure, capillary electrophoresis separation parameters and field-amplified sample injection conditions are discussed in detail. The capillary electrophoresis separation was achieved within 5 min under the following conditions: an uncoated fused-silica capillary, 12 mM HAc + 10 mM NaAc (pH = 4.6) as running buffer, separation voltage of +13 kV, electrokinetic injection of +12 kV × 10 s. Preliminary validation of the method performance with spiked melamine provided recoveries >90%, with limits of detection and quantification of 0.015 and 0.050 mg/kg, respectively. The relative standard deviations of intra- and inter-day were below 6%. This newly developed method is sensitive and cost effective, therefore, suitable for screening of melamine contamination in milk products.

  11. Performance and characteristics of a high pressure, high temperature capillary cell with facile construction for operando x-ray absorption spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Bansode, Atul; Urakawa, Atsushi, E-mail: aurakawa@iciq.es [Institute of Chemical Research of Catalonia (ICIQ), Av. Països Catalans 16, 43007 Tarragona (Spain); Guilera, Gemma; Simonelli, Laura; Avila, Marta [ALBA Synchrotron Light Source, Crta. BP 1413, Km. 3.3, 08290 Cerdanyola del Vallès, Barcelona (Spain); Cuartero, Vera [ALBA Synchrotron Light Source, Crta. BP 1413, Km. 3.3, 08290 Cerdanyola del Vallès, Barcelona (Spain); European Synchrotron Radiation Facility (ESRF), CS40220, F-38043, Grenoble Cedex (France)

    2014-08-15

    We demonstrate the use of commercially available fused silica capillary and fittings to construct a cell for operando X-ray absorption spectroscopy (XAS) for the study of heterogeneously catalyzed reactions under high pressure (up to 200 bars) and high temperature (up to 280 °C) conditions. As the first demonstration, the cell was used for CO{sub 2} hydrogenation reaction to examine the state of copper in a conventional Cu/ZnO/Al{sub 2}O{sub 3} methanol synthesis catalyst. The active copper component of the catalyst was shown to remain in the metallic state under supercritical reaction conditions, at 200 bars and up to 260 °C. With the coiled heating system around the capillary, one can easily change the length of the capillary and control the amount of catalyst under investigation. With precise control of reactant(s) flow, the cell can mimic and serve as a conventional fixed-bed micro-reactor system to obtain reliable catalytic data. This high comparability of the reaction performance of the cell and laboratory reactors is crucial to gain insights into the nature of actual active sites under technologically relevant reaction conditions. The large length of the capillary can cause its bending upon heating when it is only fixed at both ends because of the thermal expansion. The degree of the bending can vary depending on the heating mode, and solutions to this problem are also presented. Furthermore, the cell is suitable for Raman studies, nowadays available at several beamlines for combined measurements. A concise study of CO{sub 2} phase behavior by Raman spectroscopy is presented to demonstrate a potential of the cell for combined XAS-Raman studies.

  12. Sweeping of alprenolol enantiomers with an organic solvent and sulfated β-cyclodextrin in capillary electrophoresis.

    Science.gov (United States)

    Rabanes, Heide R; Quirino, Joselito P

    2013-05-01

    Sweeping, an on-line sample concentration technique in CE, is the picking and accumulation of analytes by the pseudostationary phase or complexing additive. In the presence of an electric field, the analytes concentrated at the additive front that initially penetrated the sample zone. Here, we describe the sweeping of cationic alprenolol enantiomers using sulfated β-CD and organic solvent. The separation solution contained the anionic additive while ACN was in the sample solution. With fused silica capillaries, positive polarity, and solutions buffered at pH 3, the direction of the enantiomers' effective electrophoretic mobility was the same as the electrophoretic mobility (or electrophoretic mobility without additive). When the amount of ACN in the sample was increased (i.e. 60%), the interaction between the analytes and additive became negligible. This caused the sweeping boundary to shift from the electrophoretically moving β-CD front to the zone between the sample and separation solution. The equation that described the narrowing of injected sample zone was derived. The performance of sweeping with 60% ACN in the sample was then studied under different operating conditions (e.g. type of injection, injection time, and CD concentration). The low interaction between enantiomers and additive gave only moderate increases in sensitivity (approximately tenfold), but was improved when field enhancement was used during electrokinetic injection. With a conductivity difference (separation/sample solution) of 70 and a short injection time of 30 s at 20 kV, peak improvements of >100-fold was easily achieved.

  13. Online preconcentration of arsenic compounds by dynamic pH junction-capillary electrophoresis.

    Science.gov (United States)

    Jaafar, Jafariah; Irwan, Zildawarni; Ahamad, Rahmalan; Terabe, Shigeru; Ikegami, Tohru; Tanaka, Nobuo

    2007-02-01

    An online preconcentration technique by dynamic pH junction was studied to improve the detection limit for anionic arsenic compounds by CE. The main target compound is roxarsone, or 3-nitro-4-hydroxyphenylarsonic acid, which is being used as an animal feed additive. The other inorganic and organoarsenic compounds studied are the possible biotransformation products of roxarsone. The arsenic species were separated by a dynamic pH junction in a fused-silica capillary using 15 mM phosphate buffer (pH 10.6) as the BGE and 15 mM acetic acid as the sample matrix. CE with UV detection was monitored at a wavelength of 192 nm. The influence of buffer pH and concentration on dynamic pH junction were investigated. The arsenic species focusing resulted in LOD improvement by a factor of 100-800. The combined use of C18 and anion exchange SPE and dynamic pH junction to CE analysis of chicken litter and soils helps to increase the detection sensitivity. Recoveries of spiked samples ranged between 70 and 72%.

  14. Polydopamine-coated open tubular column for the separation of proteins by capillary electrochromatography.

    Science.gov (United States)

    Xiao, Xing; Wang, Wentao; Chen, Jia; Jia, Li

    2015-08-01

    The separation and determination of proteins in food is an important aspect in food industry. Inspired by the self-polymerization of dopamine under alkaline conditions and the natural adhesive properties of polydopamine, in this paper, a simple and economical method was developed for the preparation of polydopamine-coated open tubular column, in which ammonium persulfate was used as the source of oxygen to induce and facilitate the polymerization of dopamine to form polydopamine. In comparison with a naked fused-silica capillary, the direction and magnitude of the electro-osmotic flow of the as-prepared polydopamine-coated open tubular column could be manipulated by varying the pH values of background solutions due to the existence of amine and phenolic hydroxyl groups on polydopamine coating. The surface morphology of the polydopamine-coated open tubular column was studied by scanning electron microscopy, and the thickness of polydopamine coating was 106 nm. The performance of the polydopamine-coated open tubular column was validated by analysis of proteins. The relative standard deviations of migration times of proteins representing run-to-run, day-to-day, and column-to-column were less than 3.5%. In addition, the feasibility of the polydopamine-coated open tubular column for real samples was verified by the separation of proteins in chicken egg white and pure milk. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Determination of lipoic acid in human urine by capillary zone electrophoresis.

    Science.gov (United States)

    Kubalczyk, Paweł; Głowacki, Rafał

    2017-07-01

    Fast, simple, and accurate CE method enabling determination of lipoic acid (LA) in human urine has been developed and validated. LA is a disulfide-containing natural compound absorbed from the organism's diet. Due to powerful antioxidant activity, LA has been used for prevention and treatment of various diseases and disorders, e.g. cardiovascular diseases, neurodegenerative disorders, and cancer. The proposed analytical procedure consists of liquid-liquid sample extraction, reduction of LA with tris(2-carboxyethyl)phosphine, derivatization with 1-benzyl-2-chloropyridinium bromide (BCPB) followed by field amplified sample injection stacking, capillary zone electrophoresis separation, and ultraviolet-absorbance detection of LA-BCPB derivative at 322 nm. Effective baseline electrophoretic separation was achieved within 6 min under the separation voltage of 20 kV (∼80 μA) using a standard fused-silica capillary (effective length 51.5 cm, 75 μm id) and BGE consisted of 0.05 mol/L borate buffer adjusted to pH 9. The experimentally determined limit of detection for LA in urine was 1.2 μmol/L. The calibration curve obtained for LA in urine showed linearity in the range 2.5-80 μmol/L, with R(2) 0.9998. The relative standard deviation of the points of the calibration curve was lower than 10%. The analytical procedure was successfully applied to analysis of real urine samples from seven healthy volunteers who received single 100 mg dose of LA. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Sheath liquid effects in capillary high-performance liquid chromatography-electrospray mass spectrometry of oligonucleotides.

    Science.gov (United States)

    Huber, C G; Krajete, A

    2000-02-18

    Fused-silica capillary columns of 200 microm inner diameter were packed with micropellicular, octadecylated, 2.3 microm poly(styrene-divinylbenzene) particles and applied to the separation of oligonucleotides by ion-pair reversed-phase high-performance liquid chromatography. Oligonucleotides were eluted at 50 degrees C with gradients of 3-13% acetonitrile in 50 mM triethylammonium bicarbonate. Addition of sheath liquid to the column effluent allowed the detection of oligonucleotides by electrospray ionization mass spectrometry using full-scan data acquisition with a detectability comparable to that obtained with UV detection. The signal-to-noise ratios with different sheath liquids increased in the order isopropanolcapillary ion-pair reversed-phase high-performance liquid chromatography-electrospray ionization mass spectrometry was

  17. Simultaneous determination of paracetamol, caffeine and propyphenazone in ternary mixtures by micellar electrokinetic capillary chromatography.

    Science.gov (United States)

    Emre, Deniz; Ozaltin, Nuran

    2007-03-01

    A new micellar electrokinetic capillary chromatographic method has been developed to analyze the pharmaceutical preparations containing ternary combination of paracetamol (PAR), caffeine (CAF) and propyphenazone (PRO). Best results were obtained by using 20mM pH 9.0 borate buffer containing 30mM sodiumdodecylsulphate as the background electrolyte. Diflunisal (DIF) was used as internal standard (IS). The separation was performed through a fused silica capillary (50microm internal diameter, 44cm total length, 35.5cm effective length) at 25 degrees C with the application of 3s of hydrodynamic injection at 50mbar pressure and a potential of 29kV. Detection wavelength was 200nm. Under these conditions, the migration times were found to be 5.174min for PAR, 5.513min for CAF, 7.195min for DIF, and 9.366min for PRO. Linearity ranges for the method were determined as 2-200microgmL(-1) for PAR and CAF and 3-200microgmL(-1) for PRO. Limit of detections were found as 0.6microgmL(-1) for PAR and CAF and 0.8microgmL(-1) for PRO. According to the validation study, the developed method was proved to be accurate, precise, sensitive, specific, rugged and robust. Three pharmaceutical preparations, which are produced by different drug companies in Turkey, were analyzed by the developed method. One of the same preparations was also analyzed by the derivative ratio spectro zero-crossing spectrophotometric method reported in literature. No significant differences were found statistically.

  18. Liquefier Dynamics in Fused Deposition

    DEFF Research Database (Denmark)

    Bellini, Anna; Guceri, Selcuk; Bertoldi, Maurizio

    2004-01-01

    Layered manufacturing (LM) is an evolution of rapid prototyping (RP) technology whereby a part is built in layers. Fused deposition modeling (FDM) is a particular LM technique in which each section is fabricated through vector style deposition of building blocks, called roads, which...

  19. Optimization of capillary electrophoresis-inductively coupled plasma mass spectrometry for species analysis of metallothionein-like proteins extracted from liver tissues of Elbe-bream and Roe deer

    Energy Technology Data Exchange (ETDEWEB)

    Proefrock, Daniel; Prange, Andreas E-mail: andreas.prange@gkss.de; Schaumloeffel, Dirk; Ruck, Wolfgang

    2003-08-15

    Species analysis of metallothionein-like proteins (MLP) in liver tissues from Elbe-Bream (Abramis brama L.) and Roe Deer (Capreolus capreolus L.) using capillary electrophoresis (CE) combined with inductively coupled plasma mass spectrometry detection is described. In order to allow systematic development of the method, commercially available metallothionein (MT) preparations of rabbit liver were used. Optimum separation efficiency was obtained by investigating the influence of parameters such as voltage, capillary temperature, buffer concentration, buffer pH and the use of different buffer systems. Instrumental parameters such as CE capillary position, interface adjustment and contamination problems are also discussed. Separation was performed using uncoated fused silica capillaries with 75 {mu}m i.d. and 70 cm length. The optimum conditions were found to be: Separation voltage 30 kV, positive polarity, capillary temperature 288.15 K and a buffer concentration of 100 mmol l{sup -1} Tricine-NH{sub 3} adjusted to pH 7.2. Sample preparation was performed so as to minimize oxidation and heavy metal contamination of the samples. The high molecular mass protein matrix was reduced by acetonitrile precipitation. For commercial MT preparations the relative standard deviations (R.S.D) in the retention times were 0.9% for MT-1 and 1.9% for MT-2; the R.S.D.'s in the peak areas were less than 6% for MT-1 and 16% for MT-2, respectively. Under optimized conditions the MLPs in the real samples could be separated efficiently in less than 10 min. By comparison with the migration times of commercially available MT preparations, two of the observed peaks could be assigned to MT-1 and MT-2.

  20. Intramedullary capillary haemangioma.

    LENUS (Irish Health Repository)

    Kelleher, T

    2012-02-03

    Intramedullary capillary haemangioma is extremely rare and only four cases have been previously reported. We describe a further case, outlining the clinical, radiological, surgical and pathological features.

  1. High-sensitivity capillary electrophoresis method for monitoring purine nucleoside phosphorylase and adenosine deaminase reactions by a reversed electrode polarity switching mode.

    Science.gov (United States)

    Iqbal, Jamshed; Müller, Christa E

    2011-07-22

    A simple, efficient, and highly sensitive in-line CE method was developed for the characterization and for inhibition studies of the nucleoside-metabolizing enzymes purine nucleoside phosphorylase (PNP) and adenosine deaminase (ADA) present in membrane preparations of human 1539 melanoma cells. After filling the running buffer (50 mM borate buffer, 100 mM SDS, pH 9.10) into a fused-silica capillary (50 cm effective length × 75 μm), a large sample volume was loaded by hydrodynamic injection (5 psi, 36 s), followed by the removal of the large plug of sample matrix from the capillary using polarity switching (-20 kV). The current was monitored and the polarity was reversed when 95% of the current had been recovered. The separation of the neutral analytes (nucleosides and nucleobases) was performed by applying a voltage of 15 kV. An about 10-fold improvement of sensitivity for the five investigated analytes (adenosine, inosine, adenine, hypoxanthine, xanthine) was achieved by large-volume stacking with polarity switching when compared with CE without stacking. For inosine and adenine detection limits as low as 60 nM were achieved. To the best of our knowledge, this represents the highest sensitivity for nucleoside and nucleobase analysis using CE with UV detection reported so far. The Michaelis-Menten constants (K(m)) for PNP and ADA and the inhibition constants (K(i)) for standard inhibitors determined with the new method were consistent with literature data.

  2. Development and validation of a stability-indicating capillary zone electrophoretic method for the assessment of entecavir and its correlation with liquid chromatographic methods.

    Science.gov (United States)

    Dalmora, Sergio Luiz; Nogueira, Daniele Rubert; D'Avila, Felipe Bianchini; Souto, Ricardo Bizogne; Leal, Diogo Paim

    2011-01-01

    A stability-indicating capillary zone electrophoresis (CZE) method was validated for the analysis of entecavir in pharmaceutical formulations, using nimesulide as an internal standard. A fused-silica capillary (50 µm i.d.; effective length, 40 cm) was used while being maintained at 25°C; the applied voltage was 25 kV. A background electrolyte solution consisted of a 20 mM sodium tetraborate solution at pH 10. Injections were performed using a pressure mode at 50 mbar for 5 s, with detection at 216 nm. The specificity and stability-indicating capability were proven through forced degradation studies, evaluating also the in vitro cytotoxicity test of the degraded products. The method was linear over the concentration range of 1-200 µg mL(-1) (r(2) = 0.9999), and was applied for the analysis of entecavir in tablet dosage forms. The results were correlated to those of validated conventional and fast LC methods, showing non-significant differences (p > 0.05).

  3. Sub-minute method for simultaneous determination of aspartame, cyclamate, acesulfame-K and saccharin in food and pharmaceutical samples by capillary zone electrophoresis.

    Science.gov (United States)

    Vistuba, Jacqueline Pereira; Dolzan, Maressa Danielli; Vitali, Luciano; de Oliveira, Marcone Augusto Leal; Micke, Gustavo Amadeu

    2015-05-29

    This paper reports the development of a sub-minute separation method by capillary zone electrophoresis for the determination of aspartame, cyclamate, acesulfame-K and saccharin in food products and pharmaceutical samples. Separations were performed in a fused uncoated silica capillary with UV detection at 220nm. Samples and standards were injected hydrodynamically using the short-end injection procedure. The electrophoretic system was operated under constant voltage of -30kV. The background electrolyte was composed of 45mmolL(-1) 2-amino-2-(hydroxymethyl)-1,3-propanediol and 15mmolL(-1) benzoic acid at pH 8.4. The separation time for all analytes was less than 1min. Evaluation of analytical parameters of the method showed good linearity (r(2)>0.9972), limit of detection of 3.3-6.4mgL(-1), intermediate precision better than 9.75% (peak area of sample) and recovery in the range of 91-117%.

  4. Application of capillary electrophoresis-frontal analysis for comparative evaluation of the binding interaction of captopril with human serum albumin in the absence and presence of hydrochlorothiazide.

    Science.gov (United States)

    Liu, Ting-Ting; Xiang, Li-Li; Wang, Jian-Ling; Chen, Dong-Ying

    2015-11-10

    The application of capillary electrophoresis-frontal analysis for comparative evaluation of the binding interaction between antihypertensive drug captopril and human serum albumin in the absence and presence of diuretic drug hydrochlorothiazide was presented in this work. At near-physiological conditions (67mM phosphate buffer, pH 7.4, I=0.17, 37°C), the individual solution of 100μM captopril and the co-binding solution with 60μM hydrochlorothiazide added were pre-equilibrated with series concentrations of HSA (10-475μM) respectively, introducing hydrodynamically into an uncoated fused silica capillary (35cm×50μm I.D. with 26.5cm effective length). The values of number of binding sites, the binding constant for captopril and hydrochlorothiazide binding to HSA were obtained, respectively. It can be found that both drugs exhibit moderate binding properties towards HSA and there does not exist significant competitive binding effects between them. Copyright © 2015 Elsevier B.V. All rights reserved.

  5. Chromatographic selectivity of poly(alkyl methacrylate-co-divinylbenzene) monolithic columns for polar aromatic compounds by pressure-driven capillary liquid chromatography.

    Science.gov (United States)

    Lin, Shu-Ling; Wang, Chih-Chieh; Fuh, Ming-Ren

    2016-10-05

    In this study, divinylbenzene (DVB) was used as the cross-linker to prepare alkyl methacrylate (AlMA) monoliths for incorporating π-π interactions between the aromatic analytes and AlMA-DVB monolithic stationary phases in capillary LC analysis. Various AlMA/DVB ratios were investigated to prepare a series of 30% AlMA-DVB monolithic stationary phases in fused-silica capillaries (250-μm i.d.). The physical properties (such as porosity, permeability, and column efficiency) of the synthesized AlMA-DVB monolithic columns were investigated for characterization. Isocratic elution of phenol derivatives was first employed to evaluate the suitability of the prepared AlMA-DVB columns for small molecule separation. The run-to-run (0.16-1.20%, RSD; n = 3) and column-to-column (0.26-2.95%, RSD; n = 3) repeatabilities on retention times were also examined using the selected AlMA-DVB monolithic columns. The π-π interactions between the aromatic ring and the DVB-based stationary phase offered better recognition on polar analytes with aromatic moieties, which resulted in better separation resolution of aromatic analytes on the AlMA-DVB monolithic columns. In order to demonstrate the capability of potential environmental and/or food safety applications, eight phenylurea herbicides with single benzene ring and seven sulfonamide antibiotics with polyaromatic moieties were analyzed using the selected AlMA-DVB monolithic columns.

  6. On-Line Organic Solvent Field Enhanced Sample Injection in Capillary Zone Electrophoresis for Analysis of Quetiapine in Beagle Dog Plasma.

    Science.gov (United States)

    Cao, Yuqing; Wen, Jun; Zhou, Tingting; Fan, Guorong

    2016-01-21

    A rapid and sensitive capillary zone electrophoresis (CZE) method with field enhanced sample injection (FESI) was developed and validated for the determination of quetiapine fumarate in beagle dog plasma, with a sample pretreatment by LLE in 96-well deep format plate. The optimum separation was carried out in an uncoated 31.2 cm × 75 μm fused-silica capillary with an applied voltage of 13 kV. The electrophoretic analysis was performed by 50 mM phosphate at pH 2.5. The detection wavelength was 210 nm. Under these optimized conditions, FESI with acetonitrile enhanced the sensitivity of quetiapine about 40-50 folds in total. The method was suitably validated with respect to stability, specificity, linearity, lower limit of quantitation, accuracy, precision and extraction recovery. Using mirtazapine as an internal standard (100 ng/mL), the response of quetiapine was linear over the range of 1-1000 ng/mL. The lower limit of quantification was 1 ng/mL. The intra- and inter-day precisions for the assay were within 4.8% and 12.7%, respectively. The method represents the first application of FESI-CZE to the analysis of quetiapine fumarate in beagle dog plasma after oral administration.

  7. Elution behavior of lambda-DNA with ternary mixed carrier solvents in an open-tubular capillary under laminar flow conditions.

    Science.gov (United States)

    Nogami, Takahiro; Fujinaga, Satoshi; Jinno, Naoya; Hashimoto, Masahiko; Tsukagoshi, Kazuhiko

    2012-01-01

    An open-tubular capillary chromatography was developed based on the tube radial distribution of the ternary mixed carrier solvents that generated the inner and outer phases under laminar flow conditions. This is called "tube radial distribution chromatography" (TRDC). In this report, the elution behavior of lambda-DNA (48502 bp) as a biopolymer was examined by the TRDC system. The ternary mixture of water-acetonitrile-ethyl acetate, 15:3:2 or 3:8:4 volume ratio, as a carrier solution was fed into the capillary tube made of polytetrafluoroethylene (PTFE) or fused-silica. The mixture of hydrophobic 1-naphthol and hydrophilic lambda-DNA was subjected to the TRDC system using the water-rich carrier solution. Lambda-DNA and 1-naphthol were distributed between the inner and outer phases due to their hydrophilic and hydrophobic nature, and then eluted in this order, undergoing chromatographic separation. The mixture of hydrophilic 2,6-naphthalenedisulfonic acid and hydrophobic lambda-DNA that was treated with surfactants was also examined with the organic solvent-rich carrier solution. The modified hydrophobic DNA and 2,6-naphthalenedisulfonic acid were distributed and eluted in this order due to their nature.

  8. Determination of marbofloxacin by high performance capillary zone electrophoresis%高效毛细管电泳法用于麻保沙星的测定

    Institute of Scientific and Technical Information of China (English)

    李志伟; 崔哲; 刘波; 赵云超

    2011-01-01

    建立了一种高效毛细管电泳法测定麻保沙星原料药含量的方法.采用未涂层石英毛细管柱,以15 mmol/L硼酸钠缓冲液(pH值为9.2)为电泳介质,分离电压为20 kV,采用高度差进样10s,检测波长为295 nm,麻保沙星在10~100μg/mL范围内线性良好,平均回收率为100.2%,RSD值为0.97%.%A high performance capillary zone electrophoresis method was established for the determination of marbofloxacin drug substance. An untreated fused-silica capillary was used with 15 mmol/L sodium borate buffer (pH 9.2) as running buffer at the detection wavelength of 295 nm, separation voltage of 20 kV and the injection volume of sample for 10 s. The calibration curve for marbofloxacin is linear in the concentration range of 10 ~ 100 μg/mL. The average recovery is 100. 2% with RSD of 0.97%.

  9. On-Line Organic Solvent Field Enhanced Sample Injection in Capillary Zone Electrophoresis for Analysis of Quetiapine in Beagle Dog Plasma

    Directory of Open Access Journals (Sweden)

    Yuqing Cao

    2016-01-01

    Full Text Available A rapid and sensitive capillary zone electrophoresis (CZE method with field enhanced sample injection (FESI was developed and validated for the determination of quetiapine fumarate in beagle dog plasma, with a sample pretreatment by LLE in 96-well deep format plate. The optimum separation was carried out in an uncoated 31.2 cm × 75 μm fused-silica capillary with an applied voltage of 13 kV. The electrophoretic analysis was performed by 50 mM phosphate at pH 2.5. The detection wavelength was 210 nm. Under these optimized conditions, FESI with acetonitrile enhanced the sensitivity of quetiapine about 40–50 folds in total. The method was suitably validated with respect to stability, specificity, linearity, lower limit of quantitation, accuracy, precision and extraction recovery. Using mirtazapine as an internal standard (100 ng/mL, the response of quetiapine was linear over the range of 1–1000 ng/mL. The lower limit of quantification was 1 ng/mL. The intra- and inter-day precisions for the assay were within 4.8% and 12.7%, respectively. The method represents the first application of FESI-CZE to the analysis of quetiapine fumarate in beagle dog plasma after oral administration.

  10. Hollow silica spheres: synthesis and mechanical properties.

    Science.gov (United States)

    Zhang, Lijuan; D'Acunzi, Maria; Kappl, Michael; Auernhammer, Günter K; Vollmer, Doris; van Kats, Carlos M; van Blaaderen, Alfons

    2009-03-03

    Core-shell polystyrene-silica spheres with diameters of 800 nm and 1.9 microm were synthesized by soap-free emulsion and dispersion polymerization of the polystyrene core, respectively. The polystyrene spheres were used as templates for the synthesis of silica shells of tunable thickness employing the Stöber method [Graf et al. Langmuir 2003, 19, 6693]. The polystyrene template was removed by thermal decomposition at 500 degrees C, resulting in smooth silica shells of well-defined thickness (15-70 nm). The elastic response of these hollow spheres was probed by atomic force microscopy (AFM). A point load was applied to the particle surface through a sharp AFM tip, and successively increased until the shell broke. In agreement with the predictions of shell theory, for small deformations the deformation increased linearly with applied force. The Young's modulus (18 +/- 6 GPa) was about 4 times smaller than that of fused silica [Adachi and Sakka J. Mater. Sci. 1990, 25, 4732] but identical to that of bulk silica spheres (800 nm) synthesized by the Stöber method, indicating that it yields silica of lower density. The minimum force needed to irreversibly deform (buckle) the shell increased quadratically with shell thickness.

  11. All-silica nanofluidic devices for DNA-analysis fabricated by imprint of sol-gel silica with silicon stamp

    DEFF Research Database (Denmark)

    Mikkelsen, Morten Bo Lindholm; Letailleur, Alban A; Søndergård, Elin

    2011-01-01

    We present a simple and cheap method for fabrication of silica nanofluidic devices for single-molecule studies. By imprinting sol-gel materials with a multi-level stamp comprising micro- and nanofeatures, channels of different depth are produced in a single process step. Calcination of the imprin......We present a simple and cheap method for fabrication of silica nanofluidic devices for single-molecule studies. By imprinting sol-gel materials with a multi-level stamp comprising micro- and nanofeatures, channels of different depth are produced in a single process step. Calcination...... of the imprinted hybrid sol-gel material produces purely inorganic silica, which has very low autofluorescence and can be fusion bonded to a glass lid. Compared to top-down processing of fused silica or silicon substrates, imprint of sol-gel silica enables fabrication of high-quality nanofluidic devices without...

  12. Biodegradation-tunable mesoporous silica nanorods for controlled drug delivery.

    Science.gov (United States)

    Park, Sung Bum; Joo, Young-Ho; Kim, Hyunryung; Ryu, WonHyoung; Park, Yong-il

    2015-05-01

    Mesoporous silica in the forms of micro- or nanoparticles showed great potentials in the field of controlled drug delivery. However, for precision control of drug release from mesoporous silica-based delivery systems, it is critical to control the rate of biodegradation. Thus, in this study, we demonstrate a simple and robust method to fabricate "biodegradation-tunable" mesoporous silica nanorods based on capillary wetting of anodic aluminum oxide (AAO) template with an aqueous alkoxide precursor solution. The porosity and nanostructure of silica nanorods were conveniently controlled by adjusting the water/alkoxide molar ratio of precursor solutions, heat-treatment temperature, and Na addition. The porosity and biodegradation kinetics of the fabricated mesoporous nanorods were analyzed using N2 adsorption/desorption isotherm, TGA, DTA, and XRD. Finally, the performance of the mesoporous silica nanorods as drug delivery carrier was demonstrated with initial burst and subsequent "zero-order" release of anti-cancer drug, doxorubicin.

  13. [Analysis of tartrazine aluminum lake and sunset yellow aluminum lake in foods by capillary zone electrophoresis].

    Science.gov (United States)

    Zhang, Yiding; Chang, Cuilan; Guo, Qilei; Cao, Hong; Bai, Yu; Liu, Huwei

    2014-04-01

    A novel analytical method for tartrazine aluminum lake and sunset yellow aluminum lake using capillary zone electrophoresis (CZE) was studied. The pigments contained in the color lakes were successfully separated from the aluminum matrix in the pre-treatment process, which included the following steps: dissolve the color lakes in 0.1 mol/L H2SO4, adjust the pH of the solution to 5.0, then mix it with the solution of EDTA x 2Na and heat it in a water bath, then use polyamide powder as the stationary phase of solid phase extraction to separate the pigments from the solution, and finally elute the pigments with 0.1 mol/L NaOH. The CZE conditions systematically optimized for tartrazine aluminum lake were: 48.50 cm of a fused silica capillary with 40.00 cm effective length and 50 microm i. d., the temperature controlled at 20.0 degrees C, 29.0 kV applied, HPO4(2-)-PO4(3-) (0.015 mol/L, pH 11.45) solution as running buffer, detection at 263 nm. The conditions for sunset yellow aluminum lake were: the same capillary and temperature, 25.0 kV applied, HPO4(2-)-PO4(3-) (0.025 mol/L, pH 11.45) solution as running buffer, detection at 240 nm. The limits of detection were 0.26 mg/L and 0.27 mg/L, and the linear ranges were 0.53-1.3 x 10(2) mg/L and 0.54-1.4 x 10(2) mg/L for tartrazine aluminum lake and sunset yellow aluminum lake, respectively. The RSDs were 4.3% and 5.7% (run to run, n = 6), 5.6% and 6.0% (day to day, n = 6) for tartrazine aluminum lake and sunset yellow aluminum lake, respectively. Further developments for this method could make it a routinely used method analyzing color lakes in foods.

  14. Flow counterbalanced capillary electrophoresis using packed capillary columns: resolution of enantiomers and isotopomers.

    Science.gov (United States)

    Henley, W Hampton; Wilburn, Richard T; Crouch, Andrew M; Jorgenson, James W

    2005-11-01

    A method with the ability to increase greatly both the resolution and efficiency of a given capillary electrophoretic system is described. This method differs from traditional capillary electrophoresis (CE) in that a counterflow is induced in the direction opposite to the electrokinetic migration of the analyte. This has the effect of extending not only the time the analytes migrate in the electric field but also the effective length and the effective applied voltage of the system. Previous work in our group with flow counterbalanced capillary electrophoresis has utilized an open tube of small inner diameter to reduce peak broadening caused by hydrodynamic flow. Narrow-diameter capillaries (5-10 microm) restricted analysis to fluorescent analytes and laser-induced fluorescence detection. The method described here uses a capillary of much larger inner diameter (75 microm) that has been packed with nonporous silica particles. The packing material reduces the amount of band broadening caused by pressure-induced flow relative to that experienced in an open tube. A larger diameter capillary allows the detection of analytes by UV absorption, not only eliminating the need to tag analytes with fluorescent tags but also allowing for the detection of a much broader range of analytes. The system was evaluated by studying the separations of several enantiomers using only beta-cyclodextrin as the chiral selector. The system was also used to resolve the two naturally occurring isotopes of bromine and to resolve phenylalanine from phenylalanine-d8. Relative to traditional CE, large improvements in resolution and separation efficiency have been achieved with this method.

  15. Optimization of the enantioseparation of a diaryl-pyrazole sulfonamide derivative by capillary electrophoresis in a dual CD mode using experimental design.

    Science.gov (United States)

    Rogez-Florent, Tiphaine; Foulon, Catherine; Six, Perrine; Goossens, Laurence; Danel, Cécile; Goossens, Jean-François

    2014-10-01

    A CE method using dual cationic and neutral cyclodextrins (CD) was optimized for the enantiomeric separation of a compound presenting a diaryl sulfonamide group. Preliminary studies were made to select the optimal CDs and pH of the BGE. Two CDs (amino-β-CD and β-CD) were selected to separate the enantiomers in a 67 mM phosphate buffer at pH 7.4. However, the repeatability of the analyses obtained on bare-fused silica capillary was not acceptable owing to the adsorption of the amino-β-CD to the capillary. To prevent this, a dynamic coating of the capillary was used employing five layers of ionic-polymer (poly(diallyldimethylammonium) chloride (PDADMAC) and poly(sodium 4-styrenesulfonate). The efficiency of the coating was assessed by measuring the EOF stability. Repeatability of the injections was obtained when intermediate coating with PDADMAC was performed between each run. Secondly, this enantioseparation method was optimized using a central composite circumscribed design including three factors: amino-β-CD and β-CD concentrations and the percentage of methanol. Under the optimal conditions (i.e. 16.6 mM of amino-β-CD, 2.6 mM of β-CD, 0% MeOH in 67 mM phosphate buffer (pH 7.4) as BGE, cathodic injection 0.5 psi, 5 s, separation voltage 15 kV and a temperature of 15°C), complete enantioresolution of the analyte was obtained. It is worth mentioning that the design of experiments (DOE) protocol employed showed a significant interaction between CDs, highlighting the utility of DOE in method development. Finally, small variations in the ionic-polymer concentrations did not significantly influence the EOF, confirming the robustness of the coating method.

  16. Sol-gel immobilized cyano-polydimethylsiloxane coating for capillary microextraction of aqueous trace analytes ranging from polycyclic aromatic hydrocarbons to free fatty acids.

    Science.gov (United States)

    Kulkarni, Sameer; Fang, Li; Alhooshani, Khalid; Malik, Abdul

    2006-08-18

    Sol-gel coating containing highly polar cyanopropyl and nonpolar poly(dimethylsiloxane) components (sol-gel CN-PDMS coating) was developed for capillary microextraction (CME). The sol-gel chemistry provided an efficient means to immobilize the CN-PDMS coating by establishing chemical anchorage between the coating and the fused silica capillary inner surface. This chemical bond provided excellent thermal and solvent stability to the created sol-gel coating. For the extraction of polar and nonpolar analytes, the upper allowable conditioning temperatures were 330 degrees C and 350 degrees C, respectively. To our knowledge, this is the first time when a CN-PDMS thick coating survived such a high operation temperature. The prepared sol-gel CN-PDMS coating provided effective extraction of polar and nonpolar analytes simultaneously from aqueous samples. The cyanopropyl moiety in sol-gel CN-PDMS coatings provided effective extraction of highly polar analytes such as free fatty acids, alcohols, and phenols without requiring derivatization, pH adjustment or salting out procedures. The PDMS moiety, on the other hand, provided efficient extraction of nonpolar analytes. The extraction properties of the sol-gel CN-PDMS coatings can be fine tuned via manipulation of relative proportions of 3-cyanopropyltriethoxysilane and hydroxy-terminated PDMS in the sol solution used to create the coatings. Detection limits of nanogram/liter (ng/L) were achieved for both highly polar and nonpolar analytes directly extracted from aqueous media using sol-gel CN-PDMS coated microextraction capillaries followed by GC analysis.

  17. 阳离子交换毛细管整体柱的制备及其在毛细管离子色谱中的应用%Preparation and Application of Cation-exchange Capillary Monolithic Column in Capillary Ion Chromatography

    Institute of Scientific and Technical Information of China (English)

    李晶; 朱岩

    2013-01-01

    Polymer-based cation exchange capillary monolithic column was prepared for capillary ion chromatography (CIC) by radical polymerization in a 320-μm-i. d. fused-silica capillary tube, taking glycidyl methacrylate ( GMA ) as the functional monomer, ethylene dimethacrylate ( EDMA) as the cross-linking agent and in the presence of 1 ,4-butanediol, 1-propanol and water as the porogen solvents and azobisisobutyronitrile (AIBN) as a suitable initiator. Introduction of cation exchange sites was achieved by reacting with Na2SO3. Coupled with the prepared cation exchange capillary monolithic column, a capillary ion chromatography system was constructed with a pump (in μL/min level) , a capillary detection cell and a UV detector, on which more chromatographic characteristics were further studied. With the CIC system, 9 common univalent and divalent cations (Li+ , Na+ , NH4+ , K+ , Cs+ , Mg2+, Ca2+ , Sr2+, Ba2+) were successfully separated and determined by flow rate gradient. Another interesting separation of cations and melamine was also tested on the prepared column.%以甲基丙烯酸缩水甘油酯(GMA)为功能单体,亚乙基二甲基丙烯酸酯(EDMA)为交联剂,偶氮二异丁腈(AIBN)为自由基引发剂,在三元致孔剂(正丙醇,1,4-丁二醇,水)的存在下,在320μm内径的弹性石英毛细管柱内制备得到带有环氧功能基团的聚合物整体柱基质;利用Na2SO3对其改性,制备得到磺酸基型阳离子交换毛细管整体柱.采用微流泵、毛细管检测池和紫外检测器构建了毛细管离子色谱系统,并对所制备的整体柱的流体力学参数、色谱性能参数进行评价;采用流速梯度洗脱的方式实现9种常见阳离子(Li+,Na+,NH4+,K+,Cs+,Mg2+,Ca2+,Sr2+,Ba2+)的分离分析;此色谱系统还可应用于牛奶中阳离子和三聚氰胺的分离检测.

  18. The effect of heat treatment on the magnitude and composition of residual gas in sealed silica glass ampoules

    Science.gov (United States)

    Palosz, W.; Szofran, F. R.; Lehoczky, S. L.

    1994-01-01

    The residual gas pressure and composition in sealed silica glass ampoules as a function of different treatment procedures has been investigated. The dependence of the residual gas on the outgassing and annealing parameters has been determined. The effects of the fused silica brand, of the ampoule fabrication, and of post-outgassing procedures have been evaluated.

  19. About a New Type of Fuse Based on the Controllable Fusing Effect

    Directory of Open Access Journals (Sweden)

    PLESCA, A.

    2009-06-01

    Full Text Available Fuses are among the best known of electrical devices and there are an extremely large number in use throughout the world. Beside of the advantageous features, the nowadays fuses have certain drawbacks. Therefore, a new type of fuse based on controllable fusing concept is proposed and a study as regards the total clearing time is done. The new concept has been validated through many experimental tests at different current values. The new type of fuse based on controllable fusing concept can be integrated within an overcurrent protection system especially to protect power semiconductors where the Joule integral criterion is better satisfied.

  20. Detection and identification of volatile substances by headspace capillary gas chromatography to aid the diagnosis of acute poisoning.

    Science.gov (United States)

    Streete, P J; Ruprah, M; Ramsey, J D; Flanagan, R J

    1992-07-01

    Headspace gas chromatography with split flame-ionization-electron-capture detection is a simple method of screening for a wide range of volatile substances in biological fluids. A 60 m x 0.53 mm i.d. thick-film (5 microns) fused-silica capillary coated with SPB-1 (Supelchem) with split flame-ionization-electron-capture detection provides a valuable alternative to packed columns in this work. Most commonly abused compounds, including many with very low boiling-points such as bromochlorodifluoromethane (BCF), butane, dimethyl ether, FC 11, FC 12, isobutane and propane, can be retained and differentiated at an initial column temperature of 40 degrees C followed by programming to 200 degrees C. The total analysis time is 26 min. Retention and detector response data were generated for 244 compounds. Good peak shapes are obtained for polar analytes such as ethanol and injections of up to 0.30 cm3 of headspace can be performed with no discernable loss of efficiency. The sensitivity is thus at least as good as that attainable with packed columns. Of the commonly encountered compounds, only isobutane-methanol and paraldehyde-toluene are at all difficult to differentiate. Quantitative measurements can be performed either isothermally or by using the temperature programme.

  1. Increasing conclusiveness of metabonomic studies by chem-informatic preprocessing of capillary electrophoretic data on urinary nucleoside profiles.

    Science.gov (United States)

    Szymańska, E; Markuszewski, M J; Capron, X; van Nederkassel, A-M; Heyden, Y Vander; Markuszewski, M; Krajka, K; Kaliszan, R

    2007-01-17

    Nowadays, bioinformatics offers advanced tools and procedures of data mining aimed at finding consistent patterns or systematic relationships between variables. Numerous metabolites concentrations can readily be determined in a given biological system by high-throughput analytical methods. However, such row analytical data comprise noninformative components due to many disturbances normally occurring in analysis of biological samples. To eliminate those unwanted original analytical data components advanced chemometric data preprocessing methods might be of help. Here, such methods are applied to electrophoretic nucleoside profiles in urine samples of cancer patients and healthy volunteers. The electrophoretic nucleoside profiles were obtained under following conditions: 100 mM borate, 72.5 mM phosphate, 160 mM SDS, pH 6.7; 25 kV voltage, 30 degrees C temperature; untreated fused silica capillary 70 cm effective length, 50 microm I.D. Different most advanced preprocessing tools were applied for baseline correction, denoising and alignment of electrophoretic data. That approach was compared to standard procedure of electrophoretic peak integration. The best results of preprocessing were obtained after application of the so-called correlation optimized warping (COW) to align the data. The principal component analysis (PCA) of preprocessed data provides a clearly better consistency of the nucleoside electrophoretic profiles with health status of subjects than PCA of peak areas of original data (without preprocessing).

  2. Dynamic simulation of flywheel-type fuses

    OpenAIRE

    Editorial Office

    1996-01-01

    Rounds of ammunition are normally armed with a fuse. In this study, a fuse is developed which uses a flywheel-type mechanism controlled by time or distance. Due to its simplicity of operation and construction, the concept is expected to have high reliabil­ity. The dynamic response of all the components of this flywheel-type fuse is mathematically modelled. Simulation software was developed which connects the mathematical models of the various components. With the definition of boundary value...

  3. Stereospecific capillary electrophoresis assays using pentapeptide substrates for the study of Aspergillus nidulans methionine sulfoxide reductase A and mutant enzymes.

    Science.gov (United States)

    Zhu, Qingfu; El-Mergawy, Rabab G; Zhou, Yuzhen; Chen, Chunyang; Heinemann, Stefan H; Schönherr, Roland; Robaa, Dina; Sippl, Wolfgang; Scriba, Gerhard K E

    2016-07-01

    Stereospecific capillary electrophoresis-based methods for the analysis of methionine sulfoxide [Met(O)]-containing pentapeptides were developed in order to investigate the reduction of Met(O)-containing peptide substrates by recombinant Aspergillus nidulans methionine sulfoxide reductase A (MsrA) as well as enzymes carrying mutations in position Glu99 and Asp134. The separation of the diastereomers of the N-acetylated, C-terminally 2,4-dinitrophenyl (Dnp)-labeled pentapeptides ac-Lys-Phe-Met(O)-Lys-Lys-Dnp, ac-Lys-Asp-Met(O)-Asn-Lys-Dnp and ac-Lys-Asn-Met(O)-Asp-Lys-Dnp was achieved in 50 mM Tris-HCl buffers containing sulfated β-CD in fused-silica capillaries, while the diastereomer separation of ac-Lys-Asp-Met(O)-Asp-Lys-Dnp was achieved by sulfated β-CD-mediated MEKC. The methods were validated with regard to range, linearity, accuracy, limits of detection and quantitation as well as precision. Subsequently, the substrates were incubated with wild-type MsrA and three mutants in the presence of dithiothreitol as reductant. Wild-type MsrA displayed the highest activity towards all substrates compared to the mutants. Substitution of Glu99 by Gln resulted in the mutant with the lowest activity towards all substrates except for ac-Lys-Asn-Met(O)-Asp-Lys-Dnp, while replacement Asn for Asp134 lead to a higher activity towards ac-Lys-Asp-Met(O)-Asn-Lys-Dnp compared with the Glu99 mutant. The mutant with Glu instead of Asp134 was the most active among the mutant enzymes. Molecular modeling indicated that the conserved Glu99 residue is buried in the Met-S-(O) groove, which might contribute to the correct placing of substrates and, consequently, to the catalytic activity of MsrA, while Asp134 did not form hydrogen bonds with the substrates but only within the enzyme.

  4. FUSE Observations of eta Carinae

    CERN Document Server

    Iping, R C; Gull, T R

    2004-01-01

    Eta Carinae was observed by FUSE through the LWRS (30 arcsec x30 arcsec) and HIRS (1.25 arcsec x 20 arcsec) apertures in March and April 2004. There are significant differences between the two spectra. About half of the LWRS flux appears to be due to two B-type stars near the edge of the LWRS aperture, 14 arcsec from eta Carinae. The HIRS spectrum (LiF1 channel) therefore reveals the intrinsic FUV spectrum of eta Carinae without this stellar contamination. The HIRS spectrum contains strong interstellar H2 having high rotational excitation (up to J=8). Most of the atomic species with prominent ISM features (C II, Fe II, Ar I, P II, etc) also have strong blue-shifted absorption to v= ~ -580 km/s that is associated with expanding debris from the 1840 eruption.

  5. Gas-Filled Capillary Model

    Science.gov (United States)

    Steinhauer, L. C.; Kimura, W. D.

    2006-11-01

    We have developed a 1-D, quasi-steady-state numerical model for a gas-filled capillary discharge that is designed to aid in selecting the optimum capillary radius in order to guide a laser beam with the required intensity through the capillary. The model also includes the option for an external solenoid B-field around the capillary, which increases the depth of the parabolic density channel in the capillary, thereby allowing for propagation of smaller laser beam waists. The model has been used to select the parameters for gas-filled capillaries to be utilized during the Staged Electron Laser Acceleration — Laser Wakefield (STELLA-LW) experiment.

  6. Stability of capillary gels for automated sequencing of DNA.

    Science.gov (United States)

    Swerdlow, H; Dew-Jager, K E; Brady, K; Grey, R; Dovichi, N J; Gesteland, R

    1992-08-01

    Recent interest in capillary gel electrophoresis has been fueled by the Human Genome Project and other large-scale sequencing projects. Advances in gel polymerization techniques and detector design have enabled sequencing of DNA directly in capillaries. Efforts to exploit this technology have been hampered by problems with the reproducibility and stability of gels. Gel instability manifests itself during electrophoresis as a decrease in the current passing through the capillary under a constant voltage. Upon subsequent microscopic examination, bubbles are often visible at or near the injection (cathodic) end of the capillary gel. Gels have been prepared with the polyacrylamide matrix covalently attached to the silica walls of the capillary. These gels, although more stable, still suffer from problems with bubbles. The use of actual DNA sequencing samples also adversely affects gel stability. We examined the mechanisms underlying these disruptive processes by employing polyacrylamide gel-filled capillaries in which the gel was not attached to the capillary wall. Three sources of gel instability were identified. Bubbles occurring in the absence of sample introduction were attributed to electroosmotic force; replacing the denaturant urea with formamide was shown to reduce the frequency of these bubbles. The slow, steady decline in current through capillary sequencing gels interferes with the ability to detect other gel problems. This phenomenon was shown to be a result of ionic depletion at the gel-liquid interface. The decline was ameliorated by adding denaturant and acrylamide monomers to the buffer reservoirs. Sample-induced problems were shown to be due to the presence of template DNA; elimination of the template allowed sample loading to occur without complications.(ABSTRACT TRUNCATED AT 250 WORDS)

  7. A hybrid fluorous monolithic capillary column with integrated nanoelectrospray ionization emitter for determination of perfluoroalkyl acids by nano-liquid chromatography-nanoelectrospray ionization-mass spectrometry/mass spectrometry.

    Science.gov (United States)

    Zhang, Haiyang; Ou, Junjie; Wei, Yinmao; Wang, Hongwei; Liu, Zhongshan; Zou, Hanfa

    2016-04-01

    A hybrid fluorous monolithic column was simply prepared via photo-initiated free radical polymerization of an acrylopropyl polyhedral oligomeric silsesquioxane (acryl-POSS) and a perfluorous monomer (2,2,3,3,4,4,5,5,6,6,7,7-dodecafluoroheptyl acrylate) in UV-transparent fused-silica capillaries within 5min. The physical characterization of hybrid fluorous monolith, including scanning electron microscopy (SEM), Fourier transform infrared (FT-IR) spectroscopy, mercury intrusion porosimetry (MIP) and nitrogen adsorption/desorption measurement was performed. Chromatographic performance was also evaluated by capillary liquid chromatography (cLC). Due to the fluorous-fluorous interaction between fluorous monolith and analytes, fluorobenzenes could well be separated, and the column efficiencies reached 86,600-92,500plates/m at the velocity of 0.87mm/s for alkylbenzenes and 51,900-76,000plates/m at the velocity of 1.10mm/s for fluorobenzenes. Meanwhile, an approach to integrate nanoelectrospray ionization (ESI) emitter with hybrid fluorous monolithic column was developed for quantitative determination of perfluoroalkyl acids by nanoHPLC-ESI-MS/MS. The integration design could minimize extracolumn volume, thus excluding undesirable peak broadening and improving separation performance.

  8. Stability-indicating capillary zone electrophoresis method for the assessment of recombinant human granulocyte-macrophage colony-stimulating factor and its correlation with reversed-phase liquid chromatography method and bioassay.

    Science.gov (United States)

    Dalmora, Sergio Luiz; Butzge, Cairo dos Santos; Machado, Francine Trevisan; Walter, Maurício Elesbão; Dalmora, Maria Elisabeth de Ávila; Souto, Ricardo Bizogne

    2012-05-30

    A stability-indicating capillary zone electrophoresis (CZE) method was validated for the analysis of granulocyte-macrophage colony-stimulating factor (rhGM-CSF) using leuprorelin acetate (LA), as internal standard (IS). A fused-silica capillary (75 μm i.d.; effective length, 72 cm) was used at 25 °C; the applied voltage was 12 kV. The background electrolyte solution consisted of 50mM di-sodium hydrogen phosphate solution at pH 8.8. Injections were performed using a pressure mode at 50 mbar for 9s, with detection by photodiode array detector set at 200 nm. Specificity and stability-indicating capability were established in degradation studies, which also showed that there was no interference of the excipients. The method was linear over the concentration range of 2.5-200 μg mL(-1) (r(2)=0.9995) and the limit of detection (LOD) and limit of quantitation (LOQ) were 0.79 μg mL(-1) and 2.5 μg mL(-1), respectively. The accuracy was 99.14% with bias lower than 1.40%. The method was applied to the quantitative analysis of biopharmaceutical formulations, and the results were correlated to those of a validated reversed-phase LC method (RP-LC), and an in vitro bioassay, showing non-significant differences (p>0.05).

  9. Effect of air on water capillary flow in silica nanochannels

    DEFF Research Database (Denmark)

    Zambrano, Harvey; Walther, Jens Honore; Oyarzua, Elton

    2013-01-01

    Capillarity is a classical topic in fluid dynamics. The fundamental relationship between capillarity and surface tension is solidly established. Nevertheless, capillarity is an active research area especially as the miniaturization of devices is reaching the molecular scale. Currently, with the f......Capillarity is a classical topic in fluid dynamics. The fundamental relationship between capillarity and surface tension is solidly established. Nevertheless, capillarity is an active research area especially as the miniaturization of devices is reaching the molecular scale. Currently......, with the fabrication of microsystems integrated by nanochannels, a thorough understanding of the transport of fluids in nanoconfinement is required for a successful operation of the functional parts of such devices. In this work, Molecular Dynamics simulations are conducted to study the spontaneous imbibition of water...

  10. Derivatization in Capillary Electrophoresis.

    Science.gov (United States)

    Marina, M Luisa; Castro-Puyana, María

    2016-01-01

    Capillary electrophoresis is a well-established separation technique in analytical research laboratories worldwide. Its interesting advantages make CE an efficient and potent alternative to other chromatographic techniques. However, it is also recognized that its main drawback is the relatively poor sensitivity when using optical detection. One way to overcome this limitation is to perform a derivatization reaction which is intended to provide the analyte more suitable analytical characteristics enabling a high sensitive detection. Based on the analytical step where the CE derivatization takes place, it can be classified as precapillary (before separation), in-capillary (during separation), or postcapillary (after separation). This chapter describes the application of four different derivatization protocols (in-capillary and precapillary modes) to carry out the achiral and chiral analysis of different compounds in food and biological samples with three different detection modes (UV, LIF, and MS).

  11. How Capillary Rafts Sink

    CERN Document Server

    Protiere, S; Aristoff, J; Stone, H

    2010-01-01

    We present a fluid dynamics video showing how capillary rafts sink. Small objects trapped at an interface are very common in Nature (insects walking on water, ant rafts, bubbles or pollen at the water-air interface, membranes...) and are found in many multiphase industrial processes. Thanks to Archimedes principle we can easily predict whether an object sinks or floats. But what happens when several small particles are placed at an interface between two fluids. In this case surface tension also plays an important role. These particles self-assemble by capillarity and thus form what we call a "capillary raft". We show how such capillary rafts sink for varying sizes of particles and define how this parameter affects the sinking process.

  12. Fused combiners for photonic crystal bers

    DEFF Research Database (Denmark)

    Noordegraaf, Danny

    The work presented in this Ph.D. thesis focuses on the fabrication of fused combiners for high-power fiber lasers and amplifiers. The main focus of the Ph.D. project was to further develop the fused pump combiners for airclad photonic crystal bers (PCFs), and implement a signal feed...

  13. Silica in Protoplanetary Disks

    CERN Document Server

    Sargent, B A; Tayrien, C; McClure, M K; Li, A; Basu, A R; Manoj, P; Watson, D M; Bohac, C J; Furlan, E; Kim, K H; Green, J D; Sloan, G C

    2008-01-01

    Mid-infrared spectra of a few T Tauri stars (TTS) taken with the Infrared Spectrograph (IRS) on board the Spitzer Space Telescope show prominent narrow emission features indicating silica (crystalline silicon dioxide). Silica is not a major constituent of the interstellar medium; therefore, any silica present in the circumstellar protoplanetary disks of TTS must be largely the result of processing of primitive dust material in the disks surrouding these stars. We model the silica emission features in our spectra using the opacities of various polymorphs of silica and their amorphous versions computed from earth-based laboratory measurements. This modeling indicates that the two polymorphs of silica, tridymite and cristobalite, which form at successively higher temperatures and low pressures, are the dominant forms of silica in the TTS of our sample. These high temperature, low pressure polymorphs of silica present in protoplanetary disks are consistent with a grain composed mostly of tridymite named Ada found...

  14. Multifunctional mesoporous silica catalyst

    Energy Technology Data Exchange (ETDEWEB)

    Lin, Victor Shang-Yi; Tsai, Chih-Hsiang; Chen, Hung-Ting; Pruski, Marek; Kobayashi, Takeshi

    2015-03-31

    The present invention provides bifunctional silica mesoporous materials, including mesoporous silica nanoparticles ("MSN"), having pores modified with diarylammonium triflate and perfluoroaryl moieties, that are useful for the acid-catalyzed esterification of organic acids with organic alcohols.

  15. Silica extraction from geothermal water

    Science.gov (United States)

    Bourcier, William L; Bruton, Carol J

    2014-09-23

    A method of producing silica from geothermal fluid containing low concentration of the silica of less than 275 ppm includes the steps of treating the geothermal fluid containing the silica by reverse osmosis treatment thereby producing a concentrated fluid containing the silica, seasoning the concentrated fluid thereby producing a slurry having precipitated colloids containing the silica, and separating the silica from the slurry.

  16. Self-assembled covalent capillary coating of diazoresin/carboxyl fullerene for analysis of proteins by capillary electrophoresis and a comparison with diazoresin/graphene oxide coating.

    Science.gov (United States)

    Yu, Bing; Shu, Xi; Cong, Hailin; Chen, Xin; Liu, Huwei; Yuan, Hua; Chi, Ming

    2016-03-11

    Self-assembled and covalently linked capillary coatings of carboxyl fullerenes (C60-COOH) were prepared using photosensitive diazoresin (DR) as a coupling agent. Layer by layer (LBL) self-assembled DR/C60-COOH coatings based on ionic bonding was fabricated first on the inner surface of silica capillary, and subsequently converted into covalent bonding after treatment with UV light through a unique photochemistry reaction of DR. The covalently bonded coatings had the ability of suppressing protein adsorption on the inner surface of silica capillary, and thus the baseline separation of lysozyme (Lys), cytochrome c (Cyt-c), bovine serum albumin (BSA) and myoglobin (Mb) was achieved within 13min by using capillary electrophoresis (CE). The covalently linked DR/C60-COOH capillary coatings presented good chemical stability and repeatability. The reproducibility of the separation of proteins was less than 1%, 2.5%, and 3.5%, respectively, for run-to-run, day-to-day, capillary-to-capillary, respectively; and the RSD of migration time for the proteins are all less than 2.5% after a continuous 100 times running in a coating column. Compared with DR/graphene oxide (GO) coatings prepared by the same method, the DR/C60-COOH capillary coatings showed excellent protein separation performance due to a self-lubrication based anti-fouling mechanism. Because of the replacement of highly toxic and moisture sensitive silane coupling agent by DR in the covalent coating preparation, this method may provide an environmentally friendly and simple way to prepare the covalently coated capillaries for CE.

  17. Porous Properties of Nano-fibriform Silica from Natural Chrysotile

    Institute of Scientific and Technical Information of China (English)

    WANG Lijuan; LU Anhuai; WANG Changqiu; LI Xuejun; ZHENG Xishen; ZHAO Dongjun; LIU Rui

    2006-01-01

    With the TEM and physical gas adsorption techniques, porous properties of nano-fibriform silica (MLD: 92.73 %) from natural chrysotile are studied in this paper. The results indicate that porous nano-fibriform silica results from brucite octahedral sheets of nature chrysotile dissolved completely and Si-O tetrahedral sheets collapsed by acid leaching. Its length is at a micron or nanometer scale.There are two types of pores: pores among neighboring fibers and pores in nanofiber. These pores (less than 6.5 nm in diameter, mostly 2.1 nm and 3.8 nm) all belong to mesopores. The pores in fibers consist of those among SiO2 particles, those among aggregates, remnant nanotubes and capillary tubes. Nanofibriform silica proves better than the traditional silica as a carrier of catalyzer and a filler for reinforce rubber and plastics.

  18. Laser welding of fused quartz

    Science.gov (United States)

    Piltch, Martin S.; Carpenter, Robert W.; Archer, III, McIlwaine

    2003-06-10

    Refractory materials, such as fused quartz plates and rods are welded using a heat source, such as a high power continuous wave carbon dioxide laser. The radiation is optimized through a process of varying the power, the focus, and the feed rates of the laser such that full penetration welds may be accomplished. The process of optimization varies the characteristic wavelengths of the laser until the radiation is almost completely absorbed by the refractory material, thereby leading to a very rapid heating of the material to the melting point. This optimization naturally occurs when a carbon dioxide laser is used to weld quartz. As such this method of quartz welding creates a minimum sized heat-affected zone. Furthermore, the welding apparatus and process requires a ventilation system to carry away the silicon oxides that are produced during the welding process to avoid the deposition of the silicon oxides on the surface of the quartz plates or the contamination of the welds with the silicon oxides.

  19. Femtosecond laser fabrication of nanostructures in silica glass.

    Science.gov (United States)

    Taylor, R S; Hnatovsky, C; Simova, E; Rayner, D M; Bhardwaj, V R; Corkum, P B

    2003-06-15

    A femtosecond laser beam focused inside fused silica and other glasses can modify the refractive index of the glass. Chemical etching and atomic-force microscope studies show that the modified region can have a sharp-tipped cone-shaped structure with a tip diameter as small as 100 nm. Placing the structure near the bottom surface of a silica glass sample and applying a selective chemical etch to the bottom surface produces clean, circular, submicrometer-diameter holes. Holes spaced as close to one another as 1.4 microm are demonstrated.

  20. Capillary permeability in adipose tissue

    DEFF Research Database (Denmark)

    Paaske, W P; Nielsen, S L

    1976-01-01

    of about 7 ml/100 g-min. This corresponds to a capillary diffusion capacity of 2.0 ml/100 g-min which is half the value reported for vasodilated skeletal muscle having approximately twice as great capillary surface area. Thus, adipose tissue has about the same capillary permeability during slight metabolic...

  1. Porphyrins Fused with Unactivated Polycyclic Aromatic Hydrocarbons

    KAUST Repository

    Diev, Vyacheslav V.

    2012-01-06

    A systematic study of the preparation of porphyrins with extended conjugation by meso,β-fusion with polycyclic aromatic hydrocarbons (PAHs) is reported. The meso-positions of 5,15-unsubstituted porphyrins were readily functionalized with PAHs. Ring fusion using standard Scholl reaction conditions (FeCl 3, dichloromethane) occurs for perylene-substituted porphyrins to give a porphyrin β,meso annulated with perylene rings (0.7:1 ratio of syn and anti isomers). The naphthalene, pyrene, and coronene derivatives do not react under Scholl conditions but are fused using thermal cyclodehydrogenation at high temperatures, giving mixtures of syn and anti isomers of the meso,β-fused porphyrins. For pyrenyl-substituted porphyrins, a thermal method gives synthetically acceptable yields (>30%). Absorption spectra of the fused porphyrins undergo a progressive bathochromic shift in a series of naphthyl (λ max = 730 nm), coronenyl (λ max = 780 nm), pyrenyl (λ max = 815 nm), and perylenyl (λ max = 900 nm) annulated porphyrins. Despite being conjugated with unsubstituted fused PAHs, the β,meso-fused porphyrins are more soluble and processable than the parent nonfused precursors. Pyrenyl-fused porphyrins exhibit strong fluorescence in the near-infrared (NIR) spectral region, with a progressive improvement in luminescent efficiency (up to 13% with λ max = 829 nm) with increasing degree of fusion. Fused pyrenyl-porphyrins have been used as broadband absorption donor materials in photovoltaic cells, leading to devices that show comparatively high photovoltaic efficiencies. © 2011 American Chemical Society.

  2. Microelectrophoresis of Silica Rods Using Confocal Microscopy.

    Science.gov (United States)

    Bakker, Henriëtte E; Besseling, Thijs H; Wijnhoven, Judith E G J; Helfferich, Peter H; van Blaaderen, Alfons; Imhof, Arnout

    2017-01-31

    The electrophoretic mobility and the zeta potential (ζ) of fluorescently labeled colloidal silica rods, with an aspect ratio of 3.8 and 6.1, were determined with microelectrophoresis measurements using confocal microscopy. In the case where the colloidal particles all move at the same speed parallel to the direction of the electric field, we record a xyz-stack over the whole depth of the capillary. This method is faster and more robust compared to taking xyt-series at different depths inside the capillary to obtain the parabolic flow profile, as was done in previous work from our group. In some cases, rodlike particles do not move all at the same speed in the electric field, but exhibit a velocity that depends on the angle between the long axis of the rod and the electric field. We measured the orientation-dependent velocity of individual silica rods during electrophoresis as a function of κa, where κ(-1) is the double layer thickness and a is the radius of the rod associated with the diameter. Thus, we determined the anisotropic electrophoretic mobility of the silica rods with different sized double layers. The size of the double layer was tuned by suspending silica rods in different solvents at different electrolyte concentrations. We compared these results with theoretical predictions. We show that even at already relatively high κa when the Smoluchowski limiting law is assumed to be valid (κa > 10), an orientation dependent velocity was measured. Furthermore, we observed that at decreasing values of κa the anisotropy in the electrophoretic mobility of the rods increases. However, in low polar solvents with κa < 1, this trend was reversed: the anisotropy in the electrophoretic mobility of the rods decreased. We argue that this decrease is due to end effects, which was already predicted theoretically. When end effects are not taken into account, this will lead to strong underestimation of the experimentally determined zeta potential.

  3. Detachable strong cation exchange monolith, integrated with capillary zone electrophoresis and coupled with pH gradient elution, produces improved sensitivity and numbers of peptide identifications during bottom-up analysis of complex proteomes.

    Science.gov (United States)

    Zhang, Zhenbin; Yan, Xiaojing; Sun, Liangliang; Zhu, Guijie; Dovichi, Norman J

    2015-04-21

    A detachable sulfonate-silica hybrid strong cation-exchange monolith was synthesized in a fused silica capillary, and used for solid phase extraction with online pH gradient elution during capillary zone electrophoresis-tandem mass spectrometry (CZE-MS/MS) proteomic analysis. Tryptic digests were prepared in 50 mM formic acid and loaded onto the strong cation-exchange monolith. Fractions were eluted using a series of buffers with lower concentration but higher pH values than the 50 mM formic acid background electrolyte. This combination of elution and background electrolytes results in both sample stacking and formation of a dynamic pH junction and allows use of relatively large elution buffer volumes while maintaining reasonable peak efficiency and resolution. A series of five pH bumps were applied to elute E. coli tryptic peptides from the monolith, followed by analysis using CZE coupled to an LTQ-Orbitrap Velos mass spectrometer; 799 protein groups and 3381 peptides were identified from 50 ng of the digest in a 2.5 h analysis, which approaches the identification rate for this organism that was obtained with an Orbitrap Fusion. We attribute the improved numbers of peptide and protein identifications to the efficient fractionation by the online pH gradient elution, which decreased the complexity of the sample in each elution step and improved the signal intensity of low abundance peptides. We also performed a comparative analysis using a nanoACQUITY UltraPerformance LCH system. Similar numbers of protein and peptide identifications were produced by the two methods. Protein identifications showed significant overlap between the two methods, whereas peptide identifications were complementary.

  4. A novel covalent coupling method for coating of capillaries with liposomes in capillary electrophoresis.

    Science.gov (United States)

    Mei, Jie; Xu, Jian-Rong; Xiao, Yu-Xiu; Liao, Xiao-Yan; Qiu, Guo-Fu; Feng, Yu-Qi

    2008-09-01

    A novel covalent coupling method for coating of capillaries with liposomes has been developed, which includes three steps: (i) epoxy-diol coating, (ii) activation with 2,2,2-trifluoroethanesulfonyl chloride, and (iii) liposome coupling. The coating conditions, such as the reaction time and temperature of liposome coupling, the content of dimyristoylphosphatidylethanolamine in liposomes, were optimized. Vesicles were visualized on the inner silica wall as confirmed by atomic force microscopy. The effectiveness of the coating was demonstrated by investigating the effect of pH of BGE on EOF and separating neutral compounds. The intra- and inter-capillary variations in EOF are 4.02% RSD (n=30) and 6.72% RSD (n=4) respectively, and the coated capillaries can be used to perform analysis at least for one month without any performance deterioration when stored at 4 degrees C. A set of drugs with diverse structures was applied into the developed liposome-coated CE. The normalized capacity factor (K) was introduced to quantitatively evaluate drug-membrane interactions. The relationship between log K and the fraction dose absorbed in humans (Fa%) shows that the liposome-coated CE can be utilized for in vitro prediction of Fa% of drugs that follow the transcellular passive transport route.

  5. ZIC-HILIC monolithic capillary column coupled with MALDI-MS: A tool for glycan analysis

    OpenAIRE

    Šesták, J. (Jozef); Křenková, J. (Jana); Moravcová, D. (Dana); Planeta, J. (Josef); Kahle, V. (Vladislav)

    2014-01-01

    In this contribution, we report analysis of glycans enzymatically released from bovine ribonuclease B (RNase B) and human immunoglobulin G (hIgG) combining glycan separation using the synthesized zwitterionic silica-based monolithic capillary column and off-line MALDI-MS detection.

  6. Separations using a porous-shell pillar array column on a capillary LC instrument

    NARCIS (Netherlands)

    Malsche, de D.M.W.; Bruyne, de S.; Beeck, op de J.; Eeltink, S.; Detobel, F.; Gardeniers, J.G.E.; Desmet, G.

    2012-01-01

    We investigated the achievable separation performance of a 9-cm-long and 1-mm-wide pillar array channel (volume = 0.6 μL) containing 5 μm diameter Si pillars (spacing 2.5 μm) cladded with a mesoporous silica layer with a thickness of 300 nm, when this channel is directly interfaced to a capillary LC

  7. Dynamic simulation of flywheel-type fuses

    Directory of Open Access Journals (Sweden)

    Editorial Office

    1996-07-01

    Full Text Available Rounds of ammunition are normally armed with a fuse. In this study, a fuse is developed which uses a flywheel-type mechanism controlled by time or distance. Due to its simplicity of operation and construction, the concept is expected to have high reliabil­ity. The dynamic response of all the components of this flywheel-type fuse is mathematically modelled. Simulation software was developed which connects the mathematical models of the various components. With the definition of boundary values, the response of the projectile, flywheel and other components can be determined continuously for firing and in-flight conditions.

  8. Coordination chemistry in fused-salt solutions

    Science.gov (United States)

    Gruen, D. M.

    1969-01-01

    Spectrophotometric work on structural determinations with fused-salt solutions is reviewed. Constraints placed on the method, as well as interpretation of the spectra, are discussed with parallels drawn to aqueous spectrophotometric curves of the same materials.

  9. Fuse Protects Parabolic-Dish Solar Collector

    Science.gov (United States)

    Selcuk, M. K.

    1983-01-01

    Sliding barrel and shutter protect against overheating. Downward movement of shutter initiated by melting of fuse wire that suspends it. Shutter lowered or raised under operator's control by depressuring or pressurizing hydraulic cylinder.

  10. Organometallic chemistry: Fused ferrocenes come full circle

    Science.gov (United States)

    Musgrave, Rebecca A.; Manners, Ian

    2016-09-01

    Chemists have long been fascinated by electron delocalization, from both a fundamental and applied perspective. Macrocyclic oligomers containing fused ferrocenes provide a new structural framework -- containing strongly interacting metal centres -- that is capable of supporting substantial charge delocalization.

  11. Practical capillary electrophoresis

    CERN Document Server

    Weinberger, Robert

    2000-01-01

    In the 1980s, capillary electrophoresis (CE) joined high-performance liquid chromatography (HPLC) as the most powerful separation technique available to analytical chemists and biochemists. Published research using CE grew from 48 papers in the year of commercial introduction (1988) to 1200 in 1997. While only a dozen major pharmaceutical and biotech companies have reduced CE to routine practice, the applications market is showing real or potential growth in key areas, particularly in the DNA marketplace for genomic mapping and forensic identification. For drug development involving small molecules (including chiral separations), one CE instrument can replace 10 liquid chromatographs in terms of speed of analysis. CE also uses aqueous rather than organic solvents and is thus environmentally friendlier than HPLC. The second edition of Practical Capillary Electrophoresis has been extensively reorganized and rewritten to reflect modern usage in the field, with an emphasis on commercially available apparatus and ...

  12. due to Capillary Forces

    Directory of Open Access Journals (Sweden)

    Hassen M. Ouakad

    2009-01-01

    Full Text Available We present modeling and analysis for the static behavior and collapse instabilities of doubly-clamped and cantilever microbeams subjected to capillary forces. These forces can be as a result of a volume of liquid trapped underneath the microbeam during the rinsing and drying process in fabrication. The model considers the microbeam as a continuous medium, the capillary force as a nonlinear function of displacement, and accounts for the mid-plane stretching and geometric nonlinearities. The capillary force is assumed to be distributed over a specific length underneath the microbeam. The Galerkin procedure is used to derive a reduced-order model consisting of a set of nonlinear algebraic and differential equations that describe the microbeams static and dynamic behaviors. We study the collapse instability, which brings the microbeam from its unstuck configuration to touch the substrate and gets stuck in the so-called pinned configuration. We calculate the pull-in length that distinguishes the free from the pinned configurations as a function of the beam thickness and gap width for both microbeams. Comparisons are made with analytical results reported in the literature based on the Ritz method for linear and nonlinear beam models. The instability problem, which brings the microbeam from a pinned to adhered configuration is also investigated. For this case, we use a shooting technique to solve the boundary-value problem governing the deflection of the microbeams. The critical microbeam length for this second instability is also calculated.

  13. Polydopamine-assisted immobilization of zeolitic imidazolate framework-8 for open-tubular capillary electrochromatography.

    Science.gov (United States)

    Li, Yilin; Bao, Tao; Chen, Zilin

    2017-02-01

    In this work, we developed a capillary column modified with zeolitic imidazolate framework-8 as a novel stationary phase for open-tubular capillary electrochromatography. To immobilize zeolitic imidazolate framework-8 onto the inner surface of silica capillary, a bio-inspired polydopamine functionalization was used to functionalize the capillary surface with polydopamine. First, a polydopamine layer was assembled inside the capillary. Second, due to noncovalent adsorption and covalent reaction ability, polydopamine could attract and anchor zeolitic imidazolate framework-8 onto the inner surface of capillary. It has been demonstrated that zeolitic imidazolate framework-8 was successfully grafted on the inner wall of the capillary by scanning electron microscopy, and Fourier transform infrared spectroscopy. The electro-osmotic flow characteristics of capillaries were also investigated by varying the pH value and acetonitrile content of mobile phase. The zeolitic imidazolate framework-8 coating not only increased the phase ratio of open-tubular column, but also improved the interactions between tested analytes and the stationary phase. Three groups of isomers including acidic, basic, and neutral compounds were well separated on the zeolitic imidazolate framework-8 bonded column, with theoretic plate numbers up to 1.9 × 10(5) N for catechol. The repeatability of the prepared columns was also studied, and the relative standard deviations for intra- and interday runs were less than 5%. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. New multilayer coating using quaternary ammonium chitosan and κ-carrageenan in capillary electrophoresis: application in fast analysis of betaine and methionine.

    Science.gov (United States)

    Vitali, Luciano; Della Betta, Fabiana; Costa, Ana Carolina O; Vaz, Fernando Antonio Simas; Oliveira, Marcone Augusto Leal; Vistuba, Jacqueline Pereira; Fávere, Valfredo T; Micke, Gustavo A

    2014-06-01

    The aim of this study was to develop a new multilayer coating with crosslinked quaternary ammonium chitosan (hydroxypropyltrimethyl ammonium chloride chitosan; HACC) and κ-carrageenan for use in capillary electrophoresis. A new semi-permanent multilayer coating was formed using the procedure developed and the method does not require the presence of polymers in the background electrolyte (BGE). The new capillary multilayer coating showed a cathodic electroosmotic flow (EOF) of around 30×10(-9) m(2) V(-1) s(-1) which is pH-independent in the range of pH 2 to 10. The enhanced EOF at low pH obtained contributed significantly to the development of a fast method of separation. The multilayer coating was then applied in the development of a fast separation method to determine betaine and methionine in pharmaceutical formulations by capillary zone electrophoresis (CZE). The BGE used to determine the betaine and methionine concentrations was composed of 10 mmol L(-1) tris(hydroxymethyl) aminomethane, 40 mmol L(-1) phosphoric acid and 10% (v/v) ethanol, at pH 2.1. A fused-silica capillary of 32 cm (50 µm ID×375 µm OD) was used in the experiments and samples and standards were analyzed employing the short-end injection procedure (8.5 cm effective length). The instrumental analysis time of the optimized method was 1.53 min (approx. 39 runs per hour). The validation of the proposed method for the determination of betaine and methionine showed good linearity (R(2)>0.999), adequate limit of detection (LOD <8 mg L(-1)) for the concentration in the samples and inter-day precision values lower than 3.5% (peak area and time migration). The results for the quantification of the amino acids in the samples determined by the CZE-UV method developed were statistically equal to those obtained with the comparative LC-MS/MS method according to the paired t-test with a confidence level of 95%.

  15. Online analysis of europium and gadolinium species complexed or uncomplexed with humic acid by capillary electrophoresis-inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Kautenburger, Ralf; Nowotka, Karsten; Beck, Horst Philipp

    2006-03-01

    Detailed information on the geochemical behavior of radioactive and toxic metal ions under environmental conditions (in geological matrices and aquifer systems) is needed in order to assess the long-term safety of waste repositories. This includes knowledge of the mechanisms of relevant geochemical reactions, as well as associated thermodynamic and kinetic data. Several previous studies have shown that humic acid can play an important role in the immobilization or mobilization of metal ions due to complexation and colloid formation. In our project we investigate the complexation behavior of (purified Aldrich) humic acid and its influence on the migration of the lanthanides europium and gadolinium (homologs of the actinides americium and curium) in the ternary system consisting of these heavy metals, humic acid and kaolinite (KGa-1b) under almost natural conditions. Capillary electrophoresis (CE, Beckman Coulter P/ACE MDQ), with its excellent separation performance, was hyphenated with a homemade interface to inductively coupled plasma mass spectrometry (ICP-MS, VG Elemental PlasmaQuad 3) giving a system that is highly sensitive to the rare-earth element species of europium and gadolinium with humic acid. The humic acid used was also halogenated with iodine, which acted as an ICP-MS marker. To couple CE to ICP-MS, a fused silica CE capillary was flexibly fitted into a MicroMist 50 mul nebulizer with a Cinnabar cyclonic spray chamber in the external homemade interface. The chamber was chilled to a temperature of 4 degrees C to optimize the sensitivity. 200 ppb of cesium were added to the CE separation buffer so that the capillary flow could be observed. A make-up fluid including 4 ppb Ho as an internal standard was combined with the flow from the capillary within the interface in order to get a fluid throughput high enough to maintain continuous nebulization. Very low detection limits were achieved: 125 ppt for 153Eu and 250 ppt for 158Gd. Using this optimized CE

  16. Polydopamine-assisted partial hydrolyzed poly(2-methyl-2-oxazolinze) as coating for determination of melamine in milk by capillary electrophoresis.

    Science.gov (United States)

    Zhang, Yalin; Chen, Lijuan; Zhang, Chong; Liu, Songtao; Zhu, Haikun; Wang, Yanmei

    2016-04-01

    Nitrogen-rich melamine (66% by mass) had been found to be illegally adulterated to milk products and animal feed in order to increase the apparent protein content, and ingestion of melamine may lead to the formation of kidney stones. Hence, the development of reliable analytical methods for the monitoring of melamine in milk products is necessary. The common methods for melamine analysis in milk products are performed via GC-MS or HPLC, however, these procedures require a large of organic solvent and several pretreatment steps. In this study, a new and facile approach was developed to modify a fused-silica capillary inner surface based on poly(dopamine) (PDA) and partial hydrolyzed poly(2-methyl-2-oxazoline) (PMOXA-EI) mixed coating, which was used to determine the melamine in milk powder quantitatively by capillary electrophoresis with ultraviolet (CE-UV) detection with simple analytes pretreatment. Firstly, the influences of the molecular mass of poly(2-methyl-2-oxazoline) (PMOXA), the hydrolysis degree of PMOXA, and the concentration ratio of DA to PMOXA-EI on the separation properties of a mixture of four basic proteins (cytochrome c, lysozyme, ribonuclease A, and α-chymotrypsinogen A) were studied in detail. As a consequence, fast and efficient separation of four proteins was obtained using PDA/PMOXA1k-EI0.4 coating (once coating). Then, a modified facile coating workflow was carried out to acquire a novel twice coating (i.e. PDA/PMOXA1k-EI0.4+PMOXA1k-EI0.4 coated capillary) for highly sensitive and stable analysis of melamine. Under the optimal conditions, the linear response of melamine concentration ranged from 6.25 to 100 µg/mL with high correlation coefficient of 0.9910, and the limit of detection (LOD) for melamine was 0.097 µg/mL. The minimum amount of melamine determined in milk powder with our proposed method was 4 mg/kg. The recoveries and relative standard deviations (RSDs) were 92.13-102.47%, 92.22-100.30%, 2.07-4.98%, and 2

  17. High-temperature solvent stability of sol-gel germania triblock polymer coatings in capillary microextraction on-line coupled to high-performance liquid chromatography.

    Science.gov (United States)

    Segro, Scott S; Malik, Abdul

    2010-09-10

    Germania-based sol-gel organic-inorganic hybrid coatings were prepared for on-line coupling of capillary microextraction with high-performance liquid chromatography. For this, a germania-based sol-gel precursor, tetra-n-butoxygermane and a hydroxy-terminated triblock copolymer, poly(ethylene oxide)-block-poly(propylene oxide)-block-poly(ethylene oxide) were used. These sol-gel germania triblock polymer coatings were chemically anchored to the inner walls of a fused silica capillary (0.25 mm I.D.) in course of its evolution from the sol solution. Scanning electron microscopy images of the sol-gel germania triblock polymer coating were obtained to estimate the coating thickness. For the first time, the analyte distribution constants between a sol-gel germania organic-inorganic hybrid coating and the samples (K(cs)) were determined. For a variety of analytes from different chemical classes, including polycyclic aromatic hydrocarbons (PAHs), ketones, alcohols, phenols and amines, the K(cs) values ranged from 8.1 x 10(1) to 5.6 x 10(4). Also, for the first time, the stability of the sol-gel germania-based coating in high-temperature reversed-phase solvent environment was evaluated. The sol-gel germania triblock polymer coatings were capable of surviving exposure to high-temperature solvent conditions (200 degrees C) with little change in extraction capabilities. This demonstrates that sol-gel germania triblock polymer hybrid materials might be suitable for further applications in high-temperature HPLC. The reproducibility of the method for preparation of the sol-gel germania triblock polymer coatings was also evaluated, and the capillary-to-capillary RSD values ranged from 5.3 to 6.5%. The use of higher flow rates in extraction was found to significantly reduce the time required (from 30-40 to 10-15 min) to reach equilibrium between the sol-gel germania triblock polymer coating and the analytes in the sample solution.

  18. Rapid confirmation of enzyme multiplied immunoassay technique (EMIT) cocaine positive urine samples by capillary gas-liquid chromatography/nitrogen phosphorus detection (GLC/NPD).

    Science.gov (United States)

    Verebey, K; DePace, A

    1989-01-01

    A rapid gas-liquid chromatographic (GLC) method was developed for the confirmation of benzoylecgonine (BE) positive urine samples screened by the enzyme multiplied immunoassay technique (EMIT) assay. The procedure is performed by solvent extraction of BE from 0.1 or 0.2 mL of urine, followed by an aqueous wash of the solvent and evaporation. The dried residue was derivatized with 50 microL of pentafluoropropionic anhydride and 25 microL of pentafluoropropropanol at 90 degrees C for 15 min. The derivatizing reagents were evaporated to dryness, and the derivatized BE, and cocaine if present, were reconstituted and injected into the gas chromatograph. The column was a 15-m by 0.2-mm fused silica capillary column, coated with 0.25 micron of DB-1, terminating in a nitrogen phosphorus detector (NPD). Cocaine and the pentafluoro BE derivatives retention times were 3.2 and 2.6 min, respectively. Nalorphine was used as reference or internal standard with a retention time of 4.78 min. The complete procedure can be performed in approximately 1.5 h. The EMIT cutoff between positive and negative urine samples is 300 ng/mL of BE. The lower limit of sensitivity of this method is 25 ng of BE extracted from urine. Validation studies resulted in confirmation of 101 out of 121 EMIT cocaine positive urine samples that could not be confirmed by thin-layer chromatography (TLC). This represents 84% confirmation efficiency.

  19. Monolithic poly (SPE-co-BVPE) capillary columns as a novel hydrophilic interaction liquid chromatography stationary phase for the separation of polar analytes.

    Science.gov (United States)

    Foo, Hsiao Ching; Heaton, James; Smith, Norman W; Stanley, Shawn

    2012-10-15

    A novel hydrophilic interaction liquid chromatography (HILIC) stationary phase was prepared by the co-polymerisation of zwitterionic N,N'-dimethyl-N-methacryloxyethyl-N-(3-sulfopropyl) ammonium betaine (SPE) and the crosslinker 1,2-bis(p-vinylphenyl) ethane (BVPE) in the presence of the porogens, toluene and methanol. Monolithic columns were produced by carrying out the α,α'-azoisobutyronitrile (AIBN) initiated reaction for 1, 2, 4, 8 and 12 h inside a 200 μm i.d. fused silica capillary at 75°C (water bath). The optimum polymerisation time was shown to be 2 h, as this resulted in good porosity, due to enlarged flow-channels and the presence of a higher proportion of mesopores provided a relatively larger surface area than the other columns. The chromatographic properties of the optimised poly (SPE-co-BVPE) monolithic column were evaluated with test mixtures containing both basic and neutral compounds in the HILIC gradient separation mode. This produced relatively sharp peaks (average peak width at half height=0.1 min) with average asymmetry factors of 1.4 and baseline resolution was obtained for all the compounds. Using the isocratic separation of the test mixture, the number of theoretical plates (N) per metre calculated was between 26,888 and 35,930 by using average values obtained for triplicate injections of the compounds thiourea, toluene and acrylamide.

  20. SILICA SURFACED CARBON FIBERS.

    Science.gov (United States)

    carbon fibers . Several economical and simple processes were developed for obtaining research quantities of silica surfaced carbon filaments. Vat dipping processes were utilized to deposit an oxide such as silica onto the surface and into the micropores of available carbon or graphite base fibers. High performance composite materials were prepared with the surface treated carbon fibers and various resin matrices. The ablative characteristics of these composites were very promising and exhibited fewer limitations than either silica or...treated

  1. Quantitative evaluation of fiber fuse initiation with exposure to arc discharge provided by a fusion splicer

    Science.gov (United States)

    Todoroki, Shin-Ichi

    2016-05-01

    The optical communication industry and power-over-fiber applications face a dilemma as a result of the expanding demand of light power delivery and the potential risks of high-power light manipulation including the fiber fuse phenomenon, a continuous destruction of the fiber core pumped by the propagating light and triggered by a heat-induced strong absorption of silica glass. However, we have limited knowledge on its initiation process in the viewpoint of energy flow in the reactive area. Therefore, the conditions required for a fiber fuse initiation in standard single-mode fibers were determined quantitatively, namely the power of a 1480 nm fiber laser and the arc discharge intensity provided by a fusion splicer for one second as an outer heat source. Systematic investigation on the energy flow balance between these energy sources revealed that the initiation process consists of two steps; the generation of a precursor at the heated spot and the transition to a stable fiber fuse. The latter step needs a certain degree of heat accumulation at the core where waveguide deformation is ongoing competitively. This method is useful for comparing the tolerance to fiber fuse initiation among various fibers with a fixed energy amount that was not noticed before.

  2. Preparation of hybrid monolithic columns via "one-pot" photoinitiated thiol-acrylate polymerization for retention-independent performance in capillary liquid chromatography.

    Science.gov (United States)

    Zhang, Haiyang; Ou, Junjie; Liu, Zhongshan; Wang, Hongwei; Wei, Yinmao; Zou, Hanfa

    2015-09-01

    A novel "one-pot" approach was developed for ultrarapid preparation of various hybrid monolithic columns in UV-transparent fused-silica capillaries via photoinitiated thiol-acrylate polymerization of an acrylopropyl polyhedral oligomertic silsesquioxane (acryl-POSS) and a monothiol monomer (1-octadecanethiol or sodium 3-mercapto-1-propanesulfonate) within 5 min, in which the acrylate not only homopolymerizes, but also couples with the thiol. This unique combination of two types of free-radical reaction mechanisms offers a simple way to fabricate various acrylate-based hybrid monoliths. The physical characterization, including scanning electron microscopy (SEM), Fourier transform infrared (FT-IR) spectroscopy, and thermal gravimetric analysis was performed. The results indicated that the monothiol monomers were successfully incorporated into acryl-POSS-based hybrid monoliths. The column efficiencies for alkylbenzenes on the C18-functionalized hybrid monolithic column reached to 60 000-73 500 plates/m at the velocity of 0.33 mm/s in capillary liquid chromatography, which was far higher than that of previously reported POSS-based columns prepared via thermal-initiated free-radical polymerization without adding any thiol monomers. By plotting the plate height (H) of the alkylbenzenes versus the linear velocity (u) of the mobile phase, the results revealed a retention-independent efficient performance of small molecules in the isocratic elution. These results indicated that more homogeneous hybrid monoliths formed via photoinitiated thiol-acrylate polymerization; particularly, the use of the multifunctional cross-linker possibly prevented the generation of gel-like micropores, reducing mass transfer resistance (C-term). Another sulfonate-containing hybrid monolithic column also exhibited hydrophobicity and ion-exchange mechanism, and the dynamic binding capacity was calculated as 71.1 ng/cm (75 μm i.d.).

  3. Capillary electrophoresis with capacitively coupled contactless conductivity detection for the determination of cis/trans isomers of octadec-9-enoic acid and other long chain fatty acids.

    Science.gov (United States)

    Wong, Yong Foo; Saad, Bahruddin; Makahleh, Ahmad

    2013-05-17

    A capillary electrophoresis (CE)-capacitively coupled contactless conductivity detection (C(4)D) method for the simultaneous separation of eleven underivatized fatty acids (FAs), namely, lauric, myristic, tridecanoic (internal standard), pentadecanoic, palmitic, stearic, oleic, elaidic, linoleic, linolenic and arachidic acids is described. The separation was carried out in normal polarity mode at 20 °C, 30 kV and using hydrodynamic injection (50 mbar for 1 s). The separation was achieved in a bare fused-silica capillary (70 cm × 75 μm i.d.) using a background electrolyte of methyl-β-cyclodextrin (~6 mM) and heptakis-(2,3,6-tri-O-methyl)-β-cyclodextrin (~8 mM) dissolved in a mixture of Na2HPO4/KH2PO4 (5 mM, pH 7.4):ACN:MeOH:n-octanol (3:4:2.5:0.5, v/v/v/v). C(4)D parameters were set at fixed amplitude of 100 V and frequency of 1000 kHz. The developed method was validated. Calibration curves of the ten FAs were well correlated (r(2)>0.99) within the range of 5-250 μg mL(-1) for lauric acid, and 3-250 μg mL(-1) for the other FAs. The method was simple and sensitive with detection limits (S/N=3) of 0.9-1.9 μg mL(-1) and good relative standard deviations of intra- and inter-day for migration times and peak areas (≤9.7%) were achieved. The method was applied to the determination of FAs in margarine samples. The proposed method offers distinct advantages over the GC and HPLC methods, especially in terms of simplicity (without derivatization) and sensitivity.

  4. Use of tube radial distribution of ternary mixed carrier solvents for introduction of absorption reagent for metal ion separation and online detection into capillary.

    Science.gov (United States)

    Fujinaga, Satoshi; Jinno, Naoya; Hashimoto, Masahiko; Tsukagoshi, Kazuhiko

    2011-10-01

    When ternary mixed solvents consisting of water-hydrophilic/hydrophobic organic solvents are fed into a micro-space under laminar flow conditions, the solvent molecules are radially distributed in the micro-space. The specific fluidic behavior of the solvents is called the "tube radial distribution phenomenon (TRDP)". A novel capillary chromatography method was developed based on the TRDP that creates the inner major and outer minor phases in a tube, where the outer phase acts as a pseudo-stationary phase. This is called "tube radial distribution chromatography (TRDC)". In this study, Chrome Azurol S as an absorption reagent was introduced into the TRDC system for metal ion separation and online detection. The fused-silica capillary tube (75 μm id and 110 cm length) and water-acetonitrile-ethyl acetate mixture (3:8:4 volume ratio) including 20 mM Chrome Azurol S as a carrier solution were used. Metal ions, i.e. Co(II), Cu(II), Ni(II), Al(III), and Fe(III), as models were injected into the present TRDC system. Characteristic individual absorption characteristics and elution times were obtained as the result of complex formation between the metal ions and Chrome Azurol S in the water-acetonitrile-ethyl acetate mixture solution. The elution times of the metal ions were examined based on their absorption behavior; Co(II), Ni(II), Al(III), Fe(III), and Cu(II) were eluted in this order over the elution times of 4.7-6.8 min. The elution orders were determined from the molar ratios of metal ion to Chrome Azurol S and Irving-Williams series for bivalent metal ions. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. A capillary electrophoresis-mass spectrometry based method for the screening of β-secretase inhibitors as potential Alzheimer's disease therapeutics.

    Science.gov (United States)

    Schejbal, Jan; Slezáčková, Lucie; Řemínek, Roman; Glatz, Zdeněk

    2017-03-03

    In this work a novel capillary electrophoresis-mass spectrometry (CE-MS) based method was developed and validated for the assay of β-secretase (BACE1) activity as a potential target for Alzheimer's disease (AD) treatment. In contrast with the typically used Förster resonance energy transfer (FRET) assays, an unlabelled decapeptide derived from the amyloid precursor protein BACE1 site with the "Swedish mutation" was used as the substrate. The CE usage enabled the enzymatic reaction to be carried out in as small a volume as 100μL in 60min with sufficient yields of proteolytic product, which was subsequently separated in a bare fused silica capillary using 12.5% acetic acid as a background electrolyte and detected by MS. The limits of detection and quantitation were estimated using the signal to noise ratio to be 5nM (S/N=3) and 15nM (S/N=10), respectively, both being well below the working range for kinetic and inhibition studies. Its applicability for the kinetic study of BACE1 was demonstrated using optimized enzyme assay conditions and the estimated kinetic parameter values were confirmed by classic CE-UV analyses. The method was finally used for the main purpose for which it was developed - to screen BACE1 inhibitors as potential AD therapeutics. The resulting kinetic and inhibition parameters values were compared to those published in the literature, which were almost exclusively obtained by FRET based assays. These comparisons brought up several issues that are further discussed below and favour the application of an unlabelled substrate. The proposed CE-MS based method offers a high-throughput capability for new drug development.

  6. Rapid quantitative analysis of phenazine-1-carboxylic acid and 2-hydroxyphenazine from fermentation culture of Pseudomonas chlororaphis GP72 by capillary zone electrophoresis.

    Science.gov (United States)

    Liu, Hai-Ming; Zhang, Xue-Hong; Huang, Xian-Qing; Cao, Cheng-Xi; Xu, Yu-Quan

    2008-07-15

    Natural phenazines in secondary metabolites of bacteria have been receiving increasing attention in recent years due to their potential usage as antibiotics. In the present study, a rapid and reliable capillary zone electrophoresis (CZE) method was developed and validated for monitoring for the first time dynamic phenazine-1-carboxylic acid (PCA) and the 2-hydroxyphenazine (2-OH-PHZ) production of Pseudomonas chlororaphis GP72 during the entire fermentation cycle. The paper begins with the optimization of separate conditions for 2-OH-PHZ and PCA together with phenazine (PHZ), which is used as internal standard. The optimized conditions are: 10mM, pH 7.3 phosphate buffer, a fused-silica capillary with a total length of 49 cm x 75 microm ID, 375 microm OD with an effective length of 40 cm, 25 kV, 13 mbar 10s pressure sample injection and 25 degrees C air-cooling. The three compounds could be separated within 2 min under optimized conditions. The validation of the newly developed study shows the linear response of 2-OH-PHZ and PCA ranging from 10 to 250 microg mL(-1) with high correlation coefficient (r=0.9997 and 0.9993, n=7), low limits of detection (0.47 and 0.38 microg mL(-1)) and quantification (1.56 and 1.28 microg mL(-1)), respectively. Good precision values for intra- and inter-day detection and acceptable individual recovery ranges for 2-OH-PHZ and PCA are indicated. The newly developed method was also validated through monitoring dynamic PCA and 2-OH-PHZ production of P. chlororaphis GP72 during an 84 h growth cycle.

  7. Fast and sensitive method to determine parabens by capillary electrophoresis using automatic reverse electrode polarity stacking mode: application to hair samples.

    Science.gov (United States)

    Sako, Alysson V F; Dolzan, Maressa D; Micke, Gustavo Amadeu

    2015-09-01

    This paper describes a fast and sensitive method for the determination of methyl, ethyl, propyl, and butylparaben in hair samples by capillary electrophoresis using automatic reverse electrode polarity stacking mode. In the proposed method, solutions are injected using the flush command of the analysis software (940 mbar) and the polarity switching is carried out automatically immediately after the sample injection. The advantages compared with conventional stacking methods are the increased analytical frequency, repeatability, and inter-day precision. All analyses were performed in a fused silica capillary (50 cm, 41.5 cm in effective length, 50 μm i.d.), and the background electrolyte was composed of 20 mmol L(-1) sodium tetraborate in 10 % of methanol, pH 9.3. For the reverse polarity, -25 kV/35 s was applied followed by application of +30 kV for the electrophoretic run. Temperature was set at 20 °C, and all analytes were monitored at 297 nm. The method showed acceptable linearity (r (2) > 0.997) in the studied range of 0.1-5.0 mg L(-1), limits of detection below 0.017 mg L(-1), and inter-day, intra-day, and instrumental precision better than 6.2, 3.6, and 4.6 %, respectively. Considering parabens is widely used as a preservative in many products and the reported possibility of damage to the hair and also to human health caused by these compounds, the proposed method was applied to evaluate the adsorption of parabens in hair samples. The results indicate that there is a greater adsorption of methylparaben compared to the other parabens tested and also dyed hairs had a greater adsorption capacity for parabens than natural hairs.

  8. Stability-indicating capillary zone electrophoresis method for the assessment of recombinant human interleukin-11 and its correlation with reversed-phase liquid chromatography and biossay.

    Science.gov (United States)

    Souto, Ricardo Bizogne; Stamm, Fernanda Pavani; Schumacher, Jéssica Barbieri; Cardoso, Clovis Dervil Appratto; de Freitas, Guilherme Weber; Perobelli, Rafaela Ferreira; Dalmora, Sérgio Luiz

    2014-06-01

    A stability-indicating capillary zone electrophoresis (CZE) method was validated for the analysis of recombinant human interleukin-11(rhIL-11) using rupatadine fumarate, as internal standard (IS). A fused-silica capillary, (50 µm i.d.; effective length, 40 cm) was used at 25°C; the applied voltage was 20 kV. The background electrolyte solution consisted of 50 mmol L(-1) sodium dihydrogen phosphate solution at pH 3.0. Injections were performed using a pressure mode at 50 mbar for 45 s, with detection by photodiode array detector set at 196 nm. Specificity and stability-indicating capability were established in degradation studies, which also showed that there was no interference of the excipients. The method was linear over the concentration range of 1.0-300 µg mL(-1) (r(2)=0.9992) and the limit of detection (LOD) and limit of quantitation (LOQ) were 0.2 µg mL(-1) and 1.0 µg mL(-1), respectively. The accuracy was 100.4% with bias lower than 1.1%. Moreover, the in vitro cytotoxicity test of the degraded products showed significant differences (pmethod was applied for the content/potency assessment of rhIL-11 in biopharmaceutical formulations, and the results were correlated to those of a validated reversed-phase LC method (RP-LC) and an TF-1 cell culture assay, showing non-significant differences (p>0.05). In addition the CZE and RP-LC methods were applied for the analysis of rhIL-11 in human plasma. Therefore, the proposed alternative method can be applied to monitor stability, to assure the batch-to-batch consistency and quality of the bulk and finished biotechnology-derived medicine.

  9. Determination of alternative and conventional chelating agents as copper(II) complexes by capillary zone electrophoresis--the first use of didecyldimethylammonium bromide as a flow reversal reagent.

    Science.gov (United States)

    Laamanen, Pirkko-Leena; Matilainen, Rose

    2007-02-12

    A capillary zone electrophoresis (CZE) method for analyzing 11 chelating agents [beta-alaninediacetic acid (beta-ADA), trans-1,2-diaminocyclohexane-N,N,N',N'-tetraacetic acid (CDTA), diethylenetriaminepentaacetic acid (DTPA), ethylenediaminetetraacetic acid (EDTA), N-(2-hydroxyethyl)ethylenediamine-N,N',N'-triacetic acid (HEDTA), N-(2-hydroxyethyl)iminodiacetic acid (HEIDA), iminodiacetic acid (IDA), methylglycinediacetic acid (MGDA), nitrilotriacetic acid (NTA), 1,3-diaminopropane-N,N,N',N'-tetraacetic acid (PDTA) and triethylenetetraaminehexaacetic acid (TTHA)] as negatively charged copper(II) complexes has been established. Both conventional and alternative chelating agents were included in this study, because they are used side by side in industrial applications. In this study, didecyldimethylammonium bromide (DMDDAB) was successfully used as a flow reversal reagent for the first time in an aqueous CZE method based on phosphate BGE with UV spectrophotometric detection. In addition this new flow modifier was compared to common TTAB. Method development was done using a fused silica capillary (61 cm x 50 microm i.d.). The optimized BGE was a 105 mmol L(-1) phosphate buffer with TTAB or DMDDAB in the concentration 0.5 mmol L(-1) at pH 7.1. The measurements were done with -20 kV voltage using direct UV detection at 254 nm. In both CZE methods all 11 analyte zones were properly separated (resolutions > or =2.4), and the calibrations gave excellent correlation coefficients (> or =0.998; linear range tested 0.5-2.0 mmol L(-1)). The limits of detection were < or =34 and < or =49 micromol L(-1) with the method of DMDDAB and TTAB, respectively. A clear benefit of both methods was the short analysis time; all 11 complexes were detected in less than 6 and 5.5 min with the methods of TTAB and DMDDAB, respectively. The two methods were tested with dishwashing detergents and paper mill wastewater samples and proved to be suitable for practical use.

  10. 'Click' chemistry synthesis and capillary electrophoresis study of 1,4-linked 1,2,3-triazole AZT-systemin conjugate.

    Science.gov (United States)

    Dobkowski, Michał; Szychowska, Aleksandra; Pieszko, Małgorzata; Miszka, Anna; Wojciechowska, Monika; Alenowicz, Magdalena; Ruczyński, Jarosław; Rekowski, Piotr; Celewicz, Lech; Barciszewski, Jan; Mucha, Piotr

    2014-09-01

    The Cu(I) catalyzed Huisgen 1,3-dipolar azide-alkyne cycloaddition (CuAAC) was applied for a nucleoside-peptide bioconjugation. Systemin (Sys), an 18-aa plant signaling peptide naturally produced in response to wounding or pathogen attack, was chemically synthesized as its N-propynoic acid functionalized analog (Prp-Sys) using the SPPS. Next, CuAAC was applied to conjugate Prp-Sys with 3'-azido-2',3'-dideoxythymidine (AZT), a model cargo molecule. 1,4-Linked 1,2,3-triazole AZT-Sys conjugate was designed to characterize the spreading properties and ability to translocate of cargo molecules of systemin. CuAAC allowed the synthesis of the conjugate in a chemoselective and regioselective manner, with high purity and yield. The presence of Cu(I) ions generated in situ drove the CuAAC reaction to completion within a few minutes without any by-products. Under typical separation conditions of phosphate 'buffer' at low pH and uncoated fused bare-silica capillary, an increasing peak intensity assigned to triazole-linked AZT-Sys conjugate was observed using capillary electrophoresis (CE) during CuAAC. CE analysis showed that systemin peptides are stable in tomato leaf extract for up to a few hours. CE-ESI-MS revealed that the native Sys and its conjugate with AZT are translocated through the tomato stem and can be directly detected in stem exudates. The results show potential application of systemin as a transporter of low molecular weight cargo molecules in tomato plant and of CE method to characterize a behavior of plant peptides and its analogs.

  11. Sol-gel germania triblock polymer coatings of exceptional pH stability in capillary microextraction online-coupled to high-performance liquid chromatography.

    Science.gov (United States)

    Segro, Scott S; Triplett, Judy; Malik, Abdul

    2010-05-15

    For the first time, a germania-based sol-gel coating was used in capillary microextraction (CME) in combination with high-performance liquid chromatography (HPLC). A hydroxy-terminated triblock copolymer, poly(ethylene oxide)-block-poly(propylene oxide)-block-poly(ethylene oxide), was covalently bonded into a sol-gel germania matrix in the course of its creation from an alkoxide precursor via hydrolytic polycondensation reactions. A thin layer of this in situ-created sol-gel hybrid material was covalently anchored to the inner walls of a 0.25 mm i.d. fused silica capillary to produce a sol-gel germania triblock polymeric sorbent in the form of a highly stable surface coating. Such a coating served as an effective extracting phase for the preconcentration of a wide range of polar and nonpolar analytes (e.g., alcohols, amines, ketones, phenols, and polycyclic aromatic hydrocarbons) with nanomolar and picomolar detection limits. Most significantly, the sol-gel germania triblock polymer coating demonstrated impressive resistance to extreme pH conditions, surviving 5 days of continuous exposure to 1.0 M HCl (pH approximately 0.0) or 1.0 M NaOH (pH approximately 14.0), practically without any changes in performance. This shows the suitability of sol-gel germania hybrid organic-inorganic hybrid materials for use as sorbents or stationary phases under extreme pH conditions, often needed in a variety of separation and sample preparation techniques and applications, including ion chromatography, hydrophobic interaction chromatography, proteomics, HPLC with electrochemical detection, isoelectric focusing, and extraction of acidic and basic analytes.

  12. Preparation and evaluation of poly(alkyl methacrylate-co-methacrylic acid-co-ethylene dimethacrylate) monolithic columns for separating polar small molecules by capillary liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Lin, Shu-Ling; Wu, Yu-Ru; Lin, Tzuen-Yeuan; Fuh, Ming-Ren, E-mail: msfuh@scu.edu.tw

    2015-04-29

    Highlights: • Methacrylic acid (MAA) was used to increase hydrophilicity of polymeric monoliths. • Fast separation of phenol derivatives was achieved in 5 min using MAA-incorporated column. • Separations of aflatoxins and phenicol antibiotics were achieved using MAA-incorporated column. - Abstract: In this study, methacrylic acid (MAA) was incorporated with alkyl methacrylates to increase the hydrophilicity of the synthesized ethylene dimethacrylate-based (EDMA-based) monoliths for separating polar small molecules by capillary LC analysis. Different alkyl methacrylate–MAA ratios were investigated to prepare a series of 30% alkyl methacrylate–MAA–EDMA monoliths in fused-silica capillaries (250-μm i.d.). The porosity, permeability, and column efficiency of the synthesized MAA-incorporated monolithic columns were characterized. A mixture of phenol derivatives is employed to evaluate the applicability of using the prepared monolithic columns for separating small molecules. Fast separation of six phenol derivatives was achieved in 5 min with gradient elution using the selected poly(lauryl methacrylate-co-MAA-co-EDMA) monolithic column. In addition, the effect of acetonitrile content in mobile phase on retention factor and plate height as well as the plate height-flow velocity curves were also investigated to further examine the performance of the selected poly(lauryl methacrylate-co-MAA-co-EDMA) monolithic column. Moreover, the applicability of prepared polymer-based monolithic column for potential food safety applications was also demonstrated by analyzing five aflatoxins and three phenicol antibiotics using the selected poly(lauryl methacrylate-co-MAA-co-EDMA) monolithic column.

  13. Silica in higher plants.

    Science.gov (United States)

    Sangster, A G; Hodson, M J

    1986-01-01

    Opaline silica deposits are formed by many vascular (higher) plants. The capacity of these plants for silica absorption varies considerably according to genotype and environment. Plant communities exchange silica between soil and vegetation, especially in warmer climates. Silica deposition in epidermal cell walls offers mechanical and protective advantages. Biogenic silica particles from plants are also implicated in the causation of cancer. Recent techniques are reviewed which may aid in the identification of plant pathways for soluble silica movement to deposition sites and in the determination of ionic environments. Botanical investigations have focused on silicification of cell walls in relation to plant development, using scanning and transmission electron microscopy combined with X-ray microanalysis. Silica deposition in macrohair walls of the lemma of canary grass (Phalaris) begins at inflorescence emergence and closely follows wall thickening. The structure of the deposited silica may be determined by specific organic polymers present at successive stages of wall development. Lowering of transpiration by enclosure of Phalaris inflorescences in plastic bags reduced silica deposition in macrohairs. Preliminary freeze-substitution studies have located silicon, as well as potassium and chloride, in the cell vacuole and wall deposition sites during initial silicification.

  14. Filamentation of ultrashort laser pulses in silica glass and KDP crystal: A comparative study

    CERN Document Server

    Rolle, Jérémie; Duchateau, Guillaume; Skupin, Stefan

    2014-01-01

    Ionizing 800-nm femtosecond laser pulses propagating in silica glass and in potassium dihydrogen phosphate (KDP) crystal are investigated by means of a unidirectional pulse propagation code. Filamentation in fused silica is compared with the self-channeling of light in KDP accounting for the presence of defect states and electron-hole dynamics. In KDP, laser pulses produce intense filaments with higher clamping intensities up to 200 TW/cm$^2$ and longer plasma channels with electron densities above $10^{16}$ cm$^{-3}$. Despite these differences, the propagation dynamics in silica and KDP are almost identical at equivalent ratios of input power over the critical power for self-focusing.

  15. Fuse Modeling for Reliability Study of Power Electronics Circuits

    DEFF Research Database (Denmark)

    Bahman, Amir Sajjad; Iannuzzo, Francesco; Blaabjerg, Frede

    2017-01-01

    This paper describes a comprehensive modeling approach on reliability of fuses used in power electronic circuits. When fuses are subjected to current pulses, cyclic temperature stress is introduced to the fuse element and will wear out the component. Furthermore, the fuse may be used in a large...

  16. Fuse Modeling for Reliability Study of Power Electronics Circuits

    DEFF Research Database (Denmark)

    Bahman, Amir Sajjad; Iannuzzo, Francesco; Blaabjerg, Frede

    2017-01-01

    This paper describes a comprehensive modeling approach on reliability of fuses used in power electronic circuits. When fuses are subjected to current pulses, cyclic temperature stress is introduced to the fuse element and will wear out the component. Furthermore, the fuse may be used in a large...

  17. Wafer-fused semiconductor radiation detector

    Science.gov (United States)

    Lee, Edwin Y.; James, Ralph B.

    2002-01-01

    Wafer-fused semiconductor radiation detector useful for gamma-ray and x-ray spectrometers and imaging systems. The detector is fabricated using wafer fusion to insert an electrically conductive grid, typically comprising a metal, between two solid semiconductor pieces, one having a cathode (negative electrode) and the other having an anode (positive electrode). The wafer fused semiconductor radiation detector functions like the commonly used Frisch grid radiation detector, in which an electrically conductive grid is inserted in high vacuum between the cathode and the anode. The wafer-fused semiconductor radiation detector can be fabricated using the same or two different semiconductor materials of different sizes and of the same or different thicknesses; and it may utilize a wide range of metals, or other electrically conducting materials, to form the grid, to optimize the detector performance, without being constrained by structural dissimilarity of the individual parts. The wafer-fused detector is basically formed, for example, by etching spaced grooves across one end of one of two pieces of semiconductor materials, partially filling the grooves with a selected electrical conductor which forms a grid electrode, and then fusing the grooved end of the one semiconductor piece to an end of the other semiconductor piece with a cathode and an anode being formed on opposite ends of the semiconductor pieces.

  18. OPUS: the FUSE science data pipeline

    Science.gov (United States)

    Rose, James F.; Heller-Boyer, C.; Rose, M. A.; Swam, M.; Miller, W.; Kriss, G. A.; Oegerle, William R.

    1998-07-01

    This paper describes how the OPUS pipeline, currently used for processing science data from the Hubble Space Telescope (HST), was used as the backbone for developing the science data pipeline for a much smaller mission. The far ultraviolet spectroscopic explorer (FUSE) project selected OPUS for its data processing pipeline platform and selected the OPUS team at the STScI to write the FUSE pipeline applications. A total of 105 new modules were developed for the FUSE pipeline. The foundation of over 250 modules in the OPUS libraries allowed development to proceed quickly and with considerable confidence that the underlying functionality is reliable and robust. Each task represented roughly 90 percent reuse, and the project as a whole shows over 70 percent reuse of the existing OPUS system. Taking an existing system that is operational, and will be maintained for many years to come, was a key decision for the FUSE mission. Adding the extensive experience of the OPUS team to the task resulted in the development of a complete telemetry pipeline system within a matter of months. Reusable software has been the siren song of software engineering and object- oriented design for a decade or more. The development of inexpensive software systems by adapting existing code to new applications is as attractive as it has been elusive. The OPUS telemetry pipeline for the FUSE mission has proven to be a significant exception to that trend.

  19. Surface-dependent chemical equilibrium constants and capacitances for bare and 3-cyanopropyldimethylchlorosilane coated silica nanochannels

    DEFF Research Database (Denmark)

    Andersen, Mathias Bækbo; Frey, Jared; Pennathur, Sumita

    2011-01-01

    We present a combined theoretical and experimental analysis of the solid–liquid interface of fused-silica nanofabricated channels with and without a hydrophilic 3-cyanopropyldimethylchlorosilane (cyanosilane) coating. We develop a model that relaxes the assumption that the surface parameters C1, C2...... filling length ratio on ionic strength for different surface compositions, which can be difficult to achieve otherwise....

  20. Endodontic and post-endodontic management of a fused molar

    Directory of Open Access Journals (Sweden)

    Ruchi Gupta

    2013-01-01

    Full Text Available Treatment of fused teeth needs special care and attention to the bizarre anatomy. This paper describes root canal treatment of a fused carious tooth presenting with apical periodontitis. It is a rare case of fusion of the mandibular second molar with a paramolar. There is no literature regarding placement of crown over endodontically treated fused teeth. In this case, the fused teeth were endodontically treated and restored by a porcelain fused to metal crown.

  1. Crystalline Silica Primer

    Science.gov (United States)

    ,

    1992-01-01

    Crystalline silica is the scientific name for a group of minerals composed of silicon and oxygen. The term crystalline refers to the fact that the oxygen and silicon atoms are arranged in a threedimensional repeating pattern. This group of minerals has shaped human history since the beginning of civilization. From the sand used for making glass to the piezoelectric quartz crystals used in advanced communication systems, crystalline silica has been a part of our technological development. Crystalline silica's pervasiveness in our technology is matched only by its abundance in nature. It's found in samples from every geologic era and from every location around the globe. Scientists have known for decades that prolonged and excessive exposure to crystalline silica dust in mining environments can cause silicosis, a noncancerous lung disease. During the 1980's, studies were conducted that suggested that crystalline silica also was a carcinogen. As a result of these findings, crystalline silica has been regulated under the Occupational Safety and Health Administration's (OSHA) Hazard Communication Standard (HCS). Under HCS, OSHAregulated businesses that use materials containing 0.1% or more crystalline silica must follow Federal guidelines concerning hazard communication and worker training. Although the HCS does not require that samples be analyzed for crystalline silica, mineral suppliers or OSHAregulated

  2. Silica Refractory Bricks

    Institute of Scientific and Technical Information of China (English)

    Yu Lingyan; Peng Xigao

    2011-01-01

    @@ 1.Scope This standard specifies the classification,technical requirements,test methods,quality appraisal procedures,packing,marking,transportation,storage,and quality certificate of silica refractory bricks.This standard is applicable to silica refractory bricks with single weight≤40 kg.

  3. Rapid Preparation of Monolithic Columns for Capillary Electrochromatography Separation

    Institute of Scientific and Technical Information of China (English)

    Wen Jun GONG; Yi Jun ZHANG; Yu Ping ZHANG; Seong Ho CHOI

    2006-01-01

    Fritless packed silica gel columns were prepared using sol-gel technology. The part of a75 μm i.d. capillary was filled with a mixture of methacryloxypropyltrimethoxysilane, toluene and hydrochloric acid. Four different photoinitiators such as benzoin methyl ether, Irgacure 819,Irgacure 1700 and irgacure 1800 were added in the presence or absence of sodium dodecyl sulfate during the polymerization process. The above eight solutions were irradiated at 365 nm about5-10 min to prepare the porous monolithic sol-gel columns by a one-step process.

  4. Tapered capillary optics

    Science.gov (United States)

    Hirsch, Gregory

    1998-01-01

    A metal or glass wire is etched with great precision into a very narrowly tapering cone which has the shape of the desired final capillary-optics bore. By controlling the rate of removal of the wire from an etchant bath, a carefully controlled taper is produced. A sensor measures the diameter of the wire as it leaves the surface of the etchant. This signal is used for feedback control of the withdrawal speed. The etched wire undergoes a treatment to produce an extremely low surface-roughness. The etched and smoothed wire is coated with the material of choice for optimizing the reflectivity of the radiation being focused. This could be a vacuum evaporation, sputtering, CVD or aqueous chemical process. The coated wire is either electroplated, built up with electroless plating, or encapsulated in a polymer cylinder such as epoxy to increase the diameter of the wire for easier handling and greater robustness. During this process, the wire is vertically oriented and tensioned to assure that the wire is absolutely straight. The coated and electroformed wire is bonded to a flat, rigid substrate and is then periodically segmented by cutting or etching a series of narrow slits or grooves into the wire. The wire is vertically oriented and tensioned during the bonding process to assure that it is straight. The original wire material is then chemically etched away through the slits or otherwise withdrawn to leave the hollow internal bore of the final tapered-capillary optical element.

  5. Fusing Facial Features for Face Recognition

    Directory of Open Access Journals (Sweden)

    Jamal Ahmad Dargham

    2012-06-01

    Full Text Available Face recognition is an important biometric method because of its potential applications in many fields, such as access control, surveillance, and human-computer interaction. In this paper, a face recognition system that fuses the outputs of three face recognition systems based on Gabor jets is presented. The first system uses the magnitude, the second uses the phase, and the third uses the phase-weighted magnitude of the jets. The jets are generated from facial landmarks selected using three selection methods. It was found out that fusing the facial features gives better recognition rate than either facial feature used individually regardless of the landmark selection method.

  6. Plasmonic excitations on metallic nanowires embedded in silica photonic crystal fibers

    Energy Technology Data Exchange (ETDEWEB)

    Prill Sempere, Luis

    2010-06-17

    This thesis describes the theoretical and experimental investigation of metal-filled photonic crystal fibers (PCFs) and their fabrication. The thesis explains how to overcome the obstacles when infiltrating molten metals into sub-micron holes in fused silica (SiO{sub 2}) PCF. The optical properties of such filled fibers are theoretically and experimentally investigated, focusing on the coupling between the core mode of the fibers and the surface plasmon polaritons (SPPs) on the metal wires. The thesis introduces the ideas, physical challenges and results of two new filling techniques: the pressure cell technique and the splicing technique. These techniques make it possible for the first time to fill different fiber structures with sub-micron sized holes, such as PCFs and single-hole capillaries, with different metals like gold (Au) and silver (Ag). Samples with hole diameters between 120 nm and 20 {mu}m and aspect ratios as high as 75000 have been realized. Theoretical simulations and models have been developed in order to understand the optical behavior of these novel structures. The light guided in the core of the filled PCF structure will couple to SPP modes on the wires. Several measurements have been performed to determine the resonance wavelengths and losses of such filled PCF structures. Also, different phenomena such as the shift of the resonance position with the wire diameter or pitch and the polarization dependence of SPP in polarization maintaining (PM)-PCF have been investigated. The fabrication of free standing metal arrays was another focus of this work. The critical question was how to remove the surrounding SiO{sub 2} from the metal wires. Two different approaches have been tried: etching of the SiO{sub 2} and cleaving the PCF. (orig.)

  7. Capillaries modified by noncovalent anionic polymer adsorption for capillary zone electrophoresis, micellar electrokinetic capillary chromatography and capillary electrophoresis mass spectrometry

    DEFF Research Database (Denmark)

    Bendahl, L; Hansen, S H; Gammelgaard, Bente

    2001-01-01

    A simple coating procedure for generation of a high and pH-independent electroosmotic flow in capillary zone electrophoresis (CZE) and micellar electrokinetic capillary chromatography (MEKC) is described. The bilayer coating was formed by noncovalent adsorption of the ionic polymers Polybrene...

  8. The Synthesis and Characterization of β-cyclodextrin Derivated Pancreatin Used as Chiral Selector in Capillary Electrochromatography

    Institute of Scientific and Technical Information of China (English)

    2005-01-01

    The preparation of capillary electrochromatography column for chiral separation with β-cyclodextrin derivatized Pancreatin was investigated, which had three steps, synthesis ofβ-cyclodextrin derivated pancreatin, the modification of the capillary internal surface and the covalent binding of β-cyclodextrin derivated pancreatin on the capillary internal wall. β-cyclodextrin derivated pancreatin was synthesized using β-cyclodextrin and protein in the presence of ethylene glycol diglycidyl ether (EGDE) in boric acid buffer at pH = 8.7. Amino group was coated on the internal surface of the silica capillary by sol-gel technology using triethoxylmethylsiloxane and (3- aminopropyl ) trimethoxysiloxane . Covalent binding of β- cyclodextrin derivated pancreatin was performed by glutaraldehyde. Chlorpheniramine, phenylalanine and troopine were separated baseline by β-cyclodextrin derivated pancreatin in capillary electrochromatography.

  9. Graphene oxide-SiO2 hybrid nanostructure as coating material for capillary electrochromatography.

    Science.gov (United States)

    Qu, Qishu; Xuan, Han; Zhang, Kehua; Ding, Yi; Xu, Qin

    2016-05-01

    Graphene oxide (GO) has been considered as a promising stationary phase for chromatographic separation. However, the very strong adsorption of the analytes on the GO surface lead to the severe peak tailing, which in turn resulting in decreased separation performance. In this work, GO and silica nanoparticles hybrid nanostructures (GO/SiO2 NPs@column) were coated onto the capillary inner wall by passing the mixture of GO and silica sol through the capillary column. The successful of coating of GO/SiO2 NPs onto the capillary wall was confirmed by SEM and electroosmotic flow mobilities test. By partially covering the GO surface with silica nanoparticles, the peak tailing was decreased greatly while the unique high shape selectivity arises from the surface of remained GO was kept. Consequently, compared with the column modified with GO (GO@column), the column modified with GO and silica nanoparticles through layer-by-layer method (GO-SiO2 NPs@column), or the column modified with silica nanoparticles (SiO2 NPs@column), GO/SiO2 NPs@column possessed highest resolutions. The GO/SiO2 NPs@column was applied to separate egg white and both acidic and basic proteins as well as three glycoisoforms of ovalbumin were separated in a single run within 36 min. The intra-day, inter-day, and column-to-column reproducibilities were evaluated by calculating the RSDs of the retention of naphthalene and biphenyl in open-tubular capillary electrochromatography. The RSD values were found to be less than 7.1%.

  10. Biomedical applications of capillary electrophoresis

    Science.gov (United States)

    Kartsova, L. A.; Bessonova, E. A.

    2015-08-01

    The review deals with modern analytical approaches used in capillary electrophoresis for solving medical and biological problems: search for biomarkers of various diseases and rapid diagnosis based on characteristic profiles of biologically active compounds by capillary electrophoresis with mass spectrometric detection; monitoring of the residual drugs in biological fluids for evaluating the efficiency of drug therapy; testing of the enantiomeric purity of pharmaceutical products; the use of novel materials as components of stationary and pseudo-stationary phases in capillary electrophoresis and capillary electrochromatography to increase the selectivity of separation of components of complex matrices; and identification of various on-line preconcentration techniques to reduce the detection limits of biologically active analytes. A topical trend in capillary electrophoresis required in clinical practice, viz., the design of microfluidic systems, is discussed. The bibliography includes 173 references.

  11. Control of silicification by genetically engineered fusion proteins: Silk–silica binding peptides

    Science.gov (United States)

    Zhou, Shun; Huang, Wenwen; Belton, David J.; Simmons, Leo O.; Perry, Carole C.; Wang, Xiaoqin; Kaplan, David L.

    2014-01-01

    In the present study, an artificial spider silk gene, 6mer, derived from the consensus sequence of Nephila clavipes dragline silk gene, was fused with different silica-binding peptides (SiBPs), A1, A3 and R5, to study the impact of the fusion protein sequence chemistry on silica formation and the ability to generate a silk–silica composite in two different bioinspired silicification systems: solution–solution and solution– solid. Condensed silica nanoscale particles (600–800 nm) were formed in the presence of the recombinant silk and chimeras, which were smaller than those formed by 15mer-SiBP chimeras [1], revealing that the molecular weight of the silk domain correlated to the sizes of the condensed silica particles in the solution system. In addition, the chimeras (6mer-A1/A3/R5) produced smaller condensed silica particles than the control (6mer), revealing that the silica particle size formed in the solution system is controlled by the size of protein assemblies in solution. In the solution–solid interface system, silicification reactions were performed on the surface of films fabricated from the recombinant silk proteins and chimeras and then treated to induce β-sheet formation. A higher density of condensed silica formed on the films containing the lowest β-sheet content while the films with the highest β-sheet content precipitated the lowest density of silica, revealing an inverse correlation between the β-sheet secondary structure and the silica content formed on the films. Intriguingly, the 6mer-A3 showed the highest rate of silica condensation but the lowest density of silica deposition on the films, compared with 6mer-A1 and -R5, revealing antagonistic crosstalk between the silk and the SiBP domains in terms of protein assembly. These findings offer a path forward in the tailoring of biopolymer–silica composites for biomaterial related needs. PMID:25462851

  12. Physiological factors influencing capillary growth.

    Science.gov (United States)

    Egginton, S

    2011-07-01

    (1) Angiogenesis (growth of new capillaries from an existing capillary bed) may result from a mismatch in microvascular supply and metabolic demand (metabolic error signal). Krogh examined the distribution and number of capillaries to explore the correlation between O(2) delivery and O(2) consumption. Subsequently, the heterogeneity in angiogenic response within a muscle has been shown to reflect either differences in fibre type composition or mechanical load. However, local control leads to targetted angiogenesis in the vicinity of glycolytic fibre types following muscle stimulation, or oxidative fibres following endurance training, while heterogeneity of capillary spacing is maintained during ontogenetic growth. (2) Despite limited microscopy resolution and lack of specific markers, Krogh's interest in the structure of the capillary wall paved the way for understanding the mechanisms of capillary growth. Angiogenesis may be influenced by the response of perivascular or stromal cells (fibroblasts, macrophages and pericytes) to altered activity, likely acting as a source for chemical signals modulating capillary growth such as vascular endothelial growth factor. In addition, haemodynamic factors such as shear stress and muscle stretch play a significant role in adaptive remodelling of the microcirculation. (3) Most indices of capillarity are highly dependent on fibre size, resulting in possible bias because of scaling. To examine the consequences of capillary distribution, it is therefore helpful to quantify the area of tissue supplied by individual capillaries. This allows the spatial limitations inherent in most models of tissue oxygenation to be overcome generating an alternative approach to Krogh's tissue cylinder, the capillary domain, to improve descriptions of intracellular oxygen diffusion. © 2010 The Author. Acta Physiologica © 2010 Scandinavian Physiological Society.

  13. Fungal Systematics and Evolution: FUSE 1

    NARCIS (Netherlands)

    Crous, Pedro W; Schumacher, René K; Wingfield, Michael J; Lombard, Lorenzo; Giraldo, Alejandra; Christensen, Martha; Gardiennet, Alain; Nakashima, Chiharu; Pereira, Olinto L; Smith, Alexander J; Groenewald, Johannes Z

    2015-01-01

    Fungal Systematics and Evolution (FUSE) is introduced as a new series to expedite the publication of issues relating to the epitypification of formerly described species, report new sexual-asexual connections, the merging of sexual and asexual gen¬era following the end of dual nomenclature, and to

  14. Fused aromatic thienopyrazines: structure, properties and function

    KAUST Repository

    Mondal, Rajib

    2010-01-01

    Recent development of a fused aromatic thieno[3.4-b]pyrazine system and their application in optoelectronic devices are reviewed. Introduction of a fused aromatic unit followed by side chain engineering, dramatically enhanced the charge carrier mobility in thin film transistor devices and mobilities up to 0.2 cm2/Vs were achieved. The optoelectronic properties of these fused aromatic thienopyrazine polymers (Eg = 1.3 to 1.6 eV, HOMO = -4.9 to -5.2 V) were tuned by introduction of various fused aromatic rings within thienopyrazine. By balancing the fundamental properties of these polymers, both high charge carrier mobilities and moderate PCEs in solar cells were achieved. Further, effects of copolymerizing units are discussed. Low band gap semiconducting polymer (Eg ∼ 1 eV) with high field effect mobility (0.044 cm2/Vs) was obtained using cyclopentadithiophene as copolymerizing unit. Finally, a molecular design approach to enhance the absorption coefficients is discussed, which resulted in improved power conversion efficiency in bulk heterojunction solar cells. © 2010 The Royal Society of Chemistry.

  15. Renovating a Fusee Ceramique Barrel Vault

    NARCIS (Netherlands)

    Kamerling, M.W.

    2015-01-01

    This paper describes a proposal to renovate a Fusee Ceramique Barrel Vault with steel diagonals In 1956 two workshops, varying in height and span, were built in Wormerveer, The Netherlands. Both workshops were roofed with a concrete barrel vault with a thickness of 110 mm. The cylindrical vaults w

  16. 30 CFR 56.6502 - Safety fuse.

    Science.gov (United States)

    2010-07-01

    ... 30 Mineral Resources 1 2010-07-01 2010-07-01 false Safety fuse. 56.6502 Section 56.6502 Mineral Resources MINE SAFETY AND HEALTH ADMINISTRATION, DEPARTMENT OF LABOR METAL AND NONMETAL MINE SAFETY AND... initiation systems, igniter cord and connectors, or other nonelectric initiation systems shall be used...

  17. Demonstrating Earth Connections and Fuses Working Together

    Science.gov (United States)

    Harrison, Mark

    2017-01-01

    Earth wires and fuses work together in UK mains circuits to keep users safe from electric shocks and are taught in many school contexts. The subject can be quite abstract and difficult for pupils to grasp, and a simple but visually clear and direct demonstration is described which would be easy for most physics departments to build and which can…

  18. A fast and sensitive method for the determination of nitrite in human plasma by capillary electrophoresis with fluorescence detection.

    Science.gov (United States)

    Wang, Xu; Adams, Erwin; Van Schepdael, Ann

    2012-08-15

    Analysis of nitrite, the indicator of nitric oxide (NO) generation in vivo, provides a useful tool to study NO synthesis in vivo. A fast and sensitive fluorometric CE method was developed for determination of nitrite in human plasma through its derivatization with 2,3-diaminonaphthalene (DAN). Nitrite in human plasma was easily reacted with DAN under acid conditions to yield the highly fluorescent 2,3-naphthotriazole (NAT). Fluorescence detection was optimized to achieve subnanomolar detection which allows a direct analysis of plasma samples unlike most CE-UV methods using sample stacking. Acetonitrile was used to remove the protein. Short-end injection and a high voltage (-30 kV) were used to shorten the analysis time. The good separation was achieved with 20 mM borate buffer at pH 9.23. The separation of NAT was obtained within 1.4 min. The deproteinized plasma sample was injected hydrodynamically for 5s at -50 mbar into a 60 cm × 75 μm internal diameter uncoated fused-silica capillary. Excitation wavelength was selected with a broad-band filter (240-400 nm), and the emitted light was measured at 418 nm by the use of a cutoff filter. A good linearity (R(2)=0.9975) was obtained in the range from 2 to 500 nM. The detection limit of nitrite was 0.6 nM in original plasma samples, which is 750 times lower than our previous CE-UV method. The developed fluorometric CE method offers the advantages of more simple system and lower cost compared with the current fluorometric HPLC methods without losing sensitivity. The detected mean nitrite concentration in human plasma by this method was consistent with the most frequently reported values.

  19. Microchip capillary electrophoresis for frontal analysis of free bilirubin and study of its interaction with human serum albumin.

    Science.gov (United States)

    Nie, Zhou; Fung, Ying Sing

    2008-05-01

    To meet the need for bedside monitoring of free bilirubin for neonates under critical conditions, a microfluidic chip was fabricated and tested for its coupling with CE/frontal analysis (FA) to determine free bilirubin and study of its binding interaction with HSA, which regulated its concentration in plasma. The poly(methyl methacrylate) (PMMA) multichannel chip was fabricated by CO2 laser ablation and bonded with a fused-silica separation capillary for CE/FA separation with UV detection. The chip was designed to allow a complete assay of four electrophoretic runs using preconditioned channels to speed up the determination of free bilirubin and to deliver quick results for bedside monitoring. Under optimized conditions, the linear working range for free bilirubin was from 10 to 200 micromol with RSDs from 2.1 to 5.0% for n=3, and the LOD at 9 micromol for S/N=3. From a binding study between bilirubin and HSA under FA condition, the second binding constant for bilirubin-HSA was determined as 1.07x10(5) L/mol and the number of binding sites per HSA as 3.46. The results enabled the calculation of free bilirubin for jaundiced infants based on the clinically significant level of total bilirubin, producing a range of 118.3-119.4 micromol/L. The developed method is shown to meet the clinical requirement with additional margin of protection to detect the early rising level of free bilirubin prior to jaundice condition. The low-cost microchip CE/FA device is shown to produce quick results with high potential to deliver a suitable bed-side monitoring method for bilirubin management in neonates.

  20. Multidimensional capillary electrophoresis.

    Science.gov (United States)

    Grochocki, Wojciech; Markuszewski, Michał J; Quirino, Joselito P

    2015-01-01

    Multidimensional separation where two or more orthogonal displacement mechanisms are combined is a promising approach to increase peak capacity in CE. The combinations allow dramatic improvement of analytical performance since the total peak capacity is given by a product of the peak capacities of all methods. The initial reports were concentrated on the construction of effective connections between capillaries for 2D analysis. Today, 2D and 3D CE systems are now able to separate real complex biological or environmental mixtures with good repeatability, improved resolution with minimal loss of sample. This review will present the developments in the field of multidimensional CE during the last 15 years. The endeavors in this specific field were on the development of interfaces, interface-free techniques including integrated separations, microdevices, and on-line sample concentration techniques to improve detection sensitivity.

  1. Capillaries for use in a multiplexed capillary electrophoresis system

    Science.gov (United States)

    Yeung, E.S.; Chang, H.T.; Fung, E.N.

    1997-12-09

    The invention provides a side-entry optical excitation geometry for use in a multiplexed capillary electrophoresis system. A charge-injection device is optically coupled to capillaries in the array such that the interior of a capillary is imaged onto only one pixel. In Sanger-type 4-label DNA sequencing reactions, nucleotide identification (``base calling``) is improved by using two long-pass filters to split fluorescence emission into two emission channels. A binary poly(ethyleneoxide) matrix is used in the electrophoretic separations. 19 figs.

  2. Feasibility of the preparation of silica monoliths for gas chromatography: fast separation of light hydrocarbons.

    Science.gov (United States)

    Azzouz, Imadeddine; Essoussi, Anouar; Fleury, Joachim; Haudebourg, Raphael; Thiebaut, Didier; Vial, Jerome

    2015-02-27

    The preparation conditions of silica monoliths for gas chromatography were investigated. Silica-based monolithic capillary columns based on sol-gel process were tested in the course of high-speed gas chromatographic separations of light hydrocarbons mixture (C1-C4). The impact of modifying the amount of porogen and/or catalyst on the monolith properties were studied. At the best precursor/catalyst/porogen ratio evaluated, a column efficiency of about 6500 theoretical plates per meter was reached with a very good resolution (4.3) for very light compounds (C1-C2). The test mixture was baseline separated on a 70cm column. To our knowledge for the first time a silica-based monolithic capillary column was able to separate light hydrocarbons from methane to n-butane at room temperature with a back pressure in the range of gas chromatography facilities (under 4.1bar).

  3. Capillary flow solder wettability test

    Energy Technology Data Exchange (ETDEWEB)

    Vianco, P.T.; Rejent, J.A.

    1996-01-01

    A test procedure was developed to assess the capillary flow wettability of solders inside of a confined geometry. The test geometry was comprised of two parallel plates with a controlled gap of constant thickness (0.008 cm, 0.018 cm, 0.025 cm, and 0.038 cm). Capillary flow was assessed by: (1) the meniscus or capillary rise of the solder within the gap, (2) the extent of void formation in the gap, and (3) the time-dependence of the risen solder film. Tests were performed with the lead-free solders.

  4. Improvement of the Kruk-Jaroniec-Sayari method for pore size analysis of ordered silicas with cylindrical mesopores.

    Science.gov (United States)

    Jaroniec, Mietek; Solovyov, Leonid A

    2006-08-01

    In this work, the X-ray diffraction structure modeling was employed for analysis of hexagonally ordered large-pore silicas, SBA-15, to determine their pore width independently of adsorption measurements. Nitrogen adsorption isotherms were used to evaluate the relative pressure of capillary condensation in cylindrical mesopores of these materials. This approach allowed us to extend the original Kruk-Jaroniec-Sayari (KJS) relation (Langmuir 1997, 13, 6267) between the pore width and capillary condensation pressure up to 10 nm instead of previously established range from 2 to 6.5 nm for a series of MCM-41 and to improve the KJS pore size analysis of large pore silicas.

  5. Enhancement of capillary electrochromatographic separation performance by conductive polymer in a layer-by-layer fabricated graphene stationary phase.

    Science.gov (United States)

    Zhang, Juan; Zhang, Wenpeng; Bao, Tao; Chen, Zilin

    2014-04-25

    In this work, we fabricated a novel graphene-based capillary column for open-tubular capillary electrochromatography (OT-CEC) by a layer-by-layer strategy. To immobilize graphene onto the inner surface of silica capillary, a bio-inspired method was first used to functionalize the capillary surface with a layer of polydopamine (PDA). Graphene oxide (GO) was then introduced and can covalently react with polydopamine, realizing immobilization of graphene as a result. To enhance the modification efficiency of polydopamine, a conductive polymer, polyaniline (PANI) was introduced to be a sub-layer; polydopamine was then introduced following with GO, to generate a multilayer GO-PDA-PANI@capillary. Interestingly, separation efficiency of the graphene-based capillary was enhanced significantly by using conductive PANI as a sub-layer. The morphology of different layers modified on the capillary column was characterized by scanning electron microscopy (SEM). The electroosmotic flow (EOF) characteristics of capillaries modified with different layers were also investigated by varying the pH value of mobile phase. GO-PDA-PANI@capillary showed good separation efficiency towards alkylbenzenes by OT-CEC mode, with theoretic plate numbers up to 133,918 for benzene. The separation was found to follow a reversed-phase chromatographic retention mechanism. Repeatability of the GO-PDA-PANI@capillary was studied, with relative standard deviations for intra-day and inter-day runs less than 2.89%, and column-to-column runs less than 6.17%. The separation performance of GO-PDA-PANI@capillary was also compared with that of the reported graphene modified capillary.

  6. Analysis of Capillary Rise in Asymmetric Branch-Like Capillary

    Science.gov (United States)

    Li, Caoxiong; Shen, Yinghao; Ge, Hongkui; Yang, Zhihui; Su, Shuai; Ren, Kai; Huang, Heyu

    2016-05-01

    Transport in porous media is common in nature, attracting many attentions for a long time. Tree-like network model is often used as a simplification for porous space, expressing the complexity of pore spaces instead of capillary bundle. To investigate spontaneous imbibition characteristics in this network, a dynamic asymmetric branch-like capillary model is used to represent basic network structure, using fractal method to represent tortuosity. This work investigates the influence of parameters on imbibition process in the branch-like capillary model. An analytical equation for the imbibition mass versus time is derived. Parameters from capillary structures to liquid properties are taken into account and analyzed based on the numerical solution of the equation. It is found that the imbibition process in asymmetric branch-like capillary model can be recognized by four sections and brunching tubes are positive for imbibition process. Concomitantly, meniscus arrest event is simulated and discussed. Moreover, the influence of parameters on imbibition process is discussed. These parameters can be classified as static and dynamic. Static parameters mainly change the capillary force, which are related to the ultimate imbibition mass or imbibition ability, while dynamic parameters mainly have influence on resistance of flowing fluid, which are related to the imbibition speed in the imbibition process.

  7. Textiles: Some technocal information and data VI: fusing

    CSIR Research Space (South Africa)

    Cawood, MP

    1980-09-01

    Full Text Available results. However, complaints of problem do occur particularly with the technology becoming more sophisticated. Fusing interlinings are coated with an adhesive which enables them to be fused under certain conditions of temperature, time and pressure onto...

  8. Selectivity in capillary electrokinetic separations

    NARCIS (Netherlands)

    de Zeeuw, R.A; de Jong, G.J.; Ensing, K

    1999-01-01

    This review gives a survey of selectivity modes in capillary electrophoresis separations in pharmaceutical analysis and bioanalysis. Despite the high efficiencies of these separation techniques, good selectivity is required to allow quantitation or identification of a Chemistry and Toxicology, parti

  9. DNA typing by capillary electrophoresis

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, N.

    1997-10-08

    Capillary electrophoresis is becoming more and more important in nucleic acid analysis including DNA sequencing, typing and disease gene measurements. This work summarized the background of DNA typing. The recent development of capillary electrophoresis was also discussed. The second part of the thesis showed the principle of DNA typing based on using the allelic ladder as the absolute standard ladder in capillary electrophoresis system. Future work will be focused on demonstrating DNA typing on multiplex loci and examples of disease diagnosis in the on-line format of PCR-CE. Also capillary array electrophoresis system should allow high throughput, fast speed DNA typing. Only the introduction and conclusions for this report are available here. A reprint was removed for separate processing.

  10. Multimodal Plasmonics in Fused Colloidal Networks

    CERN Document Server

    Teulle, Alexandre; Girard, C; Gurunatha, Kargal L; Li, Mei; Mann, Stephen; Dujardin, Erik

    2014-01-01

    Harnessing the optical properties of noble metals down to the nanometer-scale is a key step towards fast and low-dissipative information processing. At the 10-nm length scale, metal crystallinity and patterning as well as probing of surface plasmon (SP) properties must be controlled with a challenging high level of precision. Here, we demonstrate that ultimate lateral confinement and delocalization of SP modes are simultaneously achieved in extended self-assembled networks comprising linear chains of partially fused gold nanoparticles. The spectral and spatial distributions of the SP modes associated with the colloidal superstructures are evidenced by performing monochromated electron energy loss spectroscopy with a nanometer-sized electron probe. We prepare the metallic bead strings by electron beam-induced interparticle fusion of nanoparticle networks. The fused superstructures retain the native morphology and crystallinity but develop very low energy SP modes that are capable of supporting long range and s...

  11. Demonstrating Earth connections and fuses working together

    Science.gov (United States)

    Harrison, Mark

    2017-03-01

    Earth wires and fuses work together in UK mains circuits to keep users safe from electric shocks and are taught in many school contexts. The subject can be quite abstract and difficult for pupils to grasp, and a simple but visually clear and direct demonstration is described which would be easy for most physics departments to build and which can make the concepts much more immediately understandable.

  12. Evidence of a green luminescence band related to surface flaws in high purity silica glass

    Energy Technology Data Exchange (ETDEWEB)

    Fournier, J.; Neauport, J.; Grua, P. [CEA, CESTA, F-33114 Le Barp (France); Fournier, J.; Fargin, E.; Jubera, V. [Univ Bordeaux, CNRS, ICMCB, F-33608 Pessac (France); Talaga, D. [Univ Bordeaux, CNRS, ISM, F-33405 Talence (France); Jouannigot, S. [Univ Bordeaux 1, LCTS, SAFRAN, CNRS, CEA, UMR 5801, Pessac (France)

    2010-07-01

    Using luminescence con-focal microscopy under 325 nm laser excitation, we explore the populations of defects existing in or at the vicinity of macroscopic surface flaws in fused silica. We report our luminescence results on two types of surface flaws: laser damage and indentation on fused silica polished surfaces. Luminescence cartographies are made to show the spatial distribution of each kind of defect. Three bands, centered at 1.89 eV, 2.75 eV and 2.25 eV are evidenced on laser damage and indentations. The band centered at 2.25 eV was not previously reported in photo luminescence experiments on indentations and pristine silica, for excitation wavelengths of 325 nm or larger. The luminescent objects, expected to be trapped in sub-surface micro-cracks, are possibly involved in the first step of the laser damage mechanism when fused silica is enlightened at 351 nm laser in nanosecond regime. (authors)

  13. A novel capillary microextraction on ordered mesoporous titania coating combined with electrothermal vaporization inductively coupled plasma mass spectrometry for the determination of V, Cr and Cu in environmental and biological samples.

    Science.gov (United States)

    Wu, Yiwei; Hu, Bin; Hu, Wenling; Jiang, Zucheng; Li, Boyangzi

    2007-04-01

    In this work, an ordered mesoporous titania film was introduced to coat a capillary by means of sol-gel technique. Sol-gel titania coating was developed for the preconcentration/separation of trace V, Cr and Cu by capillary microextraction (CME), and the adsorbed analytes were eluted for electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICP-MS) detection. By immobilizing sol-gel titania on the inner surface of a fused-silica microextraction capillary, the sol-gel titania coating was prepared easily. Its adsorption properties, stability and the factors affecting the adsorption behaviors of V, Cr and Cu were investigated in detail. At pH range of 7 to 9, the titania-coated capillary (50 cm x 0.25 mm) is selective towards V, Cr and Cu, and the target analytes could be desorbed quantitatively with 50 microl of 1.0 mol l(-1) HNO3 at the rate of 0.05 ml min(-1). With a consumption of 2 ml sample solution, an enrichment factor of 33.3, and a detection limit (3 s) of 1.1 pg ml(-1) (10.5 fg) for V; 3.3 pg ml(-1) (33.0 fg) for Cr and 6.3 pg ml(-1) (63.1 fg) for Cu respectively were obtained. The precisions Relative Standard Deviations (RSDs) for nine replicate measurements of 1 ng ml(-1) V, Cr and Cu were 3.4, 5.1 and 6.4%, respectively. The proposed method has been applied to the determination of V, Cr and Cu in human urine and lake water, and the recoveries for these elements were 89.2 approximately 105%. The developed method was also applied to the determination of the target elements in NIES No. 10-a (rice flour-unpolished) and NIES No. 9 (sargasso) certified reference materials, and the results found are in good agreement with the certified values. Copyright 2007 John Wiley & Sons, Ltd.

  14. The fabrication of monolithic capillary column based on poly (bisphenol A epoxy vinyl ester resin-co-ethylene glycol dimethacrylate) and its applicati