Preparation and characterization of fluorophenylboronic acid-functionalized affinity monolithic columns for the selective enrichment of cis-diol-containing biomolecules.

PubMed

Li, Qianjin; Liu, Zhen

2015-01-01

Boronate affinity monolithic columns have been developed into an important means for the selective recognition and capture of cis-diol-containing biomolecules, such as glycoproteins, nucleosides and saccharides. The ligands of boronic acids are playing an important role in boronate affinity monolithic columns. Although several boronate affinity monoliths with high affinity toward cis-diol-containing biomolecules have been reported, only few publications are focused on their detailed procedures for preparation and characterization. This chapter describes in detail the preparation and characterization of a boronate affinity monolithic column applying 2,4-difluoro-3-formyl-phenylboronic acid (DFFPBA) as a ligand. The DFFPBA-functionalized monolithic column not only exhibited an ultrahigh boronate affinity toward cis-diol-containing biomolecules, but also showed great potential for the selective enrichment of cis-diol-containing biomolecules in real samples.

Development and characterization of methacrylate-based hydrazide monoliths for oriented immobilization of antibodies.

PubMed

Brne, P; Lim, Y-P; Podgornik, A; Barut, M; Pihlar, B; Strancar, A

2009-03-27

Convective interaction media (CIM; BIA Separations) monoliths are attractive stationary phases for use in affinity chromatography because they enable fast affinity binding, which is a consequence of convectively enhanced mass transport. This work focuses on the development of novel CIM hydrazide (HZ) monoliths for the oriented immobilization of antibodies. Adipic acid dihydrazide (AADH) was covalently bound to CIM epoxy monoliths to gain hydrazide groups on the monolith surface. Two different antibodies were afterwards immobilized to hydrazide functionalized monolithic columns and prepared columns were tested for their selectivity. One column was further tested for the dynamic binding capacity.

Recognition of oxytocin by capillary electrochromatography with monolithic tetrapeptide-imprinted polymer used as the stationary phase.

PubMed

Zheng, Chao; Liu, Zhaosheng; Gao, Ruyu; Zhang, Lihua; Zhang, Yukui

2007-07-01

Using YPLG (Tyr-Pro-Leu-Gly), a tetrapeptide, as the template, an imprinted monolithic column was prepared and applied to the selective recognition of oxytocin based on the epitope approach and capillary electrochromatography (CEC). By optimizing the polymerization solution in terms of functional monomer, cross-linking reagent, porogen, and imprinted template via CEC evaluations of synthesized columns, an imprinted monolith with good recognition capacity (the imprinting factors for YPLG and oxytocin were 4.499 and 4.013, respectively) and high column efficiency (theoretical plates for YPLG and oxytocin were 22,995 plates/m and 16,952 plates/m, respectively) was achieved. In addition, the effects of various experimental parameters on the recognition of oxytocin, including the organic modifier content, the buffer concentration, and the pH value, were studied systematically. Furthermore, a mixture of oxytocin and other proteins was analyzed using this monolithic CEC column, and oxytocin was eluted much more slowly than other large biomolecules, which demonstrated the high selective recognition ability of such an imprinted monolith for oxytocin with PLG (Pro-Leu-Gly) as the epitope. Figure Separation of a mixture of oxytocin, BSA, bovine hemoglobin, ovalbumin, and lysozyme on the open column, the blank monolithic column, and the monolithic YPLG-imprinted column.

Monolith-based immobilized metal affinity chromatography increases production efficiency for plasmid DNA purification.

PubMed

Shin, Min Jae; Tan, Lihan; Jeong, Min Ho; Kim, Ji-Heung; Choe, Woo-Seok

2011-08-05

Immobilized metal affinity monolith column as a new class of chromatographic support is shown to be superior to conventional particle-based column as plasmid DNA (pDNA) purification platform. By harnessing the affinity of endotoxin to copper ions in the solution, a majority of endotoxin (90%) was removed from the alkaline cell lysate using CuCl(2)-induced precipitation. RNA and remaining endotoxin were subsequently removed to below detection limit with minimal loss of pDNA using either monolith or particle-based column. Monolith column has the additional advantage of feed concentration and flowrate-independent dynamic binding capacity for RNA molecules, enabling purification process to be conducted at high feed RNA concentration and flowrate. The use of monolith column gives three fold increased productivity of pDNA as compared to particle-based column, providing a more rapid and economical platform for pDNA purification. Copyright © 2011 Elsevier B.V. All rights reserved.

Preparation of a poly(3'-azido-3'-deoxythymidine-co-propargyl methacrylate-co-pentaerythritol triacrylate) monolithic column by in situ polymerization and a click reaction for capillary liquid chromatography of small molecules and proteins.

PubMed

Lin, Zian; Yu, Ruifang; Hu, Wenli; Zheng, Jiangnan; Tong, Ping; Zhao, Hongzhi; Cai, Zongwei

2015-07-07

Combining free radical polymerization with click chemistry via a copper-mediated azide/alkyne cycloaddition (CuAAC) reaction in a "one-pot" process, a facile approach was developed for the preparation of a poly(3'-azido-3'-deoxythymidine-co-propargyl methacrylate-co-pentaerythritol triacrylate) (AZT-co-PMA-co-PETA) monolithic column. The resulting poly(AZT-co-PMA-co-PETA) monolith showed a relatively homogeneous monolithic structure, good permeability and mechanical stability. Different ratios of monomers and porogens were used for optimizing the properties of a monolithic column. A series of alkylbenzenes, amides, anilines, and benzoic acids were used to evaluate the chromatographic properties of the polymer monolith in terms of hydrophobic, hydrophilic and cation-exchange interactions, and the results showed that the poly(AZT-co-PMA-co-PETA) monolith exhibited more flexible adjustment in chromatographic selectivity than that of the parent poly(PMA-co-PETA) and AZT-modified poly(PMA-co-PETA) monoliths. Column efficiencies for toluene, DMF, and formamide with 35,000-48,000 theoretical plates per m could be obtained at a linear velocity of 0.17 mm s(-1). The run-to-run, column-to-column, and batch-to-batch repeatabilities of the retention factors were less than 4.2%. In addition, the proposed monolith was also applied to efficient separation of sulfonamides, nucleobases and nucleosides, anesthetics and proteins for demonstrating its potential.

Preparation of epoxy-based macroporous monolithic columns for the fast and efficient immunofiltration of Staphylococcus aureus.

PubMed

Ott, Sonja; Niessner, Reinhard; Seidel, Michael

2011-08-01

Macroporous epoxy-based monolithic columns were used for immunofiltration of bacteria. The prepared monolithic polymer support is hydrophilic and has large pore sizes of 21 μm without mesopores. A surface chemistry usually applied for immobilization of antibodies on glass slides is successfully transferred to monolithic columns. Step-by-step, the surface of the epoxy-based monolith is hydrolyzed, silanized, coated with poly(ethylene glycol diamine) and activated with the homobifunctional crosslinker di(N-succinimidyl)carbonate for immobilization of antibodies on the monolithic columns. The functionalization steps are characterized to ensure the coating of each monolayer. The prepared antibody-immobilized monolithic column is optimized for immunofiltration to enrich Staphylococcus aureus as an important food contaminant. Different kinds of geometries of monolithic columns, flow rates and elution buffers are tested with the goal to get high recoveries in the shortest enrichment time as possible. An effective capture of S. aureus was achieved at a flow rate of 7.0 mL/min with low backpressures of 20.1±5.4 mbar enabling a volumetric enrichment of 1000 within 145 min. The bacteria were quantified by flow cytometry using a double-labeling approach. After immunofiltration the sensitivity was significantly increased and a detection limit of the total system of 42 S. aureus/mL was reached. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Synthesis of a specific monolithic column with artificial recognition sites for L-glutamic acid via cryo-crosslinking of imprinted nanoparticles.

PubMed

Göktürk, Ilgım; Üzek, Recep; Uzun, Lokman; Denizli, Adil

2016-06-01

In this study, a new molecular imprinting (MIP)-based monolithic cryogel column was prepared using chemically crosslinked molecularly imprinted nanoparticles, to achieve a simplified chromatographic separation (SPE) for a model compound, L-glutamic acid (L-Glu). Cryogelation through crosslinking of imprinted nanoparticles forms stable monolithic cryogel columns. This technique reduces the leakage of nanoparticles and increases the surface area, while protecting the structural features of the cryogel for stable and efficient recognition of the template molecule. A non-imprinted monolithic cryogel column (NIP) was also prepared, using non-imprinted nanoparticles produced without the addition of L-Glu during polymerization. The molecularly imprinted monolithic cryogel column (MIP) indicates apparent recognition selectivity and a good adsorption capacity compared to the NIP. Also, we have achieved a significant increase in the adsorption capacity, using the advantage of high surface area of the nanoparticles.

Carprofen-imprinted monolith prepared by reversible addition-fragmentation chain transfer polymerization in room temperature ionic liquids.

PubMed

Ban, Lu; Han, Xu; Wang, Xian-Hua; Huang, Yan-Ping; Liu, Zhao-Sheng

2013-10-01

To obtain fast separation, ionic liquids were used as porogens first in combination with reversible addition-fragmentation chain transfer (RAFT) polymerization to prepare a new type of molecularly imprinted polymer (MIP) monolith. The imprinted monolithic column was synthesized using a mixture of carprofen (template), 4-vinylpyridine, ethylene glycol dimethacrylate, [BMIM]BF4, and chain transfer agent (CTA). Some polymerization factors, such as template-monomer molar ratio, the degree of crosslinking, the composition of the porogen, and the content of CTA, on the column efficiency and imprinting effect of the resulting MIP monolith were systematically investigated. Affinity screening of structurally similar compounds with the template can be achieved in 200 s on the MIP monolith due to high column efficiency (up to 12,070 plates/m) and good column permeability. Recognition mechanism of the imprinted monolith was also investigated.

Characterization of new types of stationary phases for fast liquid chromatographic applications.

PubMed

Fekete, Szabolcs; Fekete, Jeno; Ganzler, Katalin

2009-12-05

The performance of a narrow bore silica based monolith column (5 cm x 2 mm) was compared to 5 cm long narrow bore (internal diameter < or = 2.1 mm) columns, packed with shell particles (2.7 microm) and totally porous sub-2 microm particles (1.5 microm, 1.7 microm and 1.9 microm) in gradient and isocratic elution separations of steroids. The highest peak capacity could be achieved with the column packed with 1.5 microm totally porous particles. The columns packed with porous 1.7 microm and shell 2.7 microm particles showed very similar capacity. The monolith column provided the lowest capacity during gradient elution. The plate height (HETP) of the 2.7 microm Ascentis Express column was very similar to the HETP obtained with 1.5 microm and 1.7 microm totally porous particles. The Chromolith monolithic column displayed an efficiency that is comparable to that of columns packed with spherical particles having their diameter between 3 microm and 4 microm. A kinetic plot analysis is presented to compare the theoretical analysis speed of different separation media. At 200 bar, the monolith column provided the highest performance when the required plate number was higher than 5000 (N>5000), however the efficiency drifted off faster in the range of N<5000 than in the case of packed columns. If the possibility of maximum performance was utilized (1000 bar for sub-2 microm particles, 600 bar for shell particles and 200 bar for monolith column) the monolith column would provide the poorest efficiency, while the column, packed with 1.5 microm particles offered the shortest impedance time.

"One-pot" preparation of basic amino acid-silica hybrid monolithic column for capillary electrochromatography.

PubMed

Xu, Hongrui; Xu, Zhendong; Yang, Limin; Wang, Qiuquan

2011-08-01

A novel "one-pot" strategy was developed for the preparation of amino acid (AA)-silica hybrid monolithic column. The basic AA (L-Arginine, L-Lysine and L-Histidine) was covalently incorporated into the silica hybrid skeleton via the epoxy ring-opening reaction between the amine group and the glycidyl moiety in γ-glycidoxypropyltrimethoxysilane (GPTMS), which was confirmed by elemental analysis and FT-IR studies, while the basic AA was also found to catalyze the polycondensation of tetramethoxysilane and GPTMS. The average mesopore and macropore sizes of the prepared basic AA-silica hybrid monolithic columns were 3.86 nm and 1.71 μm for the L-Lysine-silica hybrid monolith, 5.38 nm and 4.24 μm for the L-Arginine-silica hybrid monolith, and 6.38 nm and 1.24 μm for the L-Histidine-silica hybrid monolith. The hybrid monolith afforded a zwitterionic stationary phase for CEC, the direction and magnitude of EOF can be controlled by the pH of the mobile phase used. Besides an electrophoretic mechanism, the monoliths behave in a typical hydrophilic interaction with the analytes when ACN percentage in the mobile phase is over 40%. Four polar compounds (toluene, DMF, formamide and thiourea) were tested on the three AA-silica hybrid monolithic columns, and the best separation efficiency was observed in the L-Lysine-silica hybrid monolithic column, its theoretical plate height was down to 5.7 μm for thiourea when 20 mM HCOOH-HCOONH4 containing 20% ACN (pH 4.1) was used as a running buffer. The corresponding theoretical plate number for toluene, DMF, formamide and thiourea were 123,385, 103,620, 121,845 and 105,345 plates/m, respectively. Effective separation of phenols and peptides on the L-Lysine-silica hybrid monolithic column was achieved using CEC. We believe that this strategy paves a way for the easy preparation of various functional silica hybrid monolithic columns, aiming at different separation purposes. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Comparison of monolithic and microparticulate columns for reversed-phase liquid chromatography of tryptic digests of industrial enzymes in cleaning products.

PubMed

Beneito-Cambra, M; Herrero-Martínez, J M; Ramis-Ramos, G; Lindner, W; Lämmerhofer, M

2011-10-14

Enzymes of several classes used in the formulations of cleaning products were characterized by trypsin digestion followed by HPLC with UV detection. A polymeric monolithic column (ProSwift) was used to optimize the separation of both the intact enzymes and their tryptic digests. This column was adequate for the quality control of raw industrial enzyme concentrates. Then, monolithic and microparticulate columns were compared for peptide analysis. Under optimized conditions, the analysis of tryptic digests of enzymes of different classes commonly used in the formulation of cleaning products was carried out. Number of peaks, peak capacity and global resolution were obtained in order to evaluate the chromatographic performance of each column. Particulate shell-core C18 columns (Kinetex, 2.6 μm) showed the best performance, followed by a silica monolithic column (Chromolith RP-18e) and the conventional C18 packings (Gemini, 5 μm or 3 μm). A polymeric monolithic column (ProSwift) gave the worst performances. The proposed method was satisfactorily applied to the characterization of the enzymes present in spiked detergent bases and commercial cleaners. Copyright © 2011 Elsevier B.V. All rights reserved.

Titanium-scaffolded organic-monolithic stationary phases for ultra-high-pressure liquid chromatography.

PubMed

Vonk, Rudy J; Vaast, Axel; Eeltink, Sebastiaan; Schoenmakers, Peter J

2014-09-12

Organic-polymer monoliths with overall dimensions larger than one millimetre are prone to rupture - either within the monolith itself or between the monoliths and the containing wall - due to the inevitable shrinkage accompanying the formation of a cross-linked polymeric network. This problem has been addressed by creating titanium-scaffolded poly(styrene-co-divinylbenzene) (S-co-DVB) monoliths. Titanium-scaffolded monoliths were successfully used in liquid chromatography at very high pressures (up to 80MPa) and using gradients spanning the full range of water-acetonitrile compositions (0 to 100%). The kinetic-performance of (50-mm long) titanium-scaffolded monoliths was compared to that of similar monolith created in 1-mm i.d. glass-lined tubing at pressures up to 50MPa. The peak capacities obtained with the titanium-scaffolded column was about 30% lower. An increased Eddy-diffusion, due to the pillar-structure, and a decreased permeability are thought to be the main reasons for this reduced kinetic-performance. No decrease in performance was observed when the titanium-scaffolded columns were operated at pressures of 80MPa for up to 12h. The column-to-column repeatability (n=5) was acceptable in terms of observed peak widths at half heights (RSD ca. 10%) The run-to-run repeatability (n=135) in terms of retention times and peak widths at half height were found to be good. Titanium-scaffolded columns coupled in series up to a combined length of (200mm) were used for the analyses of a complex Escherichia coli protein sample. Our experiments demonstrate that columns based on titanium-scaffolded organic-polymer monolith can be operated under strenuous conditions without loss in performance. The titanium-scaffolded approach makes it feasible to create organic-polymer monoliths in wide-bore columns with accurate temperature control. Copyright © 2014 Elsevier B.V. All rights reserved.

Monolithic column based on a poly(glycidyl methacrylate-co-4-vinylphenylboronic acid-co-ethylene dimethacrylate) copolymer for capillary liquid chromatography of small molecules and proteins.

PubMed

Lin, Zian; Huang, Hui; Sun, Xiaobo; Lin, Yao; Zhang, Lan; Chen, Guonan

2012-07-13

A new polymer monolith with three modes of reverse-phase, hydrophilic and cation-exchange interaction was synthesized in 100 μm i.d. fused-silica capillary by in situ polymerization procedure. The pre-polymerization mixture consisted of glycidyl methacrylate (GMA) and 4-vinylphenylboronic acid (VPBA) as bifunctional monomers, ethylene dimethacrylate (EDMA) as crosslinker, 1,4-butanediol (BDO) and diethylene glycol (DEG) as binary porogenic solvents, and azobisisobutyronitrile (AIBN) as initiator. The resulting poly(GMA-co-VPBA-co-EDMA) monolith showed a relatively homogeneous monolithic structure, good permeability and mechanical stability. Different ratios of monomers and porogens were used for optimizing the properties of monolithic column. The column performance was assessed by the separation of a series of neutral solutes, charge solutes, phenols and anilines. Compared with poly(GMA-co-EDMA) monolith, the proposed monolith exhibited more flexible adjustment of selectivity in terms of hydrophobic, hydrophilic, as well as cation-exchange interaction in the same chromatographic conditions. High column efficiencies for benzene derivatives with 70,000-102,000 theoretical plates/m could be obtained at a linear velocity of 0.265 mm/s. The run-to-run, column-to-column, and batch-to-batch repeatabilities of the retention times were less than 8.23%. Additionally, the purposed monolith was also applied to efficient separation of alkaloids and proteins for demonstrating its potential in biomolecule separation. Crown Copyright © 2012. Published by Elsevier B.V. All rights reserved.

Measurement of the eddy diffusion term in chromatographic columns. I. Application to the first generation of 4.6mm I.D. monolithic columns.

PubMed

Gritti, Fabrice; Guiochon, Georges

2011-08-05

The corrected heights equivalent to a theoretical plate (HETP) of three 4.6mm I.D. monolithic Onyx-C(18) columns (Onyx, Phenomenex, Torrance, CA) of different lengths (2.5, 5, and 10 cm) are reported for retained (toluene, naphthalene) and non-retained (uracil, caffeine) small molecules. The moments of the peak profiles were measured according to the accurate numerical integration method. Correction for the extra-column contributions was systematically applied. The peak parking method was used in order to measure the bulk diffusion coefficients of the sample molecules, their longitudinal diffusion terms, and the eddy diffusion term of the three monolithic columns. The experimental results demonstrate that the maximum efficiency was 60,000 plates/m for retained compounds. The column length has a large impact on the plate height of non-retained species. These observations were unambiguously explained by a large trans-column eddy diffusion term in the van Deemter HETP equation. This large trans-rod eddy diffusion term is due to the combination of a large trans-rod velocity bias (≃3%), a small radial dispersion coefficient in silica monolithic columns, and a poorly designed distribution and collection of the sample streamlets at the inlet and outlet of the monolithic rod. Improving the performance of large I.D. monolithic columns will require (1) a detailed knowledge of the actual flow distribution across and along these monolithic rod and (2) the design of appropriate inlet and outlet distributors designed to minimize the nefarious impact of the radial flow heterogeneity on band broadening. Copyright © 2011 Elsevier B.V. All rights reserved.

A hybrid monolithic column based on boronate-functionalized graphene oxide nanosheets for online specific enrichment of glycoproteins.

PubMed

Zhou, Chanyuan; Chen, Xiaoman; Du, Zhuo; Li, Gongke; Xiao, Xiaohua; Cai, Zongwei

2017-05-19

A hybrid monolithic column based on aminophenylboronic acid (APBA)-functionalized graphene oxide (GO) has been developed and used for selective enrichment of glycoproteins. The APBA/GO composites were homogeneously incorporated into a polymer monolithic column with the help of oligomer matrix and followed by in situ polymerization. The effect of dispersion of APBA/GO composites in the polymerization mixture on the performance of the monolithic column was explored in detail. The presence of graphene oxide not only enlarged the BET surface area from 6.3m 2 /g to 169.4m 2 /g, but also provided abundant boronic acid moieties for glycoprotein extraction, which improved the enrichment selectivity and efficiency for glycoproteins. The APBA/GO hybrid monolithic column was incorporated into a sequential injection system, which facilitated online extraction of proteins. Combining the superior properties of extraordinary surface area of GO and the affinity interaction of APBA to glycoproteins, the APBA/GO hybrid monolithic column showed higher enrichment factors for glycoproteins than other proteins without cis-diol-containing groups. Also, under comparable or even shorter processing time and without the addition of any organic solvent, it showed higher binding capacity toward glycoproteins compared with the conventional boronate affinity monolithic column. The practical applicability of this system was demonstrated by processing of egg white samples for extraction of ovalbumin and ovotransferrin, and satisfactory results were obtained by assay with SDS-PAGE. Copyright © 2017 Elsevier B.V. All rights reserved.

Periodic imidazolium-bridged hybrid monolith for high-efficiency capillary liquid chromatography with enhanced selectivity.

PubMed

Qiao, Xiaoqiang; Zhang, Niu; Han, Manman; Li, Xueyun; Qin, Xinying; Shen, Shigang

2017-03-01

A novel periodic imidazolium-bridged hybrid monolithic column was developed. With diene imidazolium ionic liquid 1-allyl-3-vinylimidazolium bromide as both cross-linker and organic functionalized reagent, a new periodic imidazolium-bridged hybrid monolithic column was facilely prepared in capillary with homogeneously distributed cationic imidazolium by a one-step free-radical polymerization with polyhedral oligomeric silsesquioxane methacryl substituted. The successful preparation of the new column was verified by Fourier transform infrared spectroscopy, scanning electron microscopy, elemental analysis, and surface area analysis. Most interestingly, the bonded amount of 1-allyl-3-vinylimidazolium bromide of the new column is three times higher than that of the conventional imidazolium-embedded hybrid monolithic column and the specific surface area of the column reached 478 m 2 /g. The new column exhibited high stability, excellent separation efficiency, and enhanced separation selectivity. The column efficiency reached 151 000 plates/m for alkylbenzenes. Furthermore, the new column was successfully used for separation of highly polar nucleosides and nucleic acid bases with pure water as mobile phase and even bovine serum albumin tryptic digest. All these results demonstrate the periodic imidazolium-bridged hybrid monolithic column is a good separation media and can be used for chromatographic separation of small molecules and complex biological samples with high efficiency. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Dopamine-imprinted monolithic column for capillary electrochromatography.

PubMed

Aşır, Süleyman; Sarı, Duygu; Derazshamshir, Ali; Yılmaz, Fatma; Şarkaya, Koray; Denizli, Adil

2017-11-01

A dopamine-imprinted monolithic column was prepared and used in capillary electrochromatography as stationary phase for the first time. Dopamine was selectively separated from aqueous solution containing the competitor molecule norepinephrine, which is similar in size and shape to the template molecule. Morphology of the dopamine-imprinted column was observed by scanning electron microscopy. The influence of the organic solvent content of mobile phase, applied pressure and pH of the mobile phase on the recognition of dopamine by the imprinted monolithic column has been evaluated, and the imprinting effect in the dopamine-imprinted monolithic polymer was verified. Developed dopamine-imprinted monolithic column resulted in excellent separation of dopamine from structurally related competitor molecule, norepinephrine. Separation was achieved in a short period of 10 min, with the electrophoretic mobility of 5.81 × 10 -5  m 2 V -1 s -1 at pH 5.0 and 500 mbar pressure. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Preparation of polyhedral oligomeric silsesquioxane based imprinted monolith.

PubMed

Li, Fang; Chen, Xiu-Xiu; Huang, Yan-Ping; Liu, Zhao-Sheng

2015-12-18

Polyhedral oligomeric silsesquioxane (POSS) was successfully applied, for the first time, to prepare imprinted monolithic column with high porosity and good permeability. The imprinted monolithic column was synthesized with a mixture of PSS-(1-Propylmethacrylate)-heptaisobutyl substituted (MA 0702), naproxon (template), 4-vinylpyridine, and ethylene glycol dimethacrylate, in ionic liquid 1-butyl-3-methylimidazolium tetrafluoroborate ([BMIM]BF4). The influence of synthesis parameters on the retention factor and imprinting effect, including the amount of MA 0702, the ratio of template to monomer, and the ratio of monomer to crosslinker, was investigated. The greatest imprinting factor on the imprinted monolithic column prepared with MA 0702 was 22, about 10 times higher than that prepared in absence of POSS. The comparisons between MIP monoliths synthesized with POSS and without POSS were made in terms of permeability, column efficiency, surface morphology and pore size distribution. In addition, thermodynamic and Van Deemter analysis were used to evaluate the POSS-based MIP monolith. Copyright © 2015 Elsevier B.V. All rights reserved.

Chromatographic assessment of two hybrid monoliths prepared via epoxy-amine ring-opening polymerization and methacrylate-based free radical polymerization using methacrylate epoxy cyclosiloxane as functional monomer.

PubMed

Wang, Hongwei; Ou, Junjie; Lin, Hui; Liu, Zhongshan; Huang, Guang; Dong, Jing; Zou, Hanfa

2014-11-07

Two kinds of hybrid monolithic columns were prepared by using methacrylate epoxy cyclosiloxane (epoxy-MA) as functional monomer, containing three epoxy moieties and one methacrylate group. One column was in situ fabricated by ring-opening polymerization of epoxy-MA and 1,10-diaminodecane (DAD) using a porogenic system consisting of isopropanol (IPA), H2O and ethanol at 65°C for 12h. The other was prepared by free radical polymerization of epoxy-MA and ethylene dimethacrylate (EDMA) using 1-propanol and 1,4-butanediol as the porogenic solvents at 60°C for 12h. Two hybrid monoliths were investigated on the morphology and chromatographic assessment. Although two kinds of monolithic columns were prepared with epoxy-MA, their morphologies looked rather different. It could be found that the epoxy-MA-DAD monolith possessed higher column efficiencies (25,000-34,000plates/m) for the separation of alkylbenzenes than the epoxy-MA-EDMA monolith (12,000-13,000plates/m) in reversed-phase nano-liquid chromatography (nano-LC). Depending on the remaining epoxy or methacrylate groups on the surface of two pristine monoliths, the epoxy-MA-EDMA monolith could be easily modified with 1-octadecylamine (ODA) via ring-opening reaction, while the epoxy-MA-DAD monolith could be modified with stearyl methacrylate (SMA) via free radical reaction. The chromatographic performance for the separation of alkylbenzenes on SMA-modified epoxy-MA-DAD monolith was remarkably improved (42,000-54,000 plates/m) when compared with that on pristine epoxy-MA-DAD monolith, while it was not obviously enhanced on ODA-modified epoxy-MA-EDMA monolith when compared with that on pristine epoxy-MA-EDMA monolith. The enhancement of the column efficiency of epoxy-MA-DAD monolith after modification might be ascribed to the decreased mass-transfer resistence. The two kinds of hybrid monoliths were also applied for separations of six phenols and seven basic compounds in nano-LC. Copyright © 2014 Elsevier B.V. All rights reserved.

Preparation of a poly(styrene-co-DPHA-co-EDMA) monolith and its application for the separation of small molecules and biomacromolecules by HPLC.

PubMed

Wang, Xixi; Li, Xueying; Jiang, Xiaoya; Dong, Peipei; Liu, Haiyan; Bai, Ligai; Yan, Hongyuan

2017-04-01

A high performance liquid chromatography (HPLC) monolithic column was prepared by redox polymerization of styrene, dipentaerythritol hexaacrylate (DPHA) and ethylene glycol dimethacrylate (EDMA) in a porogen system of n-propanol/PEG400. The monolith was characterized by scanning electron microscopy (SEM), mercury intrusion porosimetry (MIP) and the results indicated that the monolith had a stable and homogeneous structure. The porosity of the monolithic column was 75.86% and average pore diameter was 2.1µm. Several alkylbenzenes and anilines were used to evaluate the column performance in terms of hydrophobicity. Then the column was applied to separate small molecules including phytosterol and BSA tryptic digest. Finally, five standard proteins, egg white and plasma were separated respectively and high separation capacity of protein was obtained. Copyright © 2016 Elsevier B.V. All rights reserved.

Facile preparation of SiO2/TiO2 composite monolithic capillary column and its application in enrichment of phosphopeptides.

PubMed

Wang, Shao-Ting; Wang, Meng-Ya; Su, Xin; Yuan, Bi-Feng; Feng, Yu-Qi

2012-09-18

A novel SiO(2)/TiO(2) composite monolithic capillary column was prepared by sol-gel technology and successfully applied to enrich phosphopeptides as a metal oxide affinity chromatography (MOAC) material. For the monolith preparation, tetramethoxysilane (TMOS) and tetrabutoxytitanium (TBOT) were used as silica and titania source, respectively, and glycerol was introduced to attenuate the activity of titanium precursor, which provided a mild synthetic condition. The prepared monolith was characterized by energy dispersive X-ray spectroscopy (EDX) and X-ray diffraction (XRD). The results revealed an approximate 1/2 molar ratio of titanium to silica as well as an atom-scale homogeneity in the framework. The scanning electron microscopy (SEM) results demonstrated an excellent anchorage between the column and the inner capillary wall, and nitrogen adsorption-desorption experiments showed a bimodal porosity with a narrow mesopore distribution around 3.6 nm. The prepared monolith was then applied for selective enrichment of phosphopeptides from the digestion mixture of phosphoproteins and bovine serum albumin (BSA) as well as human blood serum, nonfat milk, and egg white using an in-tube solid phase microextraction (SPME) system. Our results showed that SiO(2)/TiO(2) composite monolithic capillary column could efficiently enrich the phosphopeptides from complex matrixes. To the best of our knowledge, this is the first attempt for preparing the silica-metal composite monolithic capillary column, which offers the promising application of the monolith on phosphoproteomics study.

Fast preparation of hybrid monolithic columns via photo-initiated thiol-yne polymerization for capillary liquid chromatography.

PubMed

Ma, Shujuan; Zhang, Haiyang; Li, Ya; Li, Yanan; Zhang, Na; Ou, Junjie; Ye, Mingliang; Wei, Yinmao

2018-02-23

Although several approaches have been developed to fabricate hybrid monoliths, it would still take a few hours to finish the formation of monoliths. Herein, photo-initiated thiol-yne polymerization was first adopted to in situ fabricate hybrid monoliths within the confines of UV-transparent fused-silica capillary. A silicon-containing diyne (1,3-diethynyltetramethyl-disiloxane, DYDS) was copolymerized with three multithiols, 1,6-hexanedithiol, trimethylolpropane tris(3-mercaptopropionate) and pentaerythriol tetrakis(3-mercaptopropionate), by using a binary porogenic system of diethylene glycol diethyl ether (DEGDE)/poly(ethylene glycol) (PEG200) within 10 min. Several characterizations of three hybrid monoliths (assigned as I, II and III, respectively) were performed. The results showed that these hybrid monoliths possessed bicontinuous porous structure, which was remarkably different from that via typical free-radical polymerization. The highest column efficiency of 76,000 plates per meter for butylbenzene was obtained on the column I in reversed-phase liquid chromatography (RPLC). It was observed that the efficiencies for strong-retained butylbenzene were almost close to those of weak-retained benzene, indicating a retention-independent efficient performance of small molecules on hybrid column I. The surface area of this hybrid monolith was very small in the dry state (less than 10.0 m 2 /g), and the chromatographic behavior of hybrid monolithic columns would be possibly explained by radical-mediated step-growth process of thiol-yne polymerization. Finally, the column I was applied for separation of BSA tryptic digest by cLC-MS/MS, indicating satisfactory separation ability for complicated samples. Copyright © 2018 Elsevier B.V. All rights reserved.

Preparation and evaluation of a novel hybrid monolithic column based on pentafluorobenzyl imidazolium bromide ionic liquid.

PubMed

Shan, Yuanhong; Qiao, Lizhen; Shi, Xianzhe; Xu, Guowang

2015-01-02

To develop a novel hybrid monolithic column based on pentafluorobenzyl imidazolium bromide ionic liquid, a new ionic liquid monomer was synthesized from 1-vinylimidazole and pentafluorobenzyl bromide. By employing a facile one-step copolymerization of polyhedral-oligomeric-silsesquioxane-type (POSS) cross-linking agent and the home-made ionic liquid monomer, the hybrid monolithic columns were in situ fabricated in fused-silica capillary. The morphology of monolithic column was characterized by scanning electron microscope (SEM) and the chemical composition was confirmed by Fourier-transform infrared spectroscopy (FT-IR) and elemental analysis. Excellent mechanical stability and slight swelling propensity were exhibited which was ascribed to the rigid hybrid monolithic skeleton. Reproducibility results of run-to-run, column-to-column, batch-to-batch and day-to-day were investigated and the RSDs were less than 0.46%, 1.84%, 3.96% and 3.17%, respectively. The mixed-mode retention mechanism with hydrophobic interaction, π-π stacking, ion-exchange, electrostatic interaction and dipole-dipole interaction was explored systematically using analytes with different structure types. Satisfied separation capability and column efficiency were achieved for the analysis of small molecular compounds such as alkylbenzenes, polycyclic aromatic hydrocarbons, nucleosides and halogenated compounds. Copyright © 2014 Elsevier B.V. All rights reserved.

Highly crosslinked polymeric monoliths for reversed-phase capillary liquid chromatography of small molecules.

PubMed

Liu, Kun; Tolley, H Dennis; Lee, Milton L

2012-03-02

Seven crosslinking monomers, i.e., 1,3-butanediol dimethacrylate (1,3-BDDMA), 1,4-butanediol dimethacrylate (1,4-BDDMA), neopentyl glycol dimethacrylate (NPGDMA), 1,5-pentanediol dimethacrylate (1,5-PDDMA), 1,6-hexanediol dimethacrylate (1,6-HDDMA), 1,10-decanediol dimethacrylate (1,10-DDDMA), and 1,12-dodecanediol dimethacrylate (1,12-DoDDMA), were used to synthesize highly cross-linked monolithic capillary columns for reversed-phase liquid chromatography (RPLC) of small molecules. Dodecanol and methanol were chosen as "good" and "poor" porogenic solvents, respectively, for these monoliths, and were investigated in detail to provide insight into the selection of porogen concentration using 1,12-DoDDMA. Isocratic elution of alkylbenzenes at a flow rate of 300 nL/min was conducted for all of the monoliths. Gradient elution of alkylbenzenes and alkylparabens provided high resolution separations. Optimized monoliths synthesized from all seven crosslinking monomers showed high permeability. Several of the monoliths demonstrated column efficiencies in excess of 50,000 plates/m. Monoliths with longer alkyl-bridging chains showed very little shrinking or swelling in solvents of different polarities. Column preparation was highly reproducible; the relative standard deviation (RSD) values (n=3) for run-to-run and column-to-column were less than 0.25% and 1.20%, respectively, based on retention times of alkylbenzenes. Copyright © 2012 Elsevier B.V. All rights reserved.

Recent advances in preparation and application of hybrid organic-silica monolithic capillary columns.

PubMed

Ou, Junjie; Lin, Hui; Zhang, Zhenbin; Huang, Guang; Dong, Jing; Zou, Hanfa

2013-01-01

Hybrid organic-silica monolithic columns, regarded as a second generation of silica-based monoliths, have received much interest due to their unique properties over the pure silica-based monoliths. This review mainly focuses on development in the fields of preparation of hybrid monolithic columns in a capillary and their application for CEC and capillary liquid chromatography separation, as well as for sample pretreatment of solid-phase microextraction and immobilized enzyme reactor since July 2010. The preparation approaches are comprehensively summarized with three routes: (i) general sol-gel process using trialkoxysilanes and tetraalkoxysilanes as coprecursors; (ii) "one-pot" process of alkoxysilanes and organic monomers concomitantly proceeding sol-gel chemistry and free radical polymerization; and (iii) other polymerization approaches of organic monomers containing silanes. The modification of hybrid monoliths containing reactive groups to acquire the desired surface functionality is also described. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Comparative study of recent wide-pore materials of different stationary phase morphology, applied for the reversed-phase analysis of recombinant monoclonal antibodies.

PubMed

Fekete, Szabolcs; Veuthey, Jean-Luc; Eeltink, Sebastiaan; Guillarme, Davy

2013-04-01

Various recent wide-pore reversed-phase stationary phases were studied for the analysis of intact monoclonal antibodies (mAbs) of 150 kDa and their fragments possessing sizes between 25 and 50 kDa. Different types of column technology were evaluated, namely, a prototype silica-based inorganic monolith containing mesopores of ~250 Å and macropores of ~ 1.1 μm, a column packed with 3.6 μm wide-pore core-shell particles possessing a wide pore size distribution with an average around 200 Å and a column packed with fully porous 1.7 μm particles having pore size of ~300 Å. The performance of these wide-pore materials was compared with that of a poly(styrene-divinyl benzene) organic monolithic column, with a macropore size of approximately 1 μm but without mesopores (stagnant pores). A systematic investigation was carried out using model IgG1 and IgG2 mAbs, namely rituximab, panitumumab, and bevacizumab. Firstly, the recoveries of intact and reduced mAbs were compared on the two monolithic phases, and it appeared that adsorption was less pronounced on the organic monolith, probably due to the difference in chemistry (C18 versus phenyl) and the absence of mesopores (stagnant zones). Secondly, the kinetic performance was investigated in gradient elution mode for all columns. For this purpose, peak capacities per meter as well as peak capacities per time unit and per pressure unit (PPT) were calculated at various flow rates, to compare performance of columns with different dimensions. In terms of peak capacity per meter, the core-shell 3.6 μm and fully porous 1.7 μm columns outperformed the two monolithic phases, at a temperature of 60 °C. However, when considering the PPT values, the core-shell 3.6 μm column remained the best phase while the prototype silica-based monoliths became very interesting, mostly due to a very high permeability compared with the organic monolith. Therefore, these core-shell and silica-based monolith provided the fastest achievable separation. Finally, at the maximal working temperature of each column, the core-shell 3.6 μm column was far better than the other one, because it is the only one stable up to 90 °C. Lastly, the loading capacity was also measured on these four different phases. It appeared that the organic monolith was the less interesting and rapidly overloaded, due to the absence of mesopores. On the other hand, the loading capacity of prototype silica-based monolith was indeed reasonable.

Tuning preparation conditions towards optimized separation performance of thermally polymerized organo-silica monolithic columns in capillary liquid chromatography.

PubMed

Gharbharan, Deepa; Britsch, Denae; Soto, Gabriela; Weed, Anna-Marie Karen; Svec, Frantisek; Zajickova, Zuzana

2015-08-21

Tuning of preparation conditions, such as variations in the amount of a porogen, concentration of an aqueous acid catalyst, and adjustment in polymerization temperature and time, towards optimized chromatographic performance of thermally polymerized monolithic capillaries prepared from 3-(methacryloyloxy)propyltrimethoxysilane has been carried out. Performance of capillary columns in reversed-phase liquid chromatography was assessed utilizing various sets of solutes. Results describing hydrophobicity, steric selectivity, and extent of hydrogen bonding enabled comparison of performance of hybrid monolithic columns prepared under thermal (TSG) and photopolymerized (PSG) conditions. Reduced amounts of porogen in the polymerization mixture, and prolonged reaction times were necessary for the preparation of monolithic columns with enhanced retention and column efficiency that reached to 111,000 plates/m for alkylbenzenes with shorter alkyl chains. Both increased concentration of catalyst and higher temperature resulted in faster polymerization but inevitably in insufficient time for pore formation. Thermally polymerized monoliths produced surfaces, which were slightly more hydrophobic (a methylene selectivity of 1.28±0.002 TSG vs 1.20±0.002 PSG), with reduced number of residual silanols (a caffeine/phenol selectivity of 0.13±0.001 TSG vs 0.17±0.003 PSG). However, steric selectivity of 1.70±0.01 was the same for both types of columns. The batch-to-batch repeatability was better using thermal initiation compared to monolithic columns prepared under photopolymerized conditions. RSD for retention factor of benzene was 3.7% for TSG capillaries (n=42) vs. 6.6% for PSG capillaries (n=18). A similar trend was observed for columns prepared within the same batch. Copyright © 2015 Elsevier B.V. All rights reserved.

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

PubMed

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.

Facile construction of macroporous hybrid monoliths via thiol-methacrylate Michael addition click reaction for capillary liquid chromatography.

PubMed

Lin, Hui; Ou, Junjie; Liu, Zhongshan; Wang, Hongwei; Dong, Jing; Zou, Hanfa

2015-01-30

A facile approach based on thiol-methacrylate Michael addition click reaction was developed for construction of porous hybrid monolithic materials. Three hybrid monoliths were prepared via thiol-methacrylate click polymerization by using methacrylate-polyhedral oligomeric silsesquioxane (POSS) (cage mixture, n=8, 10, 12, POSS-MA) and three multi-thiol crosslinkers, 1,6-hexanedithiol (HDT), trimethylolpropane tris(3-mercaptopropionate) (TPTM) and pentaerythritol tetrakis(3-mercaptopropionate) (PTM), respectively, in the presence of porogenic solvents (n-propanol and PEG 200) and a catalyst (dimethylphenylphosphine, DMPP). The obtained monoliths possessed high thermal and chemical stabilities. Besides, they all exhibited high column efficiencies and excellent separation abilities in capillary liquid chromatography (cLC). The highest column efficiency could reach ca. 195,000N/m for butylbenzene on the monolith prepared with POSS-MA and TPTM (monolith POSS-TPTM) in reversed-phase (RP) mode at 0.64mm/s. Good chromatographic performance were all achieved in the separations of polycyclic aromatic hydrocarbons (PAHs), phenols, anilines, EPA 610 as well as bovine serum albumin (BSA) digest. The high column efficiencies in the range of 51,400-117,000N/m (achieved on the monolith POSS-PTM in RP mode) convincingly demonstrated the high separation abilities of these thiol-methacrylate based hybrid monoliths. All the results demonstrated the feasibility of the phosphines catalyzed thiol-methacrylate Michael addition click reaction in fabrication of monolithic columns with high efficiency for cLC applications. Copyright © 2014 Elsevier B.V. All rights reserved.

Monolithic columns with organic sorbent based on poly-1-vinylimidazole for high performance liquid chromatography

NASA Astrophysics Data System (ADS)

Patrushev, Y. V.; Sidelnikov, V. N.; Yudina, Y. S.

2017-03-01

Monolithic chromatographic columns for HPLC with sorbent based on 1-vinylimidazole are prepared. It is shown that changing the 1-vinylimidazole content in the initial solution allows us to change the polarity of columns. An example of aromatic hydrocarbons separation is presented.

Ultrafast preparation of a polyhedral oligomeric silsesquioxane-based ionic liquid hybrid monolith via photoinitiated polymerization, and its application to capillary electrochromatography of aromatic compounds.

PubMed

Zhang, Bingyu; Lei, Xiaoyun; Deng, Lijun; Li, Minsheng; Yao, Sicong; Wu, Xiaoping

2018-06-06

An ionic liquid hybrid monolithic capillary column was prepared within 7 min via photoinitiated free-radical polymerization of an ionic liquid monomer (1-butyl-3-vinylimidazolium-bis[(trifluoromethyl)sulfonyl]imide); VBIMNTF 2 ) and a methacryl substituted polyhedral oligomeric silsesquioxane (POSS-MA) acting as a cross-linker. The effects of composition of prepolymerization solution and initiation time on the porous structure and electroosmotic flow (EOF) of monolithic column were investigated. The hybrid monolith was characterized by scanning electron microscopy and FTIR. Owing to the introduction of a rigid nanosized POSS silica core and ionic liquids with multiple interaction sites, the monolithic column has a well-defined 3D skeleton morphology, good mechanical stability, and a stable anodic electroosmotic flow. The hybrid monolithic stationary phase was applied to the capillary electrochromatographic separation of various alkylbenzenes, phenols, anilines and polycyclic aromatic hydrocarbons (PAHs). The column efficiency is highest (98,000 plates/m) in case of alkylbenzenes. Mixed-mode retention mechanisms including hydrophobic interactions, π-π stacking, electrostatic interaction and electrophoretic mobility can be observed. This indicates the potential of this material in terms of efficient separation of analytes of different structural type. Graphical Abstract Preparation of a mixed-mode ionic liquid hybrid monolithic column via photoinitiated polymerization of methacryl substituted polyhedral oligomeric silsesquioxane (POSS-MA) and 1-butyl-3-vinylimidazolium-bis[(trifluoromethyl)sulfonyl]imide (VBIMNTF 2 ) ionic liquid for use in capillary electrochromatography.

Fabrication of an ionic-liquid-based polymer monolithic column and its application in the fractionation of proteins from complex biosamples.

PubMed

Zhang, Doudou; Zhang, Qian; Bai, Ligai; Han, Dandan; Liu, Haiyan; Yan, Hongyuan

2018-05-01

An ionic-liquid-based polymer monolithic column was synthesized by free radical polymerization within the confines of a stainless-steel column (50 mm × 4.6 mm id). In the processes, ionic liquid and stearyl methacrylate were used as dual monomers, ethylene glycol dimethacrylate as the cross-linking agent, and polyethylene glycol 200 and isopropanol as co-porogens. Effects of the prepolymerization solution components on the properties of the resulting monoliths were studied in detail. Scanning electron microscopy, nitrogen adsorption-desorption measurements, and mercury intrusion porosimetry were used to investigate the morphology and pore size distribution of the prepared monoliths, which showed that the homemade ionic-liquid-based monolith column possessed a relatively uniform macropore structure with a total macropore specific surface area of 44.72 m 2 /g. Compared to a non-ionic-liquid-based monolith prepared under the same conditions, the ionic-liquid-based monolith exhibited excellent selectivity and high performance for separating proteins from complex biosamples, such as egg white, snailase, bovine serum albumin digest solution, human plasma, etc., indicating promising applications in the fractionation and analysis of proteins from the complex biosamples in proteomics research. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Highly efficient monolithic silica capillary columns modified with poly(acrylic acid) for hydrophilic interaction chromatography.

PubMed

Horie, Kanta; Ikegami, Tohru; Hosoya, Ken; Saad, Nabil; Fiehn, Oliver; Tanaka, Nobuo

2007-09-14

Monolithic silica capillary columns for hydrophilic interaction liquid chromatography (HILIC) were prepared by on-column polymerization of acrylic acid on monolithic silica in a fused silica capillary modified with anchor groups. The products maintained the high permeability (K=5 x 10(-14)m(2)) and provided a plate height (H) of less than 10 microm at optimum linear velocity (u) and H below 20 microm at u=6mm/s for polar solutes including nucleosides and carbohydrates. The HILIC mode monolithic silica capillary column was able to produce 10000 theoretical plates (N) with column dead time (t(0)) of 20s at a pressure drop of 20 MPa or lower. The total performance was much higher than conventional particle-packed HILIC columns currently available. The gradient separations of peptides by a capillary LC-electrospray mass spectrometry system resulted in very different retention selectivity between reversed-phase mode separations and the HILIC mode separations with a peak capacity of ca. 100 in a 10 min gradient time in either mode. The high performance observed with the monolithic silica capillary column modified with poly(acrylic acid) suggests that the HILIC mode can be an alternative to the reversed-phase mode for a wide range of compounds, especially for those of high polarity in isocratic as well as gradient elution.

Comprehensive two-dimensional HPLC to study the interaction of multiple components in Rheum palmatum L. with HSA by coupling a silica-bonded HSA column to a silica monolithic ODS column.

PubMed

Hu, Lianghai; Li, Xin; Feng, Shun; Kong, Liang; Su, Xingye; Chen, Xueguo; Qin, Feng; Ye, Mingliang; Zou, Hanfa

2006-04-01

A mode of comprehensive 2-D LC was developed by coupling a silica-bonded HSA column to a silica monolithic ODS column. This system combined the affinity property of the HSA column and the high-speed separation ability of the monolithic ODS column. The affinity chromatography with HSA-immobilized stationary phase was applied to study the interaction of multiple components in traditional Chinese medicines (TCMs) with HSA according to their affinity to protein in the first dimension. Then the unresolved components retained on the HSA column were further separated on the silica monolithic ODS column in the second dimension. By hyphenating the 2-D separation system to diode array detector and MS detectors, the UV and molecular weight information of the separated compounds can also be obtained. The developed separation system was applied to analysis of the extract of Rheum palmatum L., a number of low-abundant components can be separated on a single peak from the HSA column after normalization of peak heights. Six compounds were preliminarily identified according to their UV and MS spectra. It showed that this system was very useful for biological fingerprinting analysis of the components in TCMs and natural products.

Enantiomeric separation by capillary electrochromatography on a sulfated poly β-cyclodextrin modified silica-based monolith.

PubMed

Yuan, Ruijuan; Wang, Yan; Ding, Guosheng

2010-01-01

A sulfated poly β-cyclodextrin (SPCD) modified silica-based monolithic column was prepared for enantiomeric separation. First, 2-hydroxy-3-allyloxy-propyl-β-cyclodextrin (allyl-β-CD) was bonded onto a bifunctional reagent 3-(methacryloxy)propyltriethoxysilane (γ-MAPS) modified silica-based monolith through radical polymerization; the column was then sulfated with chlorosulfonic acid. The SPCD chiral stationary phase resolved the boring problem associated with desalting when sulfated CDs were synthesized to act as chiral additives. The inorganic salt in the column introduced during the sulfating process could be easily removed by washing the column with water for some time. Chiral compounds investigated were successfully resolved into their enantiomers on the SPCD modified monolith in the capillary electrochromatography (CEC) mode. Due to the existence of the -SO(3)H group, electrosmotic flow (EOF) was obviously increased, and all of the separations could be carried out in 20 min with only a minor loss in the column efficiency and resolution.

Ensuring repeatability and robustness of poly(glycidyl methacrylate-co-ethylene dimethacrylate) HPLC monolithic columns of 3 mm id through covalent bonding to the column wall.

PubMed

Laaniste, Asko; Kruve, Anneli; Leito, Ivo

2013-08-01

Two different methods to reinforce the poly(glycidyl methacrylate-co-ethylene dimethacrylate) HPLC monolithic columns of 3 mm id in a glass column reservoir were studied: composite columns with polymeric particles in the monolith and surface treatment of the reservoir wall. Of the two methods used to counter the mechanical instability and formation of flow channels (composite columns and column wall surface treatment), we demonstrated that proper column wall surface treatment was sufficient to solve both problems. Our study also indicated that no surface treatment is efficient, and of the methods studied silanization in acidified ethanol solution and constant renewal of the reaction mixture (dynamic mode) proved to be the most effective. As a result of this study, we have been able to prepare repeatable and durable methacrylate HPLC columns with good efficiencies. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

The synthesis of weak acidic type hybrid monolith via thiol-ene click chemistry and its application in hydrophilic interaction chromatography.

PubMed

Zeng, Jiao; Liu, Shengquan; Wang, Menglin; Yao, Shouzhuo; Chen, Yingzhuang

2017-05-01

In this work, a porous structure and good permeability monolithic column was polymerized in UV transparent fused-silica capillaries via photo-initiated thiol-ene click polymerization of 2,4,6,8-tetravinyl-2,4,6,8-tetramethylcyclotetrasiloxane (TMTVS), pentaerythritol tetra(3-mercaptopropionate)(PETMP), itaconic acid, respectively, in the presence of porogenic solvents (tetrahydrofuranand methanol) and an initiator (2,2-dimethoxy-2-phenylacetophenone) (DMPA) within 30 min. The physical properties of this monolith were characterized by scanning electron microscopy (SEM), Fourier transform infrared (FT-IR) spectroscopy and nitrogen adsorption/desorption measurements. For an overall evaluation of the monolith in chromatographic application, separations of polycyclic aromatic hydrocarbons (PAHs), phenols, amides and bases were carried out. The column efficiency of this monolith could be as high as 112 560 N/m. It also possesses a potential application in fabrication of monoliths with high efficiency for c-LC. In addition, the resulting monolithic column demonstrated the potential use in analysis of environment waters. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Capillary trap column with strong cation-exchange monolith for automated shotgun proteome analysis.

PubMed

Wang, Fangjun; Dong, Jing; Jiang, Xiaogang; Ye, Mingliang; Zou, Hanfa

2007-09-01

A 150 microm internal diameter capillary monolithic column with a strong cation-exchange stationary phase was prepared by direct in situ polymerization of ethylene glycol methacrylate phosphate and bisacrylamide in a trinary porogenic solvent consisting dimethylsulfoxide, dodecanol, and N,N'-dimethylformamide. This phosphate monolithic column exhibits higher dynamic binding capacity, faster kinetic adsorption of peptides, and more than 10 times higher permeability than the column packed with commercially available strong cation-exchange particles. It was applied as a trap column in a nanoflow liquid chromatography-tandem mass spectrometry system for automated sample injection and online multidimensional separation. It was observed that the sample could be loaded at a flow rate as high as 40 microL/min with a back pressure of approximately 1300 psi and without compromising the separation efficiency. Because of its good orthogonality to the reversed phase separation mechanism, the phosphate monolithic trap column was coupled with a reversed-phase column for online multidimensional separation of 19 microg of the tryptic digest of yeast proteins. A total of 1522 distinct proteins were identified from 5608 unique peptides (total of 54,780 peptides) at the false positive rate only 0.46%.

Monolithic poly(1,2-bis(p-vinylphenyl)ethane) capillary columns for simultaneous separation of low- and high-molecular-weight compounds.

PubMed

Greiderer, Andreas; Ligon, S Clark; Huck, Christian W; Bonn, Günther K

2009-08-01

Monolithic poly(1,2-bis(p-vinylphenyl)ethane (BVPE)) capillary columns were prepared by thermally initiated free radical polymerisation of 1,2-bis(p-vinylphenyl)ethane in the presence of inert diluents (porogens) and alpha,alpha'-azoisobutyronitrile (AIBN) as initiator. Polymerisations were accomplished in 200 microm ID fused silica capillaries at 65 degrees C and for 60 min. Mercury intrusion porosimetry measurements of the polymeric RP support showed a broad bimodal pore-size-distribution of mesopores and small macropores in the range of 5-400 nm and flow-channels in the mum range. N(2)-adsorption (BET) analysis resulted in a tremendous enhancement of surface area (101 m(2)/g) of BVPE stationary phases compared to typical organic monoliths (approximately 20 m(2)/g), indicating the presence of a considerable amount of mesopores. Consequently, the adequate proportion of both meso- and (small) macropores allowed the rapid and high-resolution separation of low-molecular-weight compounds as well as biomolecules on the same monolithic support. At the same time, the high fraction of flow-channels provided enhanced column permeability. The chromatographic performance of poly(1,2-bis(p-vinylphenyl)ethane) capillary columns for the separation of biomolecules (proteins, oligonucleotides) and small molecules (alkyl benzenes, phenols, phenons) are demonstrated in this article. Additionally, pressure drop versus flow rate measurements of novel poly(1,2-bis(p-vinylphenyl)ethane) capillary columns confirmed high mechanical robustness, low swelling in organic solvents and high permeability. Due to the simplicity of monolith fabrication, comprehensive studies of the retention and separation behaviour of monolithic BVPE columns resulted in high run-to-run and batch-to-batch reproducibilities. All these attributes prove the excellent applicability of monolithic poly(1,2-bis(p-vinylphenyl)ethane) capillary columns for micro-HPLC towards a huge range of analytes of different chemistries and molecular sizes.

Preparation and evaluation of a macroporous molecularly imprinted hybrid silica monolithic column for recognition of proteins by high performance liquid chromatography.

PubMed

Lin, Zian; Yang, Fan; He, Xiwen; Zhao, Xiaomiao; Zhang, Yukui

2009-12-04

A novel type of macroporous molecularly imprinted hybrid silica monolithic column was first developed for recognition of proteins. The macroporous silica-based monolithic skeleton was synthesized in a 4.6mm i.d. stainless steel column by a mild sol-gel process with methyltrimethoxysilane (MTMS) as a sole precursor, and then vinyl groups were introduced onto the surface of the silica skeleton by chemical modification of gamma-methacryloxypropyltrimethoxysilane (gamma-MAPS). Subsequently, the molecularly imprinted polymer (MIP) coating was copolymerized and anchored onto the surface of the silica monolith. Bovine serum albumin (BSA) and lysozyme (Lyz), which differ greatly in molecular size, isoelectric point, and charge, were representatively selected for imprinted templates to evaluate recognition property of the hybrid silica-based MIP monolith. Some important factors, such as template-monomer molar ratio, total monomer concentration and crosslinking density, were systematically investigated. Under the optimum conditions, the obtained hybrid silica-based MIP monolith showed higher binding affinity for template than its corresponding non-imprinted (NIP) monolith. The imprinted factor (IF) for BSA and Lyz reached 9.07 and 6.52, respectively. Moreover, the hybrid silica-based MIP monolith displayed favorable binding characteristics for template over competitive protein. Compared with the imprinted silica beads for stationary phase and in situ organic polymer-based hydrogel MIP monolith, the hybrid silica MIP monolith exhibited higher recognition, stability and lifetime.

Organic monolith frits encased in polyether ether ketone tubing with improved durability for liquid chromatography.

PubMed

Park, Sin Young; Cheong, Won Jo

2015-09-01

This study introduces a preparation method for polymer-encased monolith frits with improved durability for liquid chromatography columns. The inner surface of the polyether ether ketone tubing is pretreated with sulfuric acid in the presence of catalysts (vanadium oxide and sodium sulfate). The tubing was rinsed with water and acetone, flushed with nitrogen, and treated with glycidyl methacrylate. After washing, the monolith reaction mixture composed of lauryl methacrylate, ethylene glycol dimethacrylate, initiator, and porogenic solvent was filled in the tubing and subjected to in situ polymerization. The tubing was cut into thin slices and used as frits for microcolumns. To check their durability, the frit slices were placed in a vial and a heavy impact was applied on the vial by a vortex mixer for various periods. The frits made in the presence of catalysts were found to be more durable than those made without catalysts. Furthermore, when the monolith-incorporated tubing was used as a chromatography column, the column prepared in the presence of catalysts resulted in a better separation efficiency. The separation performance of the columns installed with the polyether ether ketone encased monolith frits was comparable to that of the columns installed with the commercial stainless-steel screen frits. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Controlling retention, selectivity and magnitude of EOF by segmented monolithic columns consisting of octadecyl and naphthyl monolithic segments--applications to RP-CEC of both neutral and charged solutes.

PubMed

Karenga, Samuel; El Rassi, Ziad

2011-04-01

Monolithic capillaries made of two adjoining segments each filled with a different monolith were introduced for the control and manipulation of the electroosmotic flow (EOF), retention and selectivity in reversed phase-capillary electrochromatography (RP-CEC). These columns were called segmented monolithic columns (SMCs) where one segment was filled with a naphthyl methacrylate monolith (NMM) to provide hydrophobic and π-interactions, while the other segment was filled with an octadecyl acrylate monolith (ODM) to provide solely hydrophobic interaction. The ODM segment not only provided hydrophobic interactions but also functioned as the EOF accelerator segment. The average EOF of the SMC increased linearly with increasing the fractional length of the ODM segment. The neutral SMC provided a convenient way for tuning EOF, selectivity and retention in the absence of annoying electrostatic interactions and irreversible solute adsorption. The SMCs allowed the separation of a wide range of neutral solutes including polycyclic aromatic hydrocarbons (PAHs) that are difficult to separate using conventional alkyl-bonded stationary phases. In all cases, the k' of a given solute was a linear function of the fractional length of the ODM or NMM segment in the SMCs, thus facilitating the tailoring of a given SMC to solve a given separation problem. At some ODM fractional length, the fabricated SMC allowed the separation of charged solutes such as peptides and proteins that could not otherwise be achieved on a monolithic column made from NMM as an isotropic stationary phase due to the lower EOF exhibited by this monolith. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Enhanced capabilities of separation in Sequential Injection Chromatography--fused-core particle column and its comparison with narrow-bore monolithic column.

PubMed

Chocholouš, Petr; Kosařová, Lucie; Satínský, Dalibor; Sklenářová, Hana; Solich, Petr

2011-08-15

In the Sequential Injection Chromatography (SIC) only monolithic columns for chromatographic separations have been used so far. This article presents the first use of fused-core particle packed column in an attempt to extend of the chromatographic capabilities of the SIC system. A new fused-core particle column (2.7 μm) Ascentis(®) Express C18 (Supelco™ Analytical) 30 mm × 4.6 mm brings high separation efficiency within flow rates and pressures comparable to monolithic column Chromolith(®) Performance RP-18e 100-3 (Merck(®)) 100 mm × 3 mm. Both columns matches the conditions of the commercially produced SIC system - SIChrom™ (8-port high-pressure selection valve and medium-pressure Sapphire™ syringe pump with 4 mL reservoir - maximal work pressure 1000 PSI) (FIAlab(®), USA). The system was tested by the separation of four estrogens with similar structure and an internal standard - ethylparaben. The mobile phase composed of acetonitrile/water (40/60 (v/v)) was pumped isocratic at flow rate 0.48 mL min(-1). Spectrophotometric detection was performed at wavelength of 225 nm and injected volume of sample solutions was 10 μL. The chromatographic characteristics of both columns were compared. Obtained results and conclusions have shown that both fused-core particle column and longer narrow shaped monolithic column bring benefits into the SIC method. Copyright © 2011 Elsevier B.V. All rights reserved.

Ion chromatography for determination of nitrite and nitrate in seawater using monolithic ODS columns.

PubMed

Ito, Kazuaki; Takayama, Yohichi; Makabe, Nobuyuki; Mitsui, Ryo; Hirokawa, Takeshi

2005-08-12

A fast and highly sensitive ion chromatographic method using monolithic ODS columns was developed for the determination of nitrite (NO2-) and nitrate (NO3-) in seawater. Two monolithic ODS columns (50 mm x 4.6 mm i.d. + 100 mm x 4.6 mm i.d.) connected in series were coated and equilibrated with 5 mM cetyltrimethylammonium chloride (CTAC) aqueous solution. The column efficiency with 0.5 M NaCl as the mobile phase did not decrease in spite of the increase in flow rate of the mobile phase. Thus, good chromatograms were obtained within 3 minutes for NO2- and NO3 in artificial seawater without interferences by coexisting ions. The detection limit (S/N = 3) with UV detection at 225 nm was 0.8 and 1.6 microg/L for NO2- and NO3-, respectively. The characteristics of the monolithic CTA(+)-coated ODS columns were discussed. The present method was successfully applied to the fast and sensitive determination of NO2- and NO3- in real seawater samples.

Significant viscosity dependent deviations from classical van Deemter theory in liquid chromatography with porous silica monolithic columns.

PubMed

Nesterenko, Pavel N; Rybalko, Marina A; Paull, Brett

2005-06-01

Significant deviations from classical van Deemter behaviour, indicative of turbulent flow liquid chromatography, has been recorded for mobile phases of varying viscosity on porous silica monolithic columns at elevated mobile phase flow rates.

Green synthesis of mesoporous molecular sieve incorporated monoliths using room temperature ionic liquid and deep eutectic solvents.

PubMed

Zhang, Li-Shun; Zhao, Qing-Li; Li, Xin-Xin; Li, Xi-Xi; Huang, Yan-Ping; Liu, Zhao-Sheng

2016-12-01

A hybrid monolith incorporated with mesoporous molecular sieve MCM-41 of uniform pore structure and high surface area was prepared with binary green porogens in the first time. With a mixture of room temperature ionic liquids and deep eutectic solvents as porogens, MCM-41 was modified with 3-(trimethoxysilyl) propyl methacrylate (γ-MPS) and the resulting MCM-41-MPS was incorporated into poly (BMA-co-EDMA) monoliths covalently. Because of good dispersibility of MCM-41-MPS in the green solvent-based polymerization system, high permeability and homogeneity for the resultant hybrid monolithic columns was achieved. The MCM-41-MPS grafted monolith was characterized by scanning electron microscopy, energy dispersive spectrometer area scanning, transmission electron microscopy, FT-IR spectra and nitrogen adsorption tests. Chromatographic performance of MCM-41-MPS grafted monolith was characterized by separating small molecules in capillary electrochromatography, including phenol series, naphthyl substitutes, aniline series and alkyl benzenes. The maximum column efficiency of MCM-41-MPS grafted monolith reached 209,000 plates/m, which was twice higher than the corresponding MCM-41-MPS free monolith. Moreover, successful separation of non-steroidal anti-inflammatory drugs and polycyclic aromatic hydrocarbons demonstrated the capacity in broad-spectrum application of the MCM-41-MPS incorporated monolith. The results indicated that green synthesis using room temperature ionic liquid and deep eutectic solvents is an effective method to prepare molecular sieve-incorporated monolithic column. Copyright © 2016 Elsevier B.V. All rights reserved.

Optimization of monolithic columns for microfluidic devices

NASA Astrophysics Data System (ADS)

Pagaduan, Jayson V.; Yang, Weichun; Woolley, Adam T.

2011-06-01

Monolithic columns offer advantages as solid-phase extractors because they offer high surface area that can be tailored to a specific function, fast mass transport, and ease of fabrication. Porous glycidyl methacrylate-ethylene glycol dimethacrylate monoliths were polymerized in-situ in microfluidic devices, without pre-treatment of the poly(methyl methacrylate) channel surface. Cyclohexanol, 1-dodecanol and Tween 20 were used to control the pore size of the monoliths. The epoxy groups on the monolith surface can be utilized to immobilize target-specific probes such as antibodies, aptamers, or DNA for biomarker detection. Microfluidic devices integrated with solid-phase extractors should be useful for point-of-care diagnostics in detecting specific biomarkers from complex biological fluids.

Monolithic column modified with bifunctional ionic liquid and styrene stationary phases for capillary electrochromatography.

PubMed

Mao, Zhenkun; Chen, Zilin

2017-01-13

A novel monolithic column with ionic liquid and styrene-modified bifunctional group was prepared for capillary electrochromatography (CEC) by in situ copolymerization in a ternary porogenic solvent. Ionic liquid (1-allyl-methylimidazolium chloride, AlMeIm + Cl - ) and styrene served as the bifunctional monomer, while ethylene dimethacrylate (EDMA) was used as the cross-linker. The monomer of AlMeIm + Cl - was introduced as anion-exchange group, while styrene as hydrophobic and aromatic group; the similar conjugated structure in AlMeIm + Cl - and styrene was beneficial for offeing obvious synergistic effect. The bifunctional stationary phase possessed powerful selectivity for the separation of neutral compounds, acidic analytes and phenols. The highest column efficiency was 2.70×10 5 platesm -1 (theoretical plates, N) for toluene. A relatively strong electroosmotic flow (EOF) was obtained in a wide range of pH values from 2.0 to 12.0, which could successfully achieve the rapid separation of the analytes within 10min. The proposed monolithic column was characterized by scanning electron microscopy (SEM) and Fourier transform infrared (FT-IR). The results indicated that the resultant monolithic column had good permeability and excellent mechanical stability. Good reproducibility was obtained with relative standard deviations (RSDs) of the retention time in the range of 0.24-0.47% and 0.81-2.17% for run-to-run (n=5) and day-to-day (n=5), while 1.09-2.70% and 0.98-1.70% for column-to-column (n=3) and batch-to-batch (n=3), respectively. The combination of AlMeIm + Cl - and styrene was a promising option in the fabrication of the organic polymer monolithic column. Copyright © 2016 Elsevier B.V. All rights reserved.

Graphene oxide-based composite monolith as new sorbent for the on-line solid phase extraction and high performance liquid chromatography determination of ß-sitosterol in food samples.

PubMed

Cui, Beijiao; Guo, Bin; Wang, Huimin; Zhang, Doudou; Liu, Haiyan; Bai, Ligai; Yan, Hongyuan; Han, Dandan

2018-08-15

A composite monolithic column was prepared by redox initiation method for the on-line purification and enrichment of β-sitosterol, in which graphene oxide (GO) was embedded. The obtained monolithic column was characterized by scanning electron microscopy (SEM) and nitrogen adsorption-desorption isotherm measurement, which indicated that the monolith possessed characteristics of porous structure and high permeability. Under the optimum conditions for extraction and determination, the calibration equation was y = 47.92 × -0.1391; the linear range was 0.008-1.0 mg mL -1 ; the linear regression coefficient was 0.998; the limit of detection (LOD) is 2.4 μg mL -1 ; the limit of quantitation (LOQ) was 8 μg mL -1 ; precisions for intra-day and inter-day assays presented as relative standard deviations were less than 4.3% and 6.8%, respectively. Under the selective conditions, the enrichment factor of the method was 119. The recovery was in the range of 80.40-98.00%. Moreover, the adsorption amount of the monolith was compared with silica gel-C18 adsorbent and the monolith without graphene oxide being embedded. The polymerization monolithic column showed high selectivity and good permeability, and it was successfully used as on-line solid-phase extraction (SPE) column for determination of β-sitosterol in edible oil. Copyright © 2018 Elsevier B.V. All rights reserved.

Novel method for the rapid and specific extraction of multiple β2 -agonist residues in food by tailor-made Monolith-MIPs extraction disks and detection by gas chromatography with mass spectrometry.

PubMed

Liu, Haibo; Gan, Ning; Chen, Yinji; Ding, Qingqing; Huang, Jie; Lin, Saichai; Cao, Yuting; Li, Tianhua

2016-09-01

A quick and specific pretreatment method based on a series of extraction clean-up disks, consisting of molecularly imprinted polymer monoliths and C18 adsorbent, was developed for the specific enrichment of salbutamol and clenbuterol residues in food. The molecularly imprinted monolithic polymer disk was synthesized using salbutamol as a template through a one-step synthesis process. It can simultaneously and specifically recognize salbutamol and clenbuterol. The monolithic polymer disk and series of C18 disks were assembled with a syringe to form a set of tailor-made devices for the extraction of target molecules. In a single run, salbutamol and clenbuterol can be specifically extracted, cleaned, and eluted by methanol/acetic acid/H2 O. The target molecules, after a silylation derivatization reaction were detected by gas chromatography-mass spectrometry. The parameters including solvent desorption, sample pH, and the cycles of reloading were investigated and discussed. Under the optimized extraction and clean-up conditions, the limits of detection and quantitation were determined as 0.018-0.022 and 0.042-0.049 ng/g for salbutamol and clenbuterol, respectively. The assay described was convenient, rapid, and specific; thereby potentially efficient in the high-throughput analysis of β2 -agonists residues in real food samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Radial heterogeneity of some analytical columns used in high-performance liquid chromatography.

PubMed

Abia, Jude A; Mriziq, Khaled S; Guiochon, Georges A

2009-04-10

An on-column electrochemical microdetector was used to determine accurately the radial distribution of the mobile phase velocity and of the column efficiency at the exit of three common analytical columns, namely a 100 mm x 4.6mm C18 bonded silica-based monolithic column, a 150 mm x 4.6mm column packed with 2.7 microm porous shell particles of C18 bonded silica (HALO), and a 150 mm x 4.6mm column packed with 3 microm fully porous C18 bonded silica particles (LUNA). The results obtained demonstrate that all three columns are not radially homogeneous. In all three cases, the efficiency was found to be lower in the wall region of the column than in its core region (the central core with a radius of 1/3 the column inner radius). The decrease in local efficiency from the core to the wall regions was lower in the case of the monolith (ca. 25%) than in that of the two particle-packed columns (ca. 35-50%). The mobile phase velocity was found to be ca. 1.5% higher in the wall than in the core region of the monolithic column while, in contrast, it was ca. 2.5-4.0% lower in the wall region for the two particle-packed columns.

Polar and nonpolar organic polymer-based monolithic columns for capillary electrochromatography and high-performance liquid chromatography.

PubMed

Rathnasekara, Renuka; Khadka, Shantipriya; Jonnada, Murthy; El Rassi, Ziad

2017-01-01

This review article is a continuation of the previous reviews on the area of monolithic columns covering the progress made in the field over the last couple of years from the beginning of the second half of 2014 until the end of the first half of 2016. It summarizes and evaluates the evolvement of both polar and nonpolar organic monolithic columns and their use in hydrophilic interaction LC and CEC and reversed-phase chromatography and RP-CEC. The review article discusses the results reported in a total of 62 references. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Triazine herbicide imprinted monolithic column for capillary electrochromatography.

PubMed

Aşır, Süleyman; Derazshamshir, Ali; Yılmaz, Fatma; Denizli, Adil

2015-12-01

Trietazine was selectively separated from aqueous solution containing the competitor molecule cyanazine, which is similar in size and shape to the template molecule. Structural features of the molecularly imprinted column were figured out by SEM. The influence of the mobile-phase composition, applied electrical field, and pH of the mobile phase on the recognition of trietazine by the imprinted monolithic polymer has been evaluated, and the imprint effect in the trietazine-imprinted monolithic polymer was demonstrated by an imprinting factor. The optimized monolithic column resulted in separation of trietazine from a structurally related competitor molecule, cyanazine. In addition, fast separation was obtained within 6 min by applying higher electrical field, with the electrophoretic mobility of 2.97 × 10(-8) m(2) V(-1) s(-1) at pH 11.0. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Characteristic of theophylline imprinted monolithic column and its application for determination of xanthine derivatives caffeine and theophylline in green tea.

PubMed

Sun, Han-wen; Qiao, Feng-xia; Liu, Guang-yu

2006-11-17

Theophylline imprinted monolithic columns were designed and prepared for rapid separation of a homologous series of xanthine derivatives, caffeine, and theophylline by an in situ thermal-initiated copolymerization technique. Caffeine and theophylline were fully separated both under isocratic and gradient elutions on this kind of monolithic molecularly imprinted polymers (MIP) column. The broad peak showed in isocratic elution could be improved in gradient elution. Some chromatographic conditions such as mobile phase composition, flow rate, and the temperature on the retention times were investigated. Hydrogen bonding interaction and hydrophobic interaction played an important role in the retention and separation. The binding capacity was evaluated by static adsorption and Scatchard analysis, which showed that the dissociation constant (KD) and the maximum binding capacity (Qmax) were 1.50 mol/L, and 236 micromol/g for high affinity binding site, and 7.97 mol/L and 785 micromol/g for lower affinity binding site, respectively. Thermodynamic data (DeltaDeltaH and DeltaDeltaS) obtained by Van't Hoff plots revealed an enthalpy-controlled separation. The morphological characteristics of monolithic MIP were investigated by scanning electron microscope, which showed that both mesopores and macropores were formed in the monolith. The present monolithic MIP column was successfully applied for the quantitative determination of caffeine and theophylline in different kinds of green tea.

Controlled crosslinking of trimethylolpropane trimethacrylate for preparation of organic monolithic columns for capillary liquid chromatography.

PubMed

Gama, Mariana R; Aggarwal, Pankaj; Lee, Milton L; Bottoli, Carla B G

2017-11-01

Organic monolithic columns based on single crosslinking of trimethylolpropane trimethacrylate (TRIM) monomer were prepared in a single step by living/controlled free-radical polymerization. Full optimization of the preparation, such as using different percentages of TRIM and different amounts of radical promoter as well as various porogen solvents were explored. The resulting monolithic columns were characterized by scanning electronic microscopy and nitrogen sorption for structure morphology studies and surface area measurements, respectively. Using capillary liquid chromatography, 150 μm i.d. columns were applied to separate a mixture of small hydrophobic molecules. The results indicated that column performance is highly sensitive to the type and the amount of porogen solvents used in the polymerization mixture composition. Good resolution factors and methylene selectivity were obtained, indicating the promising potential of this material for capillary liquid chromatography separations. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A silica monolithic column prepared by the sol-gel process for enantiomeric separation by capillary electrochromatography.

PubMed

Kang, Jingwu; Wistuba, Dorothee; Schurig, Volker

2002-04-01

A method for the preparation of a silica monolithic capillary electrochromatography (CEC) column for the separation of enantiomers has been developed. The porous silica monolith was fabricated inside a fused-silica capillary column by using the sol-gel process. After gelation for 24 h, hydrothermal treatment at 100 degrees C for 24 h was performed to prevent the sol-gel matrix from cracking. The prepared monolith was then coated with Chirasil-beta-Dex which represents a chiral polymer prepared by grafting permethyl-beta-cyclodextrin to polymethylsiloxane with an octamethylene spacer. Immobilization of Chirasil-beta-Dex was performed by heat treatment at 120 degrees C for 48 h to give a nonextractable coating. The column performance was evaluated by using racemic hexobarbital as a model compound. The efficiency of 9.2 x 10(4) theoretical plates/m for the first eluted enantiomer of hexobarbital was obtained at an optimal flow rate of the mobile phase. The effect of mobile phase composition on enantiomeric separation of hexobarbital was also investigated. The column proved to be stable for more than one hundreds of runs during a two-months period. The enantiomers of several neutral and negatively charged chiral compounds were baseline separated on this column.

HPLC determination of cefprozil in tablets using monolithic and C18 silica columns.

PubMed

Can, Nafiz O

2011-08-01

Cefprozil (CPZ) is a second-generation semi-synthetic cephalosporin antibiotic that commonly exists as the mixture of Z and E diastereoisomers, at the ratio of approximately 9:1. A novel reversed-phase HPLC method for the determination of CPZ in tablets was described. The separation of CPZ diastereoisomers and caffeine (internal standard) was carried out by applying the same analytical and instrumental conditions on two stationary phases, which have different surface chemistries. The columns used in the study were monolithic silica Merck Chromolith Performance RP-18e and conventional C18 silica Phenomenex Synergi Hydro RP columns. In total, 10 μL aliquots of samples were injected into the system and eluted using water-acetonitrile (90:10, v/v) solution, which was pumped through the column at a flow rate of 1.0 mL/min. The analyte peaks were detected at 200 nm using diode array detector with high specificity. CPZ diastereoisomers and caffeine were measured within 13 min using the C18 column, whereas <5 min was required for the monolithic one. Validation studies were performed according to official recommendations. Value of a monolithic column for the assay of diastereoisomers in pharmaceutical tablets was evaluated for the first time and found as a powerful alternative to highly efficient C18 columns. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Influence of the linking spacer length and type on the enantioseparation ability of β-cyclodextrin functionalized monoliths.

PubMed

Guo, Jialiang; Xiao, Yuan; Lin, Yuanjing; Zhang, Qiaoxuan; Chang, Yiqun; Crommen, Jacques; Jiang, Zhengjin

2016-05-15

In order to investigate the effect of the linking spacer on the enantioseparation ability of β-cyclodextrin (β-CD) functionalized polymeric monoliths, three β-CD-functionalized organic polymeric monoliths with different spacer lengths were prepared by using three amino-β-CDs, i.e. mono-6-amino-6-deoxy-β-CD, mono-6-ethylenediamine-6-deoxy-β-CD, mono-6-hexamethylenediamine-6-deoxy-β-CD, as starting materials. These amino-β-CDs reacted with glycidyl methacrylate to produce functional monomers which were then copolymerized with ethylene dimethacrylate. The enantioseparation ability of the three monoliths was evaluated using 14 chiral acidic compounds, including mandelic acid derivatives, nonsteroidal anti-inflammatory drugs, N-derivatized amino acids, and chiral herbicides under optimum chromatographic conditions. Notably, the poly(GMA-NH2-β-CD-co-EDMA) column provides higher enantioresolution and enantioselectivity than the poly(GMA-EDA-β-CD-co-EDMA) and poly(GMA-HDA-β-CD-co-EDMA) columns for most tested chiral analytes. Furthermore, the enantioseparation performance of triazole-linker containing monoliths was compared to that of ethylenediamine-linker containing monoliths. The results indicate that the enantioselectivity of β-CD monolithic columns is strongly related to the length and type of spacer tethering β-CD to the polymeric support. Copyright © 2016 Elsevier B.V. All rights reserved.

Synthesis of zirconia monoliths for chromatographic separations.

PubMed

Randon, Jérôme; Huguet, Samuel; Piram, Anne; Puy, Guillaume; Demesmay, Claire; Rocca, Jean-Louis

2006-03-17

The aim of this work is to join the advantages of two different kinds of stationary phases: monolithic columns and zirconia-based supports. On the one hand, silica monolithic columns allow a higher efficiency with a lower back-pressure than traditional packed columns. On the other hand, chromatographic stationary phases based on zirconia have a higher thermal and chemical stability and specific surface properties. Combining these advantages, a zirconia monolith with a macroporous framework could be a real improvement in separation sciences. Two main strategies can be used in order to obtain a zirconia surface on a monolithic skeleton: coating or direct synthesis. The coverage by a zirconia layer of the surface of a silica-based monolith can be performed using the chemical properties of the silanol surface groups. We realized this coverage using zirconium alkoxide and we further grafted n-dodecyl groups using phosphate derivatives. Any loss of efficiency was observed and fast separations have been achieved. The main advance reported in this paper is related to the preparation of zirconia monoliths by a sol-gel process starting from zirconium alkoxide. The synthesis parameters (hydrolysis ratio, porogen type, precursor concentration, drying step, etc.) were defined in order to produce a macroporous zirconia monoliths usable in separation techniques. We produced various homogeneous structures: zirconia rod 2 cm long with a diameter of 2.3 mm, and zirconia monolith inside fused silica capillaries with a 75 microm I.D. These monoliths have a skeleton size of 2 microm and have an average through pore size of 6 microm. Several separations have been reported.

Cyclodextrins as a chiral mobile phase additive in nano-liquid chromatography: comparison of reversed-phase silica monolithic and particulate capillary columns.

PubMed

Rocco, Anna; Maruška, Audrius; Fanali, Salvatore

2012-03-01

Enantioseparations of racemic nonsteroidal anti-inflammatory drugs (naproxen, ibuprofen, ketoprofen, flurbiprofen, suprofen, indoprofen, cicloprofen, and carprofen) were performed by nano-liquid chromatography, employing achiral capillary columns and heptakis(2,3,6-tri-O-methyl)-β-cyclodextrin (TM-β-CD) or hydroxylpropyl-β-cyclodextrin (HP-β-CD) as a chiral mobile phase additive (CMPA). Working under the same experimental conditions (in terms of mobile phase and linear velocity), the performance of a RP-C18 monolithic column was compared with that of a RP-C18 packed column of the same dimensions (100 μm i.d. × 10 cm). Utilizing a mobile phase composed of 30% ACN (v/v) buffered with 50 mM sodium acetate at pH 3, and containing 30 mM TM-β-CD, the monolithic column provided faster analysis but lower resolution than the packed column. This behavior was ascribed to the high permeability of the monolithic column, as well as to its minor selectivity. HP-β-CD was chosen as an alternative to TM-β-CD. Employing the monolithic column, the effects of different parameters such as HP-β-CD concentration, mobile phase composition, and pH on the retention factor and the chiral resolution of the analytes were studied. For the most of the analytes, enantioresolution (which ranged from R(s) = 1.80 for naproxen to R(s) = 0.86 for flurbiprofen) was obtained with a mobile phase consisting of sodium acetate buffer (25 mM, pH 3), 10% MeOH, and 15 mM HP-β-CD. When the same experimental conditions were used with the packed column, no compound eluted within 1 h. Upon increasing the percentage of organic modifier to favor analyte elution, only suprofen eluted within 30 min, with an R(s) value of 1.14 (20% MeOH). Replacing MeOH with ACN resulted in a loss of enantioresolution, except for naproxen (R(s) = 0.89).

The effect of charged groups on hydrophilic monolithic stationary phases on their chromatographic properties.

PubMed

Li, Haibin; Liu, Chusheng; Wang, Qiqin; Zhou, Haibo; Jiang, Zhengjin

2016-10-21

In order to investigate the effect of charged groups present in hydrophilic monolithic stationary phases on their chromatographic properties, three charged hydrophilic monomers, i.e. N,N-dimethyl-N-acryloyloxyethyl-N-(3-sulfopropyl)ammonium betaine (SPDA), [2-(acryloyloxy)ethyl]trimethylammonium chloride (AETA), and 3-sulfopropyl acrylate potassium salt (SPA) were co-polymerized with the crosslinker N,N'-methylenebisacrylamide (MBA), respectively. The physicochemical properties of the three resulting charged hydrophilic monolithic columns were evaluated using scanning electron microscopy, ζ-potential analysis and micro-HPLC. High column efficiency was obtained on the three monolithic columns at a linear velocity of 1mm/s using thiourea as test compound. Comparative characterization of the three charged HILIC phases was then carried out using a set of model compounds, including nucleobases, nucleosides, benzoic acid derivatives, phenols, β-blockers and small peptides. Depending on the combination of stationary phase/mobile phase/solute, both hydrophilic interaction and other potential secondary interactions, including electrostatic interaction, hydrogen-bonding interaction, molecular shape selectivity, could contribute to the over-all retention of the analytes. Because of the strong electrostatic interaction provided by the quaternary ammonium groups in the poly (AETA-co-MBA) monolith, this cationic HILIC monolith exhibited the strongest retention for benzoic acid derivatives and small peptides with distorted peak shapes and the weakest retention for basic β-blockers. The sulfonyl groups on the poly (SPA-co-MBA) hydrophilic monolith could provide strong electrostatic attraction and hydrogen bonding for positively charged analytes and hydrogen-donor/acceptor containing analytes, respectively. Therefore, basic drugs, nucleobases and nucleotides exhibited the strongest retention on this anionic monolith. Because of the weak but distinct cation exchange properties of the zwitterionic poly (SPDA-co-MBA) hydrophilic monolith, it exhibited the best separation for most test analytes (including phenols, β-blockers and small peptides) in terms of selectivity, peak shape and analysis time. The poly (AETA-co-MBA) hydrophilic monolithic column provides the best separation of nucleobases and nucleosides. These results could guide the selection and application of these charged HILIC monoliths in the future. Copyright © 2016 Elsevier B.V. All rights reserved.

Development of a γ-alumina- nanoparticle-functionalized porous polymer monolith for the enrichment of Sudan dyes in red wine samples.

PubMed

Li, Wanjun; Zhou, Xiao; Ye, Juanjuan; Jia, Qiong

2013-10-01

Monolithic materials were synthesized in capillaries by in situ polymerization with N-isopropylacrylamide, glycidyl methacrylate, and ethylene dimethacrylate as the monomers, and methanol and PEG as the porogens. With γ-alumina nanoparticles attached to the surface of the porous monolithic column via epoxide groups, a novel polymer monolith microextraction (PMME) material was prepared with a good mechanical stability and a high extraction capacity. SEM and X-ray photoelectron spectroscopy were employed to characterize the modified monolithic column, demonstrating that γ-alumina nanoparticles were effectively functionalized onto the monolithic column. In addition, a new method was developed for the analysis of Sudan I-IV dyes using PMME coupled with HPLC. In order to obtain the optimum extraction efficiency, the PMME conditions including desorption solvent type, sample pH, sample volume, sample flow rate, and eluent flow rate were investigated. Under the optimum conditions, we obtained acceptable linearities, low LODs, and good intra- and interday RDSs. When applied to the determination of Sudan I-IV dyes in red wine samples, satisfactory recoveries were obtained in the range of 84.0-115.9%. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of azithromycin residue in pork using a molecularly imprinted monolithic microcolumn coupled to liquid chromatography with tandem mass spectrometry.

PubMed

Zhou, Tong; Yang, Haicui; Jin, Zhen; Liu, Qingying; Song, Xuqin; He, Limin; Fang, Binghu; Meng, Chenying

2016-04-01

Using spiramycin as a dummy template, a molecularly imprinted polymer monolithic micro-column with high selection to azithromycin was prepared in a micropipette tip. The imprinting factor of the monolithic micro-column prepared was approximately 2.67 and the morphological structure of the polymers was characterized by scanning electron microscopy. A simple, sensitive, and reproducible method based on the imprinted monolithic micro-column coupled to liquid chromatography with tandem mass spectrometry was developed for determining the residues of azithromycin in pork. Pork samples were extracted with acetonitrile, cleaned up under the optimal monolithic micro-column conditions, and analyzed using liquid chromatography with tandem mass spectrometry in the multiple reaction monitoring mode. The assay exhibited a linear dynamic range of 0.50-50 μg/L with the correlation coefficient (r(2) ) above 0.99. In the three spiking levels of 0.50, 1.0, and 10 μg/kg, the average recoveries of azithromycin from pork samples were between 85.8 and 96.5% with a relative standard deviation below 10%. The limit of detection and limit of quantitation were 0.03 and 0.1 μg/kg, respectively. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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.

PubMed

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. Copyright © 2016 Elsevier B.V. All rights reserved.

Hydrodynamic chromatography of macromolecules using polymer monolithic columns.

PubMed

Edam, Rob; Eeltink, Sebastiaan; Vanhoutte, Dominique J D; Kok, Wim Th; Schoenmakers, Peter J

2011-12-02

The selectivity window of size-based separations of macromolecules was tailored by tuning the macropore size of polymer monolithic columns. Monolithic materials with pore sizes ranging between 75 nm and 1.2 μm were prepared in situ in large I.D. columns. The dominant separation mechanism was hydrodynamic chromatography in the flow-through pores. The calibration curves for synthetic polymers matched with the elution behavior by HDC separations in packed columns with 'analyte-to-pore' aspect ratios (λ) up to 0.2. For large-macropore monoliths, a deviation in retention behavior was observed for small polystyrene polymers (M(r)<20 kDa), which may be explained by a combined HDC-SEC mechanism for λ<0.02. The availability of monoliths with very narrow pore sizes allowed investigation of separations at high λ values. For high-molecular weight polymers (M(r)>300,000 Da) confined in narrow channels, the separation strongly depended on flow rate. Flow-rate dependent elution behavior was evaluated by calculation of Deborah numbers and confirmed to be outside the scope of classic shear deformation or slalom chromatography. Shear-induced forces acting on the periphery of coiled polymers in solution may be responsible for flow-rate dependent elution. Copyright © 2011 Elsevier B.V. All rights reserved.

Mechanism of molecular recognition on molecular imprinted monolith by capillary electrochromatography.

PubMed

Liu, Zhao-Sheng; Xu, Yan-Li; Yan, Chao; Gao, Ru-Yu

2005-09-16

The recognition mechanism of molecularly imprinted polymer (MIP) in capillary electrochromatography (CEC) is complicated since it possesses a hybrid process, which comprises the features of chromatographic retention, electrophoretic migration and molecular imprinting. For an understanding of the molecular recognition of MIP in CEC, a monolithic MIP in a capillary with 1,1'-binaphthyl-2,2'-diamine (BNA) imprinting was prepared by in situ copolymerization of imprinted molecule, methacrylic acid and ethylene glycol dimethacrylate in porogenic solvent, a mixture of toluene-isooctane. Strong recognition ability and high column performance (theory plates was 43,000 plates/m) of BNA were achieved on this monolithic MIP in CEC mode. In addition, BNA and its structural analogue, 1,1'-bi-2, 2'-naphthol, differing in functional groups, were used as model compounds to study imprinting effect on the resultant BNA-imprinted monolithic column, a reference column without imprinting of BNA and a open capillary. The effects of organic modifier concentration, pH value of buffer, salt concentration of buffer and column temperature on the retention and recognition of two compounds were investigated. The results showed that the molecular recognition on MIP monolith in CEC mode mainly derived from imprinting cavities on BNA-imprinted polymer other than chromatographic retention and electrophoretic migration.

On chip preconcentration and fluorescence labeling of model proteins by use of monolithic columns: device fabrication, optimization, and automation.

PubMed

Yang, Rui; Pagaduan, Jayson V; Yu, Ming; Woolley, Adam T

2015-01-01

Microfluidic systems with monolithic columns have been developed for preconcentration and on-chip labeling of model proteins. Monoliths were prepared in microchannels by photopolymerization, and their properties were optimized by varying the composition and concentration of the monomers to improve flow and extraction. On-chip labeling of proteins was achieved by driving solutions through the monolith by use of voltage then incubating fluorescent dye with protein retained on the monolith. Subsequently, the labeled proteins were eluted, by applying voltages to reservoirs on the microdevice, and then detected, by monitoring laser-induced fluorescence. Monoliths prepared from octyl methacrylate combine the best protein retention with the possibility of separate elution of unattached fluorescent label with 50% acetonitrile. Finally, automated on-chip extraction and fluorescence labeling of a model protein were successfully demonstrated. This method involves facile sample pretreatment, and therefore has potential for production of integrated bioanalysis microchips.

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

PubMed

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. Copyright © 2015 Elsevier B.V. All rights reserved.

Zeolitic imidazolate framework-methacrylate composite monolith characterization by inverse gas chromatography.

PubMed

Yusuf, Kareem; Badjah-Hadj-Ahmed, Ahmed Yacine; Aqel, Ahmad; Aouak, Taieb; ALOthman, Zeid Abdullah

2016-04-22

Thermodynamic characterization of butyl methacrylate-co-ethylene dimethacrylate neat monolith and zeolitic imidazolate framework-8 incorporated with butyl methacrylate-co-ethylene dimethacrylate composite monolith were studied using inverse gas chromatography at infinite dilution under 1MPa column pressure and various column temperatures. The free energy of adsorption (ΔGA), enthalpy of adsorption (ΔHA) and entropy of adsorption (ΔSA) were determined using a series of n-alkanes. The dispersive component of surface energy (γS(D)) was estimated by Dorris-Gray and Schultz et al. The composite monolith showed a more energetic surface than the neat monolith. The acidic, KA, and basic, KD, parameters for both materials were estimated using a group of polar probes. A basic character was concluded with more basic behavior for the neat monolith. Flory-Huggins parameter, χ, was taken as a measure of miscibility between the probes with the low molecular weight and the high molecular weight monolith. Inverse gas chromatography provides a better understanding of the role of incorporated zeolitic imidazolate framework (ZIF-8) into the polymer matrix in its monolithic form. Copyright © 2016 Elsevier B.V. All rights reserved.

Covalent attachment of polymeric monolith to polyether ether ketone (PEEK) tubing.

PubMed

Lv, Chunguang; Heiter, Jaana; Haljasorg, Tõiv; Leito, Ivo

2016-08-17

A new method of reproducible preparation of vinylic polymeric monolithic columns with a key step of covalently anchoring the monolith to PEEK surface is described. In order to chemically attach the polymer monolith to the tube wall, methacrylate functional groups were introduced onto PEEK surface by a three-step procedure, including surface etching, surface reduction and surface methacryloylation. The chemical state of the modified tubing surface was characterized by attenuated total reflectance infrared (ATR-IR) spectroscopy. It was found that the etching step is the key to successfully modifying the PEEK tubing surface. Poly(styrene-co-divinylbenzene) monoliths were in situ synthesized by thermally initiated free radical copolymerization within the confines of surface-vinylized PEEK tubings of dimensions close to ones conventionally used in HPLC and UHPLC (1.6 mm internal diameter, 10.0-12.5 cm length). Adhesion test was done by measuring the operating pressure drop, which the prepared stationary phases can withstand. Good pressure resistance, up to 140 bar/10 cm (flow rate 0.5 mL min(-1), acetonitrile as a mobile phase), indicates strong bonding of monolith to the tubing wall. The monolithic material was proven to have a permeability of 1.7 × 10 (-14) m(2), applying acetonitrile-water 70:30 (v/v) as a mobile phase. The column performance was reproducible from column to column and was evaluated via the isocratic separation of a series of alkylbenzenes in the reversed-phase mode (acetonitrile-water 70:30, v/v). The numbers of plates per meter at optimal flow rate were found to be between 26 000 and 32 000 for the different analytes. Copyright © 2016 Elsevier B.V. All rights reserved.

A poly(alkyl methacrylate-divinylbenzene-vinylbenzyl trimethylammonium chloride) monolithic column for solid-phase microextraction.

PubMed

Liu, Wan-Ling; Lirio, Stephen; Yang, Yicong; Wu, Lin-Tai; Hsiao, Shu-Ying; Huang, Hsi-Ya

2015-05-22

In this study, an organic polymer monolithic columns, which were prepared via in situ polymerization of alkyl methacrylate-ester (AMA), divinylbenzene (DVB) and vinylbenzyl trimethylammonium chloride (VBTA, charged monomer), were developed as adsorbent for solid-phase microextraction (SPME). Different parameters affecting the extraction efficiency for nine (9) non-steroidal anti-inflammatory drugs (NSAIDs) such as the ratio of the stearyl methacrylate (SMA) to DVB monomer, column length, sample pH, extraction flow rate and desorption solvent were investigated to obtain the optimal SPME condition. Also, the permeability for each poly(AMA-DVB-VBTA) monolithic column was investigated by adding porogenic solvent (poly(ethylene glycol), PEG). Using the optimized condition, a series of AMA-based poly(AMA-DVB-VBTA) monolith columns were developed to determine the effect the extraction efficiency of NSAIDs by varying the alkyl chain length of the methacrylate ester (methyl-, butyl-, octyl-, or lauryl-methacrylate; (MMA, BMA, OMA, LMA)). Results showed that decreasing the AMA chain length increases the extraction efficiency of some NSAIDs (i.e. sulindac (sul), naproxen (nap), ketoprofen (ket) and indomethacin (idm)). Among the poly(AMA-DVB-VBTA) monolithic columns, poly(BMA-DVB-VBTA) showed a highly repeatable extraction efficiency for NSAIDs with recoveries ranging from 85.0 to 100.2% with relative standard deviation (RSD) less than 6.8% (n=3). The poly(BMA-DVB-VBTA) can also be reused for at least 50 times without any significant effect in extraction efficiency for NSAIDs. Finally, using the established conditions, the poly(BMA-DVB-VBTA) was used to extract trace-level NSAIDs (100μgL(-1)) in river water with good recoveries ranging from 75.8 to 90.8% (RSD<14.9%). Copyright © 2015 Elsevier B.V. All rights reserved.

Fabrication of zeolitic imidazolate framework-8-methacrylate monolith composite capillary columns for fast gas chromatographic separation of small molecules.

PubMed

Yusuf, Kareem; Badjah-Hadj-Ahmed, Ahmed Yacine; Aqel, Ahmad; ALOthman, Zeid Abdullah

2015-08-07

A composite zeolitic imidazolate framework-8 (ZIF-8) with a butyl methacrylate-co-ethylene dimethacrylate (BuMA-co-EDMA) monolithic capillary column (33.5cm long×250μm i.d.) was fabricated to enhance the separation efficiency of methacrylate monoliths toward small molecules using conventional low-pressure gas chromatography in comparison with a neat butyl methacrylate-co-ethylene dimethacrylate (BuMA-co-EDMA) monolithic capillary column (33.5cm long×250μm i.d.). The addition of 10mgmL(-1) ZIF-8 micro-particles increased the BET surface area of BuMA-co-EDMA by 3.4-fold. A fast separation of five linear alkanes in 36s with high resolution (Rs≥1.3) was performed using temperature program. Isothermal separation of the same sample also showed a high efficiency (3315platesm(-1) for octane) at 0.89min. Moreover, the column was able to separate skeletal isomers, such as iso-octane/octane and 2-methyl octane/nonane. In addition, an iso-butane/iso-butylene gas mixture was separated at ambient temperature. Comparison with an open tubular TR-5MS column (30m long×250μm i.d.) revealed the superiority of the composite column in separating the five-membered linear alkane mixture with 4-5 times increase in efficiency and a total separation time of 0.89min instead of 4.67min. A paint thinner sample was fully separated using the composite column in 2.43min with a good resolution (Rs≥0.89). The perfect combination between the polymeric monolith, with its high permeability, and ZIF-8, with its high surface area and flexible 0.34nm pore openings, led to the fast separation of small molecules with high efficiency and opened a new horizon in GC applications. Copyright © 2015 Elsevier B.V. All rights reserved.

Advances in organic polymer-based monolithic column technology for high-resolution liquid chromatography-mass spectrometry profiling of antibodies, intact proteins, oligonucleotides, and peptides.

PubMed

Eeltink, Sebastiaan; Wouters, Sam; Dores-Sousa, José Luís; Svec, Frantisek

2017-05-19

This review focuses on the preparation of organic polymer-based monolithic stationary phases and their application in the separation of biomolecules, including antibodies, intact proteins and protein isoforms, oligonucleotides, and protein digests. Column and material properties, and the optimization of the macropore structure towards kinetic performance are also discussed. State-of-the-art liquid chromatography-mass spectrometry biomolecule separations are reviewed and practical aspects such as ion-pairing agent selection and carryover are presented. Finally, advances in comprehensive two-dimensional LC separations using monolithic columns, in particular ion-exchange×reversed-phase and reversed-phase×reversed-phase LC separations conducted at high and low pH, are shown. Copyright © 2017 Elsevier B.V. All rights reserved.

Preparation of clenbuterol imprinted monolithic polymer with hydrophilic outer layers by reversible addition-fragmentation chain transfer radical polymerization and its application in the clenbuterol determination from human serum by on-line solid-phase extraction/HPLC analysis.

PubMed

Li, Xiaobing; Zhou, Man; Turson, Mamat; Lin, Shen; Jiang, Ping; Dong, Xiangchao

2013-05-21

A novel imprinted monolithic material with the ability of protein exclusion was developed for the selective extraction of clenbuterol (CLE) from biological samples by direct injection in the HPLC analysis. The material has an imprinted inner structure and hydrophilic outer layer. The reversible addition-fragmentation chain transfer (RAFT) polymerization was employed in the material preparation by a two-step procedure. In the first step, clenbuterol imprinted monolithic polymer was synthesized by combining the molecular imprinting and the RAFT polymerization techniques. The resulting monolithic polymer has a RAFT chain transfer agent (trithioester groups) in its structure, which was used to graft poly(glycerol mono-methacrylate) [pGMMA] in the second step by post-RAFT polymerization. The hydrophilic pGMMA layers grafted on the surface of the imprinted monolith created barriers for protein diffusion. More than 90% of bovine serum albumin can be excluded from the pGMMA coated monolithic column. Meanwhile the clenbuterol was retained selectively with a large retention factor. The result indicated that the column, denoted as RA-MIM, has both the merits of a molecularly imprinted polymer and restricted access material. By using RA-MIM as the solid-phase extraction pre-column, an on-line column-switching HPLC method for the determination of clenbuterol in human serum has been established and validated. The recoveries of clenbuterol from the serum were 87.3-96.9% in the spiked level 2-1000 ng mL(-1). Both good linearity (R = 0.999) and acceptable reproducibility (RSD < 7.0%) were obtained. The limit of detection and the limit of quantitation were 0.7 ng mL(-1) and 2.0 ng mL(-1) respectively, which is sensitive in terms of UV detection. The results have demonstrated that the RAFT polymerization can be used to synthesize bi-functional monolithic columns by using its living reaction property. The resulting RA-MIM in this research can be used for efficient clenbuterol determination by HPLC from biological samples.

Ultrafast UPLC-ESI-MS and HPLC with monolithic column for determination of principal flavor compounds in vanilla pods.

PubMed

Sharma, Upendra K; Sharma, Nandini; Sinha, Arun K; Kumar, Neeraj; Gupta, Ajai P

2009-10-01

In this study, two novel chromatographic methods based on monolithic column high-performance liquid chromatography (HPLC) and ultra-performance liquid chromatography (UPLC) were developed for the ultrafast determination of principal flavor compounds namely vanillin, vanillic acid, p-hydroxybenzoic acid, and p-hydroxybenzaldehyde in ethanolic extracts of Vanilla planifolia pods. Good separation was achieved within 2.5 min using Chromolith RP18e column (100 mm x 4.6 mm) for HPLC and Acquity BEH C-18 (100 mm x 2.1 mm, 1.7 microm) column for UPLC. Both methods were compared in terms of total analysis time, mobile phase consumption, sensitivity, and validation parameters like precision, accuracy, LOD, and LOQ. Further, system suitability test data including resolution, capacity factor, theoretical plates, and tailing factor was determined for both the methods by ten replicate injections. Monolithic column based HPLC gave better results for most of the selected parameters while UPLC was found to be more eco-friendly with low mobile phase consumption and better sensitivity. Both methods may be used conveniently for the high throughput analysis of large number of samples in comparison to traditional particulate column.

Monolithic stationary phases with a longitudinal gradient of porosity.

PubMed

Urban, Jiří; Hájek, Tomáš; Svec, Frantisek

2017-04-01

The duration of the hypercrosslinking reaction has been used to control the extent of small pores formation in polymer-based monolithic stationary phases. Segments of five columns hypercrosslinked for 30-360 min were coupled via zero-volume unions to prepare columns with segmented porosity gradients. The steepness of the porosity gradient affected column efficiency, mass transfer resistance, and separation of both small-molecule alkylbenzenes and high-molar-mass polystyrene standards. In addition, the segmented column with the steepest porosity gradient was prepared as a single column with a continuous porosity gradient. The steepness of porosity gradient in this type column was tuned. Compared to a completely hypercrosslinked column, the column with the shallower gradient produced comparable size-exclusion separation of polystyrene standards but allowed higher column permeability. The completely hypercrosslinked column and the column with porosity gradient were successfully coupled in online two-dimensional liquid chromatography of polymers. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Polyether ether ketone encased monolith frits made of polyether ether ketone tubing with a 0.25 mm opening resulting in an improved separation performance in liquid chromatography.

PubMed

Park, Sin Young; Cheong, Won Jo

2016-05-01

Tiny polyether ether ketone encased monolith frits have been prepared by modified catalytic sulfonation of the inner surface of polyether ether tubing (1.6 mm od, 0.25 mm id) followed by modified formation of organic monolith and cutting of the tubing into slices. The frit was placed below the central hole of the column outlet union and supported by a combination of a silica capillary (0.365 mm od, 0.05 mm id) and a polyether ether ketone sleeve (1.6 mm od, 0.38 mm id) tightened with a nut and a ferrule when the column was packed to prevent sinking of the frit element into the union hole (0.25 mm opening) otherwise. The column packed this way with the frits investigated in this study has shown better separation performance owing to the reduced frit volume in comparison to the column packed with a commercial stainless-steel screen frit. This study establishes the strategy of disposable microcolumns in which cheap disposable frits are used whenever the column is re-packed to yield columns of even better chromatographic performance than the columns with commercial frits. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Acylhydrazone bond dynamic covalent polymer gel monolithic column online coupling to high-performance liquid chromatography for analysis of sulfonamides and fluorescent whitening agents in food.

PubMed

Zhang, Chengjiang; Luo, Xialin; Wei, Tianfu; Hu, Yufei; Li, Gongke; Zhang, Zhuomin

2017-10-13

A new dynamic covalent polymer (DCP) gel was well designed and constructed based on imine chemistry. Polycondensation of 4,4'-biphenyldicarboxaldehyde and 1,3,5-benzenetricarbohydrazide via Schiff-base reaction resulted in an acylhydrazone bond gel (AB-gel) DCP. AB-gel DCP had three-dimensional network of interconnected nanoparticles with hierarchically porous structure. AB-gel DCP was successfully fabricated as a monolithic column by an in-situ chemical bonding method for online enrichment and separation purpose with excellent permeability. AB-gel DCP based monolithic column showed remarkable adsorption affinity towards target analytes including sulfonamides (SAs) and fluorescent whitening agents (FWAs) due to its strong π-π affinity, hydrophobic effect and hydrogen bonding interaction. Then, AB-gel DCP based monolithic column was applied for online separation and analysis of trace SAs and FWAs in food samples coupled with high-performance liquid chromatography (HPLC). Sulfathiazole (ST) and sulfadimidine (SM2) in one positive weever sample were actually found and determined with concentrations of 273.8 and 286.3μg/kg, respectively. 2,5-Bis(5-tert-butyl-2-benzoxazolyl) thiophene (FWA184) was actually quantified in one tea infusion sample with the concentration of 268.5ng/L. The spiked experiments suggested the good recoveries in range of 74.5-110% for SAs in weever and shrimp samples with relative standard deviations (RSDs) less than 9.7% and in range of 74.0-113% for FWAs in milk and tea infusion samples with RSDs less than 9.0%. AB-gel DCP monolithic column was proved to be a promising sample preparation medium for online separation and analysis of trace analytes in food samples with complex matrices. Copyright © 2017 Elsevier B.V. All rights reserved.

Analysis of bovine milk caseins on organic monolithic columns: an integrated capillary liquid chromatography-high resolution mass spectrometry approach for the study of time-dependent casein degradation.

PubMed

Pierri, Giuseppe; Kotoni, Dorina; Simone, Patrizia; Villani, Claudio; Pepe, Giacomo; Campiglia, Pietro; Dugo, Paola; Gasparrini, Francesco

2013-10-25

Casein proteins constitute approximately 80% of the proteins present in bovine milk and account for many of its nutritional and technological properties. The analysis of the casein fraction in commercially available pasteurized milk and the study of its time-dependent degradation is of considerable interest in the agro-food industry. Here we present new analytical methods for the study of caseins in fresh and expired bovine milk, based on the use of lab-made capillary organic monolithic columns. An integrated capillary high performance liquid chromatography and high-resolution mass spectrometry (Cap-LC-HRMS) approach was developed, exploiting the excellent resolution, permeability and biocompatibility of organic monoliths, which is easily adaptable to the analysis of intact proteins. The resolution obtained on the lab-made Protein-Cap-RP-Lauryl-γ-Monolithic column (270 mm × 0.250 mm length × internal diameter, L × I.D.) in the analysis of commercial standard caseins (αS-CN, β-CN and κ-CN) through Cap-HPLC-UV was compared to the one observe using two packed capillary C4 columns, the ACE C4 (3 μm, 150 mm × 0.300 mm, L × I.D.) and the Jupiter C4 column (5 μm, 150 mm × 0.300 mm, L × I.D.). Thanks to the higher resolution observed, the monolithic capillary column was chosen for the successive degradation studies of casein fractions extracted from bovine milk 1-4 weeks after expiry date. The comparison of the UV chromatographic profiles of skim, semi-skim and whole milk showed a major stability of whole milk towards time-dependent degradation of caseins, which was further sustained by high-resolution analysis on a 50-cm long monolithic column using a 120-min time gradient. Contemporarily, the exact monoisotopic and average molecular masses of intact αS-CN and β-CN protein standards were obtained through high resolution mass spectrometry and used for casein identification in Cap-LC-HRMS analysis. Finally, the proteolytic degradation of β-CN in skim milk and the contemporary formation of low-molecular-weight proteose-peptones (PP) with exact monoisotopic Mr between 9444.0989 Da and 14098.9861 Da was confirmed through the deconvolution of high resolution mass spectra and literature data. Copyright © 2013 Elsevier B.V. All rights reserved.

1.3-microm optically-pumped semiconductor disk laser by wafer fusion.

PubMed

Lyytikäinen, Jari; Rautiainen, Jussi; Toikkanen, Lauri; Sirbu, Alexei; Mereuta, Alexandru; Caliman, Andrei; Kapon, Eli; Okhotnikov, Oleg G

2009-05-25

We report a wafer-fused high power optically-pumped semiconductor disk laser operating at 1.3 microm. An InP-based active medium was fused with a GaAs/AlGaAs distributed Bragg reflector, resulting in an integrated monolithic gain mirror. Over 2.7 W of output power, obtained at temperature of 15 degrees C, represents the best achievement reported to date for this type of lasers. The results reveal an essential advantage of the wafer fusing technique over both monolithically grown AlGaInAs/GaInAsP- and GaInNAs-based structures.

A novel mixed phospholipid functionalized monolithic column for early screening of drug induced phospholipidosis risk.

PubMed

Zhao, XiangLong; Chen, WeiJia; Liu, ZhengHua; Guo, JiaLiang; Zhou, ZhengYin; Crommen, Jacques; Moaddel, Ruin; Jiang, ZhengJin

2014-11-07

Drug-induced phospholipidosis (PLD) is characterized by the excessive accumulation of phospholipids, resulting in multilamellar vesicle structure within lysosomes. In the present study, a novel mixed phospholipid functionalized monolithic column was developed for the first time through a facile one-step co-polymerization approach. The phospholipid composition of the monolith can be adjusted quantitatively and accurately to mimic the mixed phospholipid environment of different biomembranes on a solid matrix. The mixed phospholipid functionalized monolith as a promising immobilized artificial membrane technique was used to study drug-phospholipid interaction. Scanning electron microscopy, elemental analysis, FT-IR spectra, ζ-potential analysis and micro-HPLC were carried out to characterize the physicochemical properties and separation performance of the monolith. Mechanism studies revealed that both hydrophobic and electrostatic interactions play an important role in the retention of analytes. The ratio of their contributions to retention can be easily manipulated by adjusting the composition of the mixed phospholipids, in order to better mimic the interaction between drugs and cell membrane. The obtained mixed phospholipid functionalized monolithic columns were applied to the screening of drug-induced PLD potency. Data from 79 drugs on the market demonstrated that the chromatographic hydrophobicity index referring to the mixed phospholipid functionalized monolith at pH 7.4 (CHI IAM7.4) for the selected drugs were highly correlated with the drug-induced PLD potency data obtained from other in vivo or in vitro assays. Moreover, the effect of the acidic phospholipid phosphatidylserine proportion on prediction accuracy was also investigated. The monolith containing 20% phosphatidylserine and 80% phosphatidylcholine exhibited the best prediction ability for the drug-induced PLD potency of the tested compounds. This research has led to the successful development of a novel and facile approach to prepare a mixed phospholipids functionalized monolith, which offers a reliable, cost-effective and high-throughput screening tool for early prediction of the PLD potency of drug candidates. Copyright © 2014 Elsevier B.V. All rights reserved.

Applicability of multisyringe chromatography coupled to on-line solid-phase extraction to the simultaneous determination of dicamba, 2,4-D, and atrazine.

PubMed

Chávez-Moreno, C A; Guzmán-Mar, J L; Hinojosa-Reyes, L; Hernández-Ramírez, A; Ferrer, L; Cerdà, V

2012-07-01

Simultaneous determination of three herbicides (dicamba, 2,4-D, and atrazine) has been achieved by on-line solid-phase extraction (SPE) coupled to multisyringe chromatography (MSC) with UV detection. The preconcentration conditions were optimized; a preconcentration flow rate of 0.5 mL min(-1) and elution at 0.8 mL min(-1) were the optimum conditions. A C(18) (8 mm i.d.) membrane extraction disk conditioned with 0.3 mol L(-1) HCl in 0.5% MeOH was used. A 3-mL sample was preconcentrated, then eluted with 0.43 mL 40:60 water-MeOH. A C(18) monolithic column (25 mm × 4.6 mm) was used for chromatographic separation. Separation of the three compounds was achieved in 10 min by use of 0.01% aqueous acetic acid-MeOH (60:40) as mobile phase at a flow rate of 0.8 mL min(-1). The limits of detection (LOD) were 13, 57, and 22 μg L(-1) for dicamba, 2,4-D, and atrazine, respectively. The sampling frequency was three analyses per hour, and each analysis consumed only 7.3 mL solvent. The method was applied to spiked water samples, and recovery between 85 and 112% was obtained. Recovery was significantly better than in the conventional HPLC-UV method. These results indicated the reliability and accuracy of this flow-based method. This is the first time this family of herbicides has been simultaneously analyzed by on-line SPE-MSC using a monolithic column.

Affinity monolith-integrated poly(methyl methacrylate) microchips for on-line protein extraction and capillary electrophoresis.

PubMed

Sun, Xiuhua; Yang, Weichun; Pan, Tao; Woolley, Adam T

2008-07-01

Immunoaffinity monolith pretreatment columns have been coupled with capillary electrophoresis separation in poly(methyl methacrylate) (PMMA) microchips. Microdevices were designed with eight reservoirs to enable the electrically controlled transport of selected analytes and solutions to carry out integrated immunoaffinity extraction and electrophoretic separation. The PMMA microdevices were fabricated reproducibly and with high fidelity by solvent imprinting and thermal bonding methods. Monoliths with epoxy groups for antibody immobilization were prepared by direct in situ photopolymerization of glycidyl methacrylate and ethylene glycol dimethacrylate in a porogenic solvent consisting of 70% 1-dodecanol and 30% cyclohexanol. Antifluorescein isothiocyanate was utilized as a model affinity group in the monoliths, and the immobilization process was optimized. A mean elution efficiency of 92% was achieved for the monolith-based extraction of fluorescein isothiocyanate (FITC)-tagged human serum albumin. FITC-tagged proteins were purified from a contaminant protein and then separated electrophoretically using these devices. The developed immunoaffinity column/capillary electrophoresis microdevices show great promise for combining sample pretreatment and separation in biomolecular analysis.

Affinity Monolith-Integrated Poly(methyl Methacrylate) Microchips for On-Line Protein Extraction and Capillary Electrophoresis

PubMed Central

Sun, Xiuhua; Yang, Weichun; Pan, Tao; Woolley, Adam T.

2008-01-01

Immunoaffinity monolith pretreatment columns have been coupled with capillary electrophoresis separation in poly(methyl methacrylate) (PMMA) microchips. Microdevices were designed with 8 reservoirs to enable the electrically controlled transport of selected analytes and solutions to carry out integrated immunoaffinity extraction and electrophoretic separation. The PMMA microdevices were fabricated reproducibly and with high fidelity by solvent imprinting and thermal bonding methods. Monoliths with epoxy groups for antibody immobilization were prepared by direct in-situ photopolymerization of glycidyl methacrylate and ethylene dimethacrylate in a porogenic solvent consisting of 70% dodecanol and 30% hexanol. Anti-fluorescein isothiocyanate (FITC) was utilized as a model affinity group in the monoliths, and the immobilization process was optimized. A mean elution efficiency of 92% was achieved for the monolith-based extraction of FITC-tagged human serum albumin. FITC-tagged proteins were purified from a contaminant protein and then separated electrophoretically using these devices. The developed immunoaffinity column/capillary electrophoresis microdevices show great promise for combining sample pretreatment and separation in biomolecular analysis. PMID:18479142

Chip-based molecularly imprinted monolithic capillary array columns coated GO/SiO2 for selective extraction and sensitive determination of rhodamine B in chili powder.

PubMed

Zhai, Haiyun; Huang, Lu; Chen, Zuanguang; Su, Zihao; Yuan, Kaisong; Liang, Guohuan; Pan, Yufang

2017-01-01

A novel solid-phase extraction chip embedded with array columns of molecularly imprinted polymer-coated silanized graphene oxide (GO/SiO2-MISPE) was established to detect trace rhodamine B (RB) in chili powder. GO/SiO2-MISPE monolithic columns for RB detection were prepared by optimizing the supporting substrate, template, and polymerizing monomer under mild water bath conditions. Adsorption capacity and specificity, which are critical properties for the application of the GO/SiO2-MISPE monolithic column, were investigated. GO/SiO2-MIP was examined by scanning electron microscopy (SEM) and Fourier transform-infrared spectroscopy. The recovery and the intraday and interday relative standard deviations for RB ranged from 83.7% to 88.4% and 2.5% to 4.0% and the enrichment factors were higher than 110-fold. The chip-based array columns effectively eliminated impurities in chili powder, indicating that the chip-based GO/SiO2-MISPE method was reliable for RB detection in food samples using high-performance liquid chromatography. Accordingly, this method has direct applications for monitoring potentially harmful dyes in processed food. Copyright © 2016 Elsevier Ltd. All rights reserved.

In situ synthesis of metal-organic frameworks in a porous polymer monolith as the stationary phase for capillary liquid chromatography.

PubMed

Yang, Shengchao; Ye, Fanggui; Zhang, Cong; Shen, Shufen; Zhao, Shulin

2015-04-21

In this study, HKUST-1 was synthesized in situ on the porous polymer monolith as the stationary phase for capillary liquid chromatography (cLC). The unique carboxyl functionalized poly(methacrylic acid-co-ethylene dimethacrylate) (poly(MAA-co-EDMA)) monolith was used as a support to directly grow HKUST-1 by a controlled layer-by-layer self-assembly strategy. X-ray diffraction, scanning electron microscopy, energy dispersive X-ray spectrometry, and Fourier transform infrared spectroscopy of the resulting HKUST-1-poly(MAA-co-EDMA) monoliths indicated that HKUST-1 was successfully grafted onto the pore surface of the poly(MAA-co-EDMA) monolith. The column performance of HKUST-1-poly(MAA-co-EDMA) monoliths for the separation of various small molecules, such as benzenediols, xylenes, ethylbenzenes, and styrenes, was evaluated. The chromatographic performance was found to improve with increasing HKUST-1 density, and the column efficiencies and resolutions of HKUST-1-poly(MAA-co-EDMA) monoliths were 18 320-19 890 plates m(-1) and 1.62-6.42, respectively, for benzenediols. The HKUST-1-poly(MAA-co-EDMA) monolith displayed enhanced resolution for the separation of positional isomers when compared to the traditional C18 and HKUST-1 incorporated polymer monoliths. Hydrophobic, π-π, and hydrogen bonding interactions within the HKUST-1-poly(MAA-co-EDMA) monolith were observed in the separation of small molecules. The results showed that the HKUST-1-poly(MAA-co-EDMA) monoliths are promising stationary phases for cLC.

Fiber-based monolithic columns for liquid chromatography.

PubMed

Ladisch, Michael; Zhang, Leyu

2016-10-01

Fiber-based monoliths for use in liquid chromatographic separations are defined by columns packed with aligned fibers, woven matrices, or contiguous fiber structures capable of achieving rapid separations of proteins, macromolecules, and low molecular weight components. A common denominator and motivating driver for this approach, first initiated 25 years ago, was reducing the cost of bioseparations in a manner that also reduced residence time of retained components while achieving a high ratio of mass to momentum transfer. This type of medium, when packed into a liquid chromatography column, minimized the fraction of stagnant liquid and resulted in a constant plate height for non-adsorbing species. The uncoupling of dispersion from eluent flow rate enabled the surface chemistry of the stationary phase to be considered separately from fluid transport phenomena and pointed to new ways to apply chemistry for the engineering of rapid bioseparations. This paper addresses developments and current research on fiber-based monoliths and explains how the various forms of this type of chromatographic stationary phase have potential to provide new tools for analytical and preparative scale separations. The different stationary phases are discussed, and a model that captures the observed constant plate height as a function of mobile phase velocity is reviewed. Methods that enable hydrodynamically stable fiber columns to be packed and operated over a range of mobile phase flow rates, together with the development of new fiber chemistries, are shown to provide columns that extend the versatility of liquid chromatography using monoliths, particularly at the preparative scale. Graphical Abstract Schematic representation of a sample mixture being separated by a rolled-stationary phase column, resulting separated peaks shown in the chromatogram.

Effect of thickness and surface modifications on flexural strength of monolithic zirconia.

PubMed

Ozer, Fusun; Naden, Andrew; Turp, Volkan; Mante, Francis; Sen, Deniz; Blatz, Markus B

2017-10-14

A recommended minimum thickness for monolithic zirconia restorations has not been reported. Assessing a proper thickness that has the necessary load-bearing capacity but also conserves dental hard tissues is essential. The purpose of this in vitro study was to evaluate the effect of thickness and surface modifications on monolithic zirconia after simulated masticatory stresses. Monolithic zirconia disks (10 mm in diameter) were fabricated with 1.3 mm and 0.8 mm thicknesses. For each thickness, 21 disks were fabricated. The specimens of each group were further divided into 3 subgroups (n=7) according to the surface treatments applied: untreated (control), airborne-particle abrasion with 50-μm Al 2 O 3 particles at a pressure of 400 kPa at 10 mm, and grinding with a diamond rotary instrument followed by polishing. The biaxial flexure strength was determined by using a piston-on-3-balls technique in a universal testing machine. Flexural loading was applied with a 1.4-mm diameter steel cylinder, centered on the disk, at a crosshead speed of 0.5 mm/min until fracture occurred. X-ray diffraction (XRD) and scanning electron microscopy (SEM) analyses were performed. The data were statistically analyzed with 2-way ANOVA, Tamhane T2, 1-way ANOVA, and Student t tests (α=.05). The 1.3-mm specimens had significantly higher flexural strength than the 0.8-mm specimens (P<.05). Airborne-particle abrasion significantly increased the flexural strength (P<.05). Grinding and polishing did not affect the flexural strength of the specimens (P>.05). The mean flexural strength of 0.8-mm and 1.3-mm thick monolithic zirconia was greater than reported masticatory forces. Airborne-particle abrasion increased the flexural strength of monolithic zirconia. Grinding did not affect flexural strength if subsequently polished. Copyright © 2017 Editorial Council for the Journal of Prosthetic Dentistry. Published by Elsevier Inc. All rights reserved.

Incorporation of metal-organic framework HKUST-1 into porous polymer monolithic capillary columns to enhance the chromatographic separation of small molecules.

PubMed

Yang, Shengchao; Ye, Fanggui; Lv, Qinghui; Zhang, Cong; Shen, Shufen; Zhao, Shulin

2014-09-19

Metal-organic framework (MOF) HKUST-1 nanoparticles have been incorporated into poly(glycidyl methacrylate-co-ethylene dimethacrylate) (HKUST-1-poly(GMA-co-EDMA)) monoliths to afford stationary phases with enhanced chromatographic performance of small molecules in the reversed phase capillary liquid chromatography. The effect of HKUST-1 nanoparticles in the polymerization mixture on the performance of the monolithic column was explored in detail. While the bare poly(GMA-co-EDMA) monolith exhibited poor resolution (Rs<1.0) and low efficiency (800-16,300plates/m), addition of a small amount of HKUST-1 nanoparticles to the polymerization mixture provide high increased resolution (Rs≥1.3) and high efficiency ranged from 16,300 to 44,300plates/m. Chromatographic performance of HKUST-1-poly(GMA-co-EDMA) monolith was demonstrated by separation of various analytes including polycyclic aromatic hydrocarbons, ethylbenzene and styrene, phenols and aromatic acids using a binary polar mobile phase (CH3CN/H2O). The HKUST-1-poly(GMA-co-EDMA) monolith displayed enhanced hydrophobic and π-π interaction characteristics in the reversed phase separation of test analytes compared to the bare poly(GMA-co-EDMA) monolith. The experiment results showed that HKUST-1-poly(GMA-co-EDMA) monoliths are an alternative to enhance the chromatographic separation of small molecules. Copyright © 2014 Elsevier B.V. All rights reserved.

In situ polymerization of monolith based on poly(Triallyl Isocyanurate-co-trimethylolpropane triacrylate) and its application in high-performance liquid chromatography.

PubMed

Zhong, Jing; Bai, Ligai; Qin, Junxiao; Wang, Jiafei; Hao, Mengbei; Yang, Gengliang

2015-04-01

A novel organic monolithic stationary phase was prepared for high-performance liquid chromatography (HPLC) by in situ copolymerization. In which, triallyl isocyanurate (TAIC) and trimethylolpropane triacrylate (TMPTA) in a binary porogenic solvent consisting of polyethylene glycol 200 and 1, 2-propanediol were used. The resultant monoliths with different column properties (e.g., morphology and pressure) were optimized by adjusting the ratio of TMPTA/TAIC and the composition of porogenic solvent. The resulting poly(TAIC-co-TMPTA) monolith showed a relatively homogeneous structure, good permeability and mechanical stability. The chemical group of the monolith was assayed by the infrared spectra method, the morphology of monolithic material was studied by scanning electron microscopy and the pore size distribution was determined by a mercury porosimeter. A series of small molecules were used to evaluate the column performance in terms of hydrophobic mode. At an optimized flow rate of 1.0 mL min(-1), the theoretical plate number of analyte was >15,000 plates m(-1). These applications demonstrated that the monoliths could be successfully used as the stationary phase in conjunction with HPLC to separate small molecules from the mixture. © The Author 2014. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Radial distribution of the contributions to band broadening of a silica-based semi-preparative monolithic column.

PubMed

Abia, Jude A; Mriziq, Khaled S; Guiochon, Georges A

2009-04-01

Using an on-column local electrochemical microdetector operated in the amperometric mode, band elution profiles were recorded at different radial locations at the exit of a 10 mm id, 100 mm long silica-based monolithic column. HETP plots were then acquired at each of these locations, and all these results were fitted to the Knox equation. This provided a spatial distribution of the values of the eddy diffusion (A), the molecular diffusion (B), and the resistance to the kinetics of mass transfer (C) terms. Results obtained indicate that the wall region yields higher A values and smaller C values than the central core region. Significant radial fluctuations of these contributions to band broadening occur throughout the exit column cross-section. This phenomenon is due to the structural radial heterogeneity of the column.

A weak cation-exchange monolith as stationary phase for the separation of peptide diastereomers by CEC.

PubMed

Ludewig, Ronny; Nietzsche, Sandor; Scriba, Gerhard K E

2011-01-01

A CEC weak cation-exchange monolith has been prepared by in situ polymerization of acrylamide, methylenebisacrylamide and 4-acrylamidobutyric acid in a decanol-dimethylsulfoxide mixture as porogen. The columns were evaluated by SEM and characterized with regard to the separation of diastereomers and α/β-isomers of aspartyl peptides. Column preparation was reproducible as evidenced by comparison of the analyte retention times of several columns prepared simultaneously. Analyte separation was achieved using mobile phases consisting of acidic phosphate buffer and ACN. Under these conditions the peptides migrated due to their electrophoretic mobility but the EOF also contributed as driving force as a function of the pH of the mobile phase due to increasing dissociation of the carboxyl groups of the polymer. Raising the pH of the mobile phase also resulted in deprotonation of the peptides reducing analyte mobility. Due to these mechanisms each pair of diastereomeric peptides displayed the highest resolution at a different pH of the buffer component of the mobile phase. Comparing the weak-cation exchange monolith to an RP monolith and a strong cation-exchange monolith different elution order of some peptide diastereomers was observed, clearly illustrating that interactions with the stationary phase contribute to the CEC separations. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

In-situ functionalized monolithic polysiloxane-polymethacrylate composite materials from polythiol-ene double click reaction in capillary column format for enantioselective nano-high-performance liquid chromatography.

PubMed

Wolter, Marc; Lämmerhofer, Michael

2017-05-12

This work reports on the proof-of-principle of preparation of novel one step in-situ functionalized monolithic polysiloxane-polymethacrylate composite materials in capillary columns for enantioselective nano-HPLC using a thiol-ene click reaction. Quinine carbamate as functional monomer and ethylene dimethacrylate as crosslinker were both used as ene components in a thermally initiated double click-type polymerization reaction with poly(3-mercaptopropyl)methylsiloxane as thiol component in presence of 1-propanol as porogenic solvent. Elemental analysis and on-capillary fluorescence measurement proved the successful incorporation of the functional chiral monomer into the polymer. Scanning electron microscopy images revealed a macroporous polymer morphology which is typical for a nucleation and growth mechanism of pore formation. The individual microglobules appear relatively spherical and smooth indicating a non-porous nature. Nano-HPLC experiments of the chiral monolithic capillary column provided successful enantiomer separation of N-3,5-dinitrobenzoylleucine as test compound in polar organic elution mode clearly documenting the successful implementation of the proposed concept towards new functionalized monolithic composite materials. Copyright © 2017 Elsevier B.V. All rights reserved.

Determination of imidazole derivatives by micellar electrokinetic chromatography combined with solid-phase microextraction using activated carbon-polymer monolith as adsorbent.

PubMed

Shih, Yung-Han; Lirio, Stephen; Li, Chih-Keng; Liu, Wan-Ling; Huang, Hsi-Ya

2016-01-08

In this study, an effective method for the separation of imidazole derivatives 2-methylimidazole (2-MEI), 4- methylimidazole (4-MEI) and 2-acetyl-4-tetrahydroxybutylimidazole (THI) in caramel colors using cation-selective exhaustive injection and sweeping micellar electrokinetic chromatography (CSEI-sweeping-MEKC) was developed. The limits of detection (LOD) and quantitation (LOQ) for the CSEI-sweeping-MEKC method were in the range of 4.3-80μgL(-1) and 14-270μgL(-1), respectively. Meanwhile, a rapid fabrication activated carbon-polymer (AC-polymer) monolithic column as adsorbent for solid-phase microextraction (SPME) of imidazole colors was developed. Under the optimized SPME condition, the extraction recoveries for intra-day, inter-day and column-to-column were in the range of 84.5-95.1% (<6.3% RSDs), 85.6-96.1% (<4.9% RSDs), and 81.3-96.1% (<7.1% RSDs), respectively. The LODs and LOQs of AC-polymer monolithic column combined with CSEI-sweeping-MEKC method were in the range of 33.4-60.4μgL(-1) and 111.7-201.2μgL(-1), respectively. The use of AC-polymer as SPME adsorbent demonstrated the reduction of matrix effect in food samples such as soft drink and alcoholic beverage thereby benefiting successful determination of trace-level caramel colors residues using CSEI-sweeping-MEKC method. The developed AC-polymer monolithic column can be reused for more than 30 times without any significant loss in the extraction recovery for imidazole derivatives. Copyright © 2015 Elsevier B.V. All rights reserved.

Experimental and numerical validation of the effective medium theory for the B-term band broadening in 1st and 2nd generation monolithic silica columns.

PubMed

Deridder, Sander; Vanmessen, Alison; Nakanishi, Kazuki; Desmet, Gert; Cabooter, Deirdre

2014-07-18

Effective medium theory (EMT) expressions for the B-term band broadening in monolithic silica columns are presented at the whole-column as well as at the mesoporous skeleton level. Given the bi-continuous nature of the monolithic medium, regular as well as inverse formulations of the EMT-expressions have been established. The established expressions were validated by applying them to a set of experimental effective diffusion (Deff)-data obtained via peak parking on a number of 1st and 2nd generation monolithic silica columns, as well as to a set of numerical diffusion simulations in a simplified monolithic column representation (tetrahedral skeleton model) with different external porosities and internal diffusion coefficients. The numerically simulated diffusion data can be very closely represented over a very broad range of zone retention factors (up to k″=80) using the established EMT-expressions, especially when using the inverse variant. The expressions also allow representing the experimentally measured effective diffusion data very closely. The measured Deff/Dmol-values were found to decrease significantly with increasing retention factor, in general going from about Deff/Dmol=0.55 to 0.65 at low k″ (k″≅1.5-3.8) to Deff/Dmol=0.25 at very high k″ (k″≅40-80). These values are significantly larger than observed in fully-porous and core-shell particles. The intra-skeleton diffusion coefficient (Dpz) was typically found to be of the order of Dpz/Dmol=0.4, compared to Dpz/Dmol=0.2-0.35 observed in most particle-based columns. These higher Dpz/Dmol values are the cause of the higher Deff/Dmol values observed. In addition, it also appears that the higher internal diffusion is linked to the higher porosity of the mesoporous skeleton that has a relatively open structure with relatively wide pores. The observed (weak) relation between Dpz/Dmol and the zone retention factor appears to be in good agreement with that predicted when applying the regular variant of the EMT-expression directly to the mesoporous skeleton level. Copyright © 2014 Elsevier B.V. All rights reserved.

[Rapid determination of trace iodate using monolithic column ion-pair chromatography coupled with direct conductivity detection].

PubMed

Liu, Yuzhen; Yu, Hong; Li, Siwen

2011-10-01

A method was developed on a monolithic column for the fast determination of trace iodate (IO(3)- ) by ion-pair chromatography with direct conductivity detection. The analytes were separated using a mobile phase of tetrabutylammonium hydroxide (TBA)-phthalic acid-acetonitrile on a reversed-phase silica-based monolithic column. The effects of eluent, flow rate and column temperature on the retention of iodate were investigated. The optimized chromatographic conditions for the determination of the anion were as follows: 0. 25 mmol/L TBA-0. 18 mmol/L phthalic acid-3% acetonitrile (pH 5.5) as mobile phase, a flow rate of 4.0 mL/min and a column temperature of 30 degrees C. Under the optimal conditions, retention time of iodate was less than 0. 5 min and the baseline separation of iodate was achieved without any interference by other anions (Cl-, NO , SO4(2)-, I- ). The detection limit (S/N= 3) was 0.36 mg/L for IO(3)- . Relative standard deviation (RSD, n = 5) of chromatographic peak area and retention time were 0. 35% and 0. 28%, respectively. The proposed method was applied to the determination of trace iodate in iodized medicine. The spiked recovery of iodate was 96. 4%. The method is rapid, simple, accurate, reliable, and practical.

Preparation and Characterization of a Polymeric Monolithic Column for Use in High-Performance Liquid Chromatography (HPLC)

ERIC Educational Resources Information Center

Bindis, Michael P.; Bretz, Stacey Lowery; Danielson, Neil D.

2011-01-01

The high-performance liquid chromatography (HPLC) experiment, most often done in the undergraduate analytical instrumentation laboratory course, generally illustrates reversed-phase chromatography using a commercial C[subscript]18 silica column. To avoid the expense of periodic column replacement and introduce a choice of columns with different…

Molecularly imprinted coated graphene oxide solid-phase extraction monolithic capillary column for selective extraction and sensitive determination of phloxine B in coffee bean.

PubMed

Zhai, Haiyun; Su, Zihao; Chen, Zuanguang; Liu, Zhenping; Yuan, Kaisong; Huang, Lu

2015-03-20

A method was developed to sensitively determine phloxine B in coffee bean by molecularly imprinted polymers (MIPs) coated graphene oxide (GO) solid-phase extraction (GO-MISPE) coupled with high-performance liquid chromatography and laser-induced fluorescence detection (HPLC-LIF). The GO-MISPE capillary monolithic column was prepared by water-bath in situ polymerization, using GO as supporting material, phloxine B, methacrylic acid (MAA), and ethylene dimethacrylate (EDMA) as template, functional monomer, and cross-linker, respectively. The properties of the homemade GO-MISPE capillary monolithic column, including capacity and specificity, were investigated under optimized conditions. The GO-MIPs were characterized by scanning electron microscopy (SEM) and Fourier transform-infrared spectroscopy (FT-IR). The mean recoveries of phloxine B in coffee bean ranged from 89.5% to 91.4% and the intra-day and inter-day relative standard deviation (RSD) values all ranged from 3.6% to 4.7%. Good linearity was obtained over 0.001-2.0 μg mL(-1) (r=0.9995) with the detection limit (S/N=3) of 0.075 ng mL(-1). Under the selected conditions, enrichment factors of over 90-fold were obtained and extraction on the monolithic column effectively cleaned up the coffee bean matrix. The results demonstrated that the proposed GO-MISPE HPLC-LIF method can be applied to sensitively determine phloxine B in coffee bean. Copyright © 2015 Elsevier B.V. All rights reserved.

Chiral recognition ability of an (S)-naproxen- imprinted monolith by capillary electrochromatography.

PubMed

Xu, Yan-Li; Liu, Zhao-Sheng; Wang, He-Fang; Yan, Chao; Gao, Ru-Yu

2005-02-01

The racemic naproxen was selectively recognized by capillary electrochromatography (CEC) on an (S)-naproxen-imprinted monolith, which was prepared by an in situ thermal-initiated polymerization. The recognition selectivity of a selected monolith strictly relied on the CEC conditions involved. The factors that influence the imprinting selectivity as well as the electroosmotic flow (EOF), including the applied voltage, organic solvent, salt concentration and pH value of the buffer, column temperature, and surfactant modifiers were systematically studied. Once the column was prepared, the experiment results showed that the successful chiral recognition was dependent on CEC variables. For example: the recognition could be observed in acetonitrile and ethanol electrolytes, while methanol and dimethyl sulfoxide (DMSO) electrolytes had no chiral recognition ability. The buffer with pH values of 2.6 or 3.0 at a higher salt concentration had chiral recognition ability. Column temperatures of 25-35 degrees C were optimal. Three surfactants, sodium dodecyl sulfate (SDS), cetyltrimethylammonium bromide (CTAB), and polyoxyethylene sorbitan monolaurate (Tween 20), can improve the recognition. Baseline resolution was obtained under optimized conditions and the column efficiency of the later eluent (S)-naproxen was 90 000 plates/m.

Facile preparation of a stable and functionalizable hybrid monolith via ring-opening polymerization for capillary liquid chromatography.

PubMed

Lin, Hui; Ou, Junjie; Tang, Shouwan; Zhang, Zhenbin; Dong, Jing; Liu, Zhongshan; Zou, Hanfa

2013-08-02

An organic-inorganic hybrid monolith was prepared by a single-step ring-opening polymerization of octaglycidyldimethylsilyl polyhedral oligomeric silsesquioxane (POSS) with poly(ethylenimine) (PEI). The obtained hybrid monoliths possessed high ordered 3D skeletal microstructure with dual retention mechanism that exhibits reversed-phase (RP) mechanism under polar mobile phase and hydrophilic-interaction liquid chromatography (HILIC) retention mechanism under less polar mobile phase. The high column efficiencies of 110,000N/m can be achieved for separation of alkylbenzenes in capillary reversed-phase liquid chromatography (cLC). Due to the robust property of hybrid monolith and the rich primary and secondary amino groups on its surface, the resulting hybrid monolith was easily modified with γ-gluconolactone and physically coated with cellulose tris(3,5-dimethylphenylcarbamate) (CDMPC), respectively. The former was successfully applied for HILIC separation of neutral, basic and acidic polar compounds as well as small peptides, and the latter for enantioseparation of racemates in cLC. The high column efficiencies were achieved in all of those separations. These results demonstrated that the hybrid monolith (POSS-PEI) possessed high stability and good surface tailorbility, potentially being applied for other research fields. Copyright © 2013 Elsevier B.V. All rights reserved.

Separation of alpha-, beta-, gamma-, delta-tocopherols and alpha-tocopherol acetate on a pentaerythritol diacrylate monostearate-ethylene dimethacrylate monolith by capillary electrochromatography.

PubMed

Chaisuwan, Patcharin; Nacapricha, Duangjai; Wilairat, Prapin; Jiang, Zhengjin; Smith, Norman W

2008-06-01

This work reports the first use of a monolith with method development for the separation of tocopherol (TOH) compounds by CEC with UV detection. A pentaerythritol diacrylate monostearate-ethylene dimethacrylate (PEDAS-EDMA) monolithic column has been investigated for an optimised condition to separate alpha-, beta-, gamma- and delta-TOHs, and alpha-tocopherol acetate (TAc). The PEDAS-EDMA monolith showed a remarkably good selectivity for separation of the TOH isomers including the beta- and gamma-isomers which are not easily separated by standard C8 or C18 particle-packed columns. Retention studies indicated that an RP mechanism was involved in the separation on the PEDAS-EDMA column, but polar interactions with the underlying ester and hydroxyl groups enhanced the separation of the problematic beta- and gamma-isomers. Separation of all the compounds was achieved within 25 min using 3:10:87 v/v/v 100 mM Tris buffer (pH 9.3)/methanol/ACN as the mobile phase. The method was successfully applied to a pharmaceutical sample with recoveries from 93 to 99%. Intraday and interday precisions (%RSD) for peak area and retention time were less than 2.3. LODs for all four TOHs and TAc were below 1 ppm.

3D printed titanium micro-bore columns containing polymer monoliths for reversed-phase liquid chromatography.

PubMed

Gupta, Vipul; Talebi, Mohammad; Deverell, Jeremy; Sandron, Sara; Nesterenko, Pavel N; Heery, Brendan; Thompson, Fletcher; Beirne, Stephen; Wallace, Gordon G; Paull, Brett

2016-03-03

The potential of 3D selective laser melting (SLM) technology to produce compact, temperature and pressure stable titanium alloy chromatographic columns is explored. A micro bore channel (0.9 mm I.D. × 600 mm long) was produced within a 5 × 30 × 30 mm titanium alloy (Ti-6Al-4V) cuboid, in form of a double handed spiral. A poly(butyl methacrylate-co-ethyleneglycoldimethacrylate) (BuMA-co-EDMA) monolithic stationary phase was thermally polymerised within the channel for application in reversed-phase high-performance liquid chromatography. The prepared monolithic column was applied to the liquid chromatographic separation of intact proteins and peptides. Peak capacities of 69-76 (for 6-8 proteins respectively) were observed during isothermal separation of proteins at 44 °C which were further increased to 73-77 using a thermal step gradient with programmed temperature from 60 °C to 35 °C using an in-house built direct-contact heater/cooler platform based upon matching sized Peltier thermoelectric modules. Rapid temperature gradients were possible due to direct-contact between the planar metal column and the Peltier module, and the high thermal conductivity of the titanium column as compared to a similar stainless steel printed column. The separation of peptides released from a digestion of E.coli was also achieved in less than 35 min with ca. 40 distinguishable peaks at 210 nm. Copyright © 2016 Elsevier B.V. All rights reserved.

Comparison of Positively and Negatively Charged Achiral Co-Monomers Added to Cyclodextrin Monolith: Improved Chiral Separations in Capillary Electrochromatography

PubMed Central

Lu, Yang; Shamsi, Shahab A.

2014-01-01

Cyclodextrins (CDs) and their derivatives have been one of the most popular and successful chiral additives used in electrokinetic chromatography because of the presence of multiple chiral centers, which leads to multiple chiral interactions. However, there has been relatively less published work on the use of CDs as monolithic media for capillary electrochromatography (CEC). The goal of this study was to show how the addition of achiral co-monomer to a polymerizable CD such as glycidyl methacrylate β-cyclodextrin (GMA/β-CD) can affect the enantioselective separations in monolithic CEC. To achieve this goal, polymeric monoliths columns were prepared by co-polymerizing GMA/β-CD with cationic or anionic achiral co-monomers [(2-acrylamido-2-methyl-1-propanesulfonic acid (AMPS) and vinyl benzyltrimethyl-ammonium (VBTA)] in the presence of conventional crosslinker (ethylene dimethacrylate) and ternary porogen system including butanediol, propanol and water. A total of 34 negatively charged compounds, 30 positively charged compounds and 33 neutral compounds were screened to compare the enantioresolution capability on the GMA/β-CD, GMA/β-CD-VBTA and GMA/β-CD-AMPS monolithic columns. PMID:24108813

A facile and efficient single-step approach for the fabrication of vancomycin functionalized polymer-based monolith as chiral stationary phase for nano-liquid chromatography.

PubMed

Xu, Dongsheng; Shao, Huikai; Luo, Rongying; Wang, Qiqin; Sánchez-López, Elena; Fanali, Salvatore; Marina, Maria Luisa; Jiang, Zhengjin

2018-07-06

A facile single-step preparation strategy for fabricating vancomycin functionalized organic polymer-based monolith within 100μm fused-silica capillary was developed. The synthetic chiral functional monomer, i.e 2-isocyanatoethyl methacrylate (ICNEML) derivative of vancomycin, was co-polymerized with the cross-linker ethylene dimethacrylate (EDMA) in the presence of methanol and dimethyl sulfoxide as the selected porogens. The co-polymerization conditions were systematically optimized in order to obtain satisfactory column performance. Adequate permeability, stability and column morphology were observed for the optimized poly(ICNEML-vancomycin-co-EDMA) monolith. A series of chiral drugs were evaluated on the monolith in either polar organic-phase or reversed-phase modes. After the optimization of separation conditions, baseline or partial enantioseparation were obtained for series of drugs including thalidomide, colchicine, carteolol, salbutamol, clenbuterol and several other β-blockers. The proposed single-step approach not only resulted in a vancomycin functionalized organic polymer-based monolith with acceptable performance, but also significantly simplified the preparation procedure by reducing time and labor. Copyright © 2018 Elsevier B.V. All rights reserved.

Comprehensive profiling of ribonucleosides modification by affinity zirconium oxide-silica composite monolithic column online solid-phase microextraction - Mass spectrometry analysis.

PubMed

Jiang, Han-Peng; Chu, Jie-Mei; Lan, Meng-Dan; Liu, Ping; Yang, Na; Zheng, Fang; Yuan, Bi-Feng; Feng, Yu-Qi

2016-09-02

More than 140 modified ribonucleosides have been identified in RNA. Determination of endogenous modified ribonucleosides in biological fluids may serve as non-invasive disease diagnostic strategy. However, detection of the modified ribonucleosides in biological fluids is challenging, especially for the low abundant modified ribonucleosides due to the serious matrix interferences of biological fluids. Here, we developed a facile preparation strategy and successfully synthesized zirconium oxide-silica (ZrO2/SiO2) composite capillary monolithic column that exhibited excellent performance for the selective enrichment of cis-diol-containing compounds. Compared with the boronate-based affinity monolith, the ZrO2/SiO2 monolith showed ∼2 orders of magnitude higher extraction capacity and can be used under physiological pH (pH 6.5-7.5). Using the prepared ZrO2/SiO2 composite monolith as the trapping column and reversed-phase C18 column as the analytical column, we further established an online solid-phase microextraction (SPME) in combination with liquid chromatography-mass spectrometry (online SPME-LC-MS/MS) analysis for the comprehensive profiling of ribonucleosides modification in human urine. Our results showed that 68 cis-diol-containing ribosylated compounds were identified in human urine, which is, to the best of our knowledge, the highest numbers of cis-diol-containing compounds were determined in a single analysis. It is worth noting that four modified ribonucleosides were discovered in the human urine for the first time. In addition, the quantification results from the pooled urine samples showed that compared to healthy controls, the contents of sixteen ribose conjugates in the urine of gastric cancer, eleven in esophagus cancer and seven in lymphoma increased more than two folds. Among these ribose conjugates, four ribose conjugates increased more than two folds in both gastric cancer and esophagus cancer; three ribose conjugates increased more than two folds in both gastric cancer and lymphoma; one ribose conjugate increased more than two folds in both esophagus cancer and lymphoma. The developed analytical method provides a good platform to study the modified ribonucleosides in human body fluids. Copyright © 2016 Elsevier B.V. All rights reserved.

Solid-phase microextraction of phthalate esters in water sample using different activated carbon-polymer monoliths as adsorbents.

PubMed

Lirio, Stephen; Fu, Chung-Wei; Lin, Jhih-Yun; Hsu, Meng-Ju; Huang, Hsi-Ya

2016-07-13

In this study, the application of different activated carbon-polymer (AC-polymer) monoliths as adsorbents for the solid-phase microextraction (SPME) of phthalate esters (PAEs) in water sample were investigated. The activated carbon (AC) was embedded in organic polymers, poly(butyl methacrylate-co-ethylene dimethacrylate) (poly(BMA-EDMA)) or poly(styrene-co-divinylbenzene) (poly(STY-DVB)), via a 5-min microwave-assisted or a 15-min water bath heating polymerization. Preliminary investigation on the performance of the native poly(BMA-EDMA) and poly(STY-DVB) demonstrated remarkable adsorption efficiencies for PAEs. However, due to the strong hydrophobic, π-π, and hydrogen bonding interactions between the analytes and polymers, low extraction recoveries were achieved. In contrast, the presence of AC in native polymers not only enhanced the adsorption efficiencies but also assisted the PAE desorption, especially for AC-poly(STY-DVB) with extraction recovery ranged of 76.2-99.3%. Under the optimized conditions, the extraction recoveries for intra-, inter-day and column-to-column were in the range of 76.5-100.8% (<3.7% RSDs), 77.2-97.6% (<5.6% RSDs) and 75.5-99.7% (<6.2% RSDs), respectively. The developed AC-poly(STY-DVB) monolithic column showed good mechanical stability, which can be reused for more than 30 extraction times without any significant loss in the extraction recoveries of PAEs. The AC-poly(STY-DVB) monolithic column was successfully applied in SPME of PAEs in water sample with extraction recovery ranged of 78.8%-104.6% (<5.5% RSDs). Copyright © 2016 Elsevier B.V. All rights reserved.

A monolithic column based on covalent cross-linked polymer gels for online extraction and analysis of trace aflatoxins in food sample.

PubMed

Wei, Tianfu; Chen, Zhengyi; Li, Gongke; Zhang, Zhuomin

2018-05-04

Aflatoxins are highly toxic mycotoxin contamination, which pose serious food safety incidents. It is very important to precisely and rapidly determine trace aflatoxins in food. In this study, we designed porous monolithic column based on covalent cross-linked polymer gels for online extraction and analysis of trace aflatoxins in food samples with complicated matrices coupled with high-performance liquid chromatography-ultraviolet detector (HPLC-UV). The prepared monolithic column showed excellent enrichment performance due to its good permeability, good reproducibility and long life span. The study of adsorption mechanism suggested that the excellent enrichment performance of this monolithic column was attributed to the multiple effect of π-π stacking interaction, hydrophobic effect and steric effect. When the online analytical method was applied for the determine of trace aflatoxins in real food samples, aflatoxins G 1 and aflatoxins B 1 could be actually found in one positive bean sauce sample and quantified to be 32.8 and 26.4 μg/kg, respectively. Aflatoxins G 1 in one bean sample could be also found and quantified to be 25.9 μg/kg. The low detection limits of the developed method were achieved in range of 0.08-0.2 μg/kg. And the recoveries for spiked samples were in range from 76.1 to 113% with RSDs of 1.1-9.6%. The developed method was proved to be a promising method for online enrichment and analysis of trace aflatoxins in complicated food samples. Copyright © 2018 Elsevier B.V. All rights reserved.

On-chip sample pretreatment using a porous polymer monolithic column for solid-phase microextraction and chemiluminescence determination of catechins in green tea.

PubMed

Lin, Ling; Chen, Hui; Wei, Huibin; Wang, Feng; Lin, Jin-Ming

2011-10-21

A porous polymer monolithic column for solid-phase microextraction and chemiluminescence detection was integrated into a simple microfluidic chip for the extraction and determination of catechins in green tea. The porous polymer was prepared by poly(glycidyl methacrylate-co-ethylene dimethacrylate) and modified with ethylenediamine. Catechins can be concentrated in the porous polymer monolithic column and react with potassium permanganate to give chemiluminescence. The microfluidic chip is reusable with high sensitivity and very low reagent consumption. The on-line preconcentration and detection can be realized without an elution step. The enrichment factor was calculated to be about 20 for catechins. The relative chemiluminescence intensity increased linearly with concentration of catechin from 5.0 × 10(-9) to 1.0 × 10(-6) M and the limit of detection was 1.0 × 10(-9) M. The proposed method was applied to determine catechin in green tea. The recoveries are from 90% to 110% which benefits the actual application for green tea samples.

MicroSPE-nanoLC-ESI-MS/MS Using 10-μm-i.d. Silica-Based Monolithic Columns for Proteomics

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

Luo, Quanzhou; Page, Jason S.; Tang, Keqi

2007-01-01

Silica-based monolithic narrow bore capillary columns (25 cm x 10 µm i.d.) with an integrated nanoESI emitter has been developed to provide high quality and robust microSPE-nanoLC-ESI-MS analyses. The integrated nanoESI emitter adds no dead volume to the LC separation, allowing stable electrospray performance to be obtained at flow rates of ~10 nL/min. In an initial application we identified 5510 unique peptides covering 1443 distinct Shewanella oneidensis proteins from a 300 ng tryptic digest sample in a single 4-h LC-MS/MS analysis using a linear ion trap MS (LTQ). We found the use of an integrated monolithic ESI emitter provided enhancedmore » resistance to clogging and good run-to-run reproducibility.« less

Analyses of sulfonamide antibiotics in meat samples by on-line concentration capillary electrochromatography-mass spectrometry.

PubMed

Cheng, Yi-Jie; Huang, Sing-Hao; Singco, Brenda; Huang, Hsi-Ya

2011-10-21

In this work, a series of poly(divinylbenzene-alkyl methacrylate) monolithic stationary phases, which were prepared by single step in situ polymerization of divinylbenzene and various alkyl methacrylates (butyl-, octyl-, lauryl- or stearyl methacrylate), were developed as separation columns of nine common sulfonamide antibiotics for capillary electrochromatography (CEC) coupled to mass spectrometry (MS). Results indicated that the sulfonamide's retention became weak with increased carbon chain length of alkyl methacrylate monomer (for example, t(R)=68 min and 21 min for butyl- and lauryl methacrylate, respectively). Among them, the poly(divinylbenzene-octyl methacrylate) (poly(DVB-OMA)) monolith was regarded as the optimal separation column as this provided better resolution within the shortest retention time. Moreover, the cross-sectional roughness of the monolithic column-end, that was used to couple to the ESI interface, strongly influenced the electrospray stability in the CEC-MS. Before the column was connected to the ESI-MS, a simple polishing was done to reduce the roughness of the column end that resulted to a great improvement in the signal stability. The relative standard deviations (RSDs) of the peak areas for the unpolished and polished ends of the poly(DVB-OMA) columns (n=5) were in the range of 46.1-60.2% and 8.9-16.4%, respectively. Furthermore, optimization of the mobile phase composition and the gradient elution strategy successfully determined the sulfonamide antibiotics in meat samples with as low as 10 μg/L level. Copyright © 2011 Elsevier B.V. All rights reserved.

Enrichment of Glycoproteins using Nano-scale Chelating Con A Monolithic Capillary Chromatography

PubMed Central

Feng, Shun; Yang, Na; Pennathur, Subramaniam; Goodison, Steve; Lubman, David M.

2009-01-01

Immobilized lectin chromatography can be employed for glycoprotein enrichment, but commonly used columns have limitations of yield and resolution. In order to improve efficiency and to make the technique applicable to minimal sample material, we have developed a nano-scale chelating Concanavalin A (Con A) monolithic capillary prepared using GMA-EDMA (glycidyl methacrylate–co-ethylene dimethacrylate) as polymeric support. Con A was immobilized on Cu(II)-charged iminodiacetic acid (IDA) regenerable sorbents by forming a IDA:Cu(II):Con A sandwich affinity structure that has high column capacity as well as stability. When compared with conventional Con A lectin chromatography, the monolithic capillary enabled the better reproducible detection of over double the number of unique N-glycoproteins in human urine samples. Utility for analysis of minimal biological samples was confirmed by the successful elucidation of glycoprotein profiles in mouse urine samples at the microliter scale. The improved efficiency of the nano-scale monolithic capillary will impact the analysis of glycoproteins in complex biological samples, especially where only limited material may be available. PMID:19366252

Reaction-Mediated Desorption of Macromolecules: Novel Phenomenon Enabling Simultaneous Reaction and Separation.

PubMed

Isakari, Yu; Kishi, Yuhi; Yoshimoto, Noriko; Yamamoto, Shuichi; Podgornik, Aleš

2018-02-02

Combining chemical reaction with separation offers several advantages. In this work possibility to induce spontaneous desorption of adsorbed macromolecules, once being PEGylated, through adjustment of the reagent composition is investigated. Bovine serum albumin (BSA) and activated oligonucleotide, 9T, are used as the test molecules and 20 kDa linear activated PEG is used for their PEGylation. BSA solid-phase PEGylation is performed on Q Sepharose HP. Distribution coefficient of BSA and PEG-BSA as a function of NaCl is determined using linear gradient elution (LGE) experiments and Yamamoto model. According to the distribution coefficient the selectivity between BSA and PEG - BSA of around 15 is adjusted by using NaCl. Spontaneous desorption of PEG - BSA is detected with no presence of BSA. However, due to a rather low selectivity, also desorption of BSA occurred at high elution volume. A similar procedure is applied for activated 9T oligonucleotide, this time using monolithic CIM QA disk monolithic column for adsorption. Selectivity of over 2000 is obtained by proper adjustment of PEG reagent composition. High selectivity enables spontaneous desorption of PEG-9T without any desorption of activated 9T. Both experiments demonstrates that reaction-mediated desorption of macromolecules is possible when the reaction conditions are properly tuned. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Methacrylate monolithic columns functionalized with epinephrine for capillary electrochromatography applications.

PubMed

Carrasco-Correa, Enrique Javier; Ramis-Ramos, Guillermo; Herrero-Martínez, José Manuel

2013-07-12

Epinephrine-bonded polymeric monoliths for capillary electrochromatography (CEC) were developed by nucleophilic substitution reaction of epoxide groups of poly(glycidyl-methacrylate-co-ethylenedimethacrylate) (poly(GMA-co-EDMA)) monoliths using epinephrine as nucleophilic reagent. The ring opening reaction under dynamic conditions was optimized. Successful chemical modification of the monolith surface was ascertained by in situ Raman spectroscopy characterization. In addition, the amount of epinephrine groups that was bound to the monolith surface was evaluated by oxidation of the catechol groups with Ce(IV), followed by spectrophotometric measurement of unreacted Ce(IV). About 9% of all theoretical epoxide groups of the parent monolith were bonded to epinephrine. The chromatographic behavior of the epinephrine-bonded monolith in CEC conditions was assessed with test mixtures of alkyl benzenes, aniline derivatives and substituted phenols. In comparison to the poly(GMA-co-EDMA) monoliths, the epinephrine-bonded monoliths exhibited a much higher retention and slight differences in selectivity. The epinephrine-bonded monolith was further modified by oxidation with a Ce(IV) solution and compared with the epinephrine-bonded monoliths. The resulting monolithic stationary phases were evaluated in terms of reproducibility, giving RSD values below 9% in the parameters investigated. Copyright © 2013 Elsevier B.V. All rights reserved.

Vinyl functionalized silica hybrid monolith-based trypsin microreactor for on line digestion and separation via thiol-ene "click" strategy.

PubMed

Chen, Yingzhuang; Wu, Minghuo; Wang, Keyi; Chen, Bo; Yao, Shouzhuo; Zou, Hanfa; Nie, Lihua

2011-11-04

A novel thiol-ene "click" strategy for the preparation of monolithic trypsin microreactor was proposed. The hybrid organic-inorganic monolithic capillary column with ene-functionality was fabricated by sol-gel process using tetramethoxysilane (TMOS) and γ-methacryloxypropyltrimethoxysilane (γ-MAPS) as precursors. The disulfide bonds of trypsin were reduced to form free thiol groups. Then the trypsin containing free thiol groups was attached on the γ-MAPS hybrid monolithic column with ene-functionality via thiol-ene click chemistry to form a trypsin microreactor. The activity of the trypsin microreactor was characterized by detecting the substrate (Nα-p-tosyl-L-arginine methyl ester hydrochloride, TAME) and the product (Nα-p-tosyl-L-arginine, TA) with on-line capillary zone electrophoresis. After investigating various synthesizing conditions, it was found that the microreactor with poly(N,N'-methylenebisacrylamide) as spacer can deliver the highest activity, yielding a rapid reaction rate. After repeatedly sampling and analyzing for 100 times, the monolithic trypsin microreactor still remained 87.5% of its initial activity. It was demonstrated that thiol-ene "click" strategy for the construction of enzyme microreactor is a promising method for the highly selective immobilization of proteins under mild conditions, especially enzymes with free thiol radicals. Copyright © 2011 Elsevier B.V. All rights reserved.

[Synchronous extraction and determination of phenoxy acid herbicides in water by on-line monolithic solid phase microextraction-high performance liquid chromatography].

PubMed

Wang, Jiabin; Wu, Fangling; Zhao, Qi

2015-08-01

A C18 monolithic capillary column was utilized as the solid phase microextraction column to construct an in-tube SPME-HPLC system which was used to simultaneously extract and detect five phenoxy acid herbicides, including 2,4-dichlorophenoxyacetic acid (2,4-D), 2- (2-chloro)-phenoxy propionic acid (2,2-CPPA), 2-(3-chloro)-phenoxy propionic acid (2,3- CPPA), phenoxy propionic acid (PPA) and 2-(2,4-dichlorophenoxy) propionic acid (2,4-DP). The operating parameters of the in-tube SPME-HPLC system, including the length of the monolithic column, the sampling flow rate, the sampling time, the elution flow rate and the elution time, had been investigated in detail. The optimized operating parameters of the in-tube SPME-HPLC system were as follow: the length of the monolithic column was 20 cm, the sampling flow rate was 0. 04 mL/min, sampling time was 13 min; the elution flow rate was 0.02 mL/min, elution time was 5 min. Under the optimized conditions, the detection limits of the five phenoxy acid herbicides were as follows: 9 µg/L for PPA, 4 µg/L for 2,2-CPPA, 4 µg/L for 2,3-CPPA, 5 µg/L for 2,4-D, 5 µg/L for 2,4-DP. Compared with the HPLC method with direct injection, the combined system showed a good enrichment factors to the analytes. The recoveries of the five phenoxy acid herbicides were between 79.0% and 98.0% (RSD ≤ 3.9%). This method was successfully used to detect the five phenoxy acid herbicides in water samples with satisfactory results.

Simultaneous separation of water- and fat-soluble vitamins in isocratic pressure-assisted capillary electrochromatography using a methacrylate-based monolithic column.

PubMed

Yamada, Hiroki; Kitagawa, Shinya; Ohtani, Hajime

2013-06-01

A method of simultaneous separation of water- and fat-soluble vitamins using pressure-assisted CEC with a methacrylate-based capillary monolithic column was developed. In the proposed method, water-soluble vitamins were mainly separated electrophoretically, while fat soluble-ones were separated chromatographically by the interaction with a methacrylate-based monolith. A mixture of six water-soluble and four fat-soluble vitamins was separated simultaneously within 20 min with an isocratic elution using 1 M formic acid (pH 1.9)/acetonitrile (30:70, v/v) containing 10 mM ammonium formate as a mobile phase. When the method was applied to a commercial multivitamin tablet and a spiked one, the vitamins were successfully analyzed, and no influence of the matrix contained in the tablet was observed. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Composite polymer: Glass edge cladding for laser disks

DOEpatents

Powell, H.T.; Wolfe, C.A.; Campbell, J.H.; Murray, J.E.; Riley, M.O.; Lyon, R.E.; Jessop, E.S.

1987-11-02

Large neodymium glass laser disks for disk amplifiers such as those used in the Nova laser require an edge cladding which absorbs at 1 micrometer. This cladding prevents edge reflections from causing parasitic oscillations which would otherwise deplete the gain. Nova now utilizes volume-absorbing monolithic-glass claddings which are fused at high temperature to the disks. These perform quite well but are expensive to produce. Absorbing glass strips are adhesively bonded to the edges of polygonal disks using a bonding agent whose index of refraction matches that of both the laser and absorbing glass. Optical finishing occurs after the strips are attached. Laser disks constructed with such claddings have shown identical gain performance to the previous Nova disks and have been tested for hundreds of shots without significant degradation. 18 figs.

Composite polymer-glass edge cladding for laser disks

DOEpatents

Powell, Howard T.; Riley, Michael O.; Wolfe, Charles R.; Lyon, Richard E.; Campbell, John H.; Jessop, Edward S.; Murray, James E.

1989-01-01

Large neodymium glass laser disks for disk amplifiers such as those used in the Nova laser require an edge cladding which absorbs at 1 micrometer. This cladding prevents edge reflections from causing parasitic oscillations which would otherwise deplete the gain. Nova now utilizes volume-absorbing monolithic-glass claddings which are fused at high temperature to the disks. These perform quite well but are expensive to produce. Absorbing glass strips are adhesively bonded to the edges of polygonal disks using a bonding agent whose index of refraction matches that of both the laser and absorbing glass. Optical finishing occurs after the strips are attached. Laser disks constructed with such claddings have shown identical gain performance to the previous Nova disks and have been tested for hundreds of shots without significant degradation.

Aluminum based metal-organic framework-polymer monolith in solid-phase microextraction of penicillins in river water and milk samples.

PubMed

Lirio, Stephen; Liu, Wan-Ling; Lin, Chen-Lan; Lin, Chia-Her; Huang, Hsi-Ya

2016-01-08

In this study, aluminum based metal-organic framework (Al-MOF)-organic polymer monoliths were prepared via microwave-assisted polymerization of ethylene dimethacrylate (EDMA), butyl methacrylate (BMA) with different weight percentages of Al-MOF (MIL-53; 37.5-62.5%) and subsequently utilized as sorbent in solid-phase microextraction (SPME) of penicillins (penicillin G, penicillin V, oxacillin, cloxacillin, dicloxacillin, nafcillin). The Al-MOF-polymer was characterized using Fourier transform infrared (FTIR) spectroscopy, powder X-ray diffraction (XRD), scanning electron microscopy (SEM) and SEM-energy-dispersive X-ray spectroscopy (SEM-EDS) to clarify the retained crystalline structure well as the homogeneous dispersion of Al-MOF (MIL-53) in polymer monolith. The developed Al-MOF-polymer (MIL-53) monolithic column was evaluated according to its extraction recovery of penicillins. Several parameters affecting the extraction recoveries of penicillins using fabricated Al-MOF-polymer (MIL-53) monolithic column including different MIL-53 weight percentages, column length, pH, desorption solvent, and mobile phase flow rate were investigated. For comparison, different Al-based MOFs (MIL-68, CYCU-4 and DUT-5) were fabricated using the optimized condition for MIL-53-polymer (sample matrix at pH 3, 200μL desorption volume using methanol, 37.5% of MOF, 4-cm column length at 0.100mLmin(-1) flow rate). Among all the Al-MOF-polymers, MIL-53(Al)-polymer still afforded the best extraction recovery for penicillins ranging from 90.5 to 95.7% for intra-day with less than 3.5% relative standard deviations (RSDs) and inter-day precision were in the range of 90.7-97.6% with less than 4.2% RSDs. Meanwhile, the recoveries for column-to-column were in the range of 89.5-93.5% (<3.4% RSDs) while 88.5-90.5% (<5.8% RSDs) for batch-to-batch (n=3). Under the optimal conditions, the limit of detections were in the range of 0.06-0.26μgL(-1) and limit of quantifications between 0.20 and 0.87μgL(-1). Finally, the MIL-53-polymer was applied for the extraction of penicillin in river water and milk by spiking trace-level penicillin for as low as 50μgL(-1) and 100μgL(-1) with recoveries ranging from 80.8% to 90.9% (<6.7% RSDs) in river water and 81.1% to 100.7% (<7.1% RSDs) in milk sample, respectively. Copyright © 2015 Elsevier B.V. All rights reserved.

Determination of ambroxol hydrochloride, methylparaben and benzoic acid in pharmaceutical preparations based on sequential injection technique coupled with monolithic column.

PubMed

Satínský, Dalibor; Huclová, Jitka; Ferreira, Raquel L C; Montenegro, Maria Conceição B S M; Solich, Petr

2006-02-13

The porous monolithic columns show high performance at relatively low pressure. The coupling of short monoliths with sequential injection technique (SIA) results in a new approach to implementation of separation step to non-separation low-pressure method. In this contribution, a new separation method for simultaneous determination of ambroxol, methylparaben and benzoic acid was developed based on a novel reversed-phase sequential injection chromatography (SIC) technique with UV detection. A Chromolith SpeedROD RP-18e, 50-4.6 mm column with 10 mm precolumn and a FIAlab 3000 system with a six-port selection valve and 5 ml syringe were used for sequential injection chromatographic separations in our study. The mobile phase used was acetonitrile-tetrahydrofuran-0.05M acetic acid (10:10:90, v/v/v), pH 3.75 adjusted with triethylamine, flow rate 0.48 mlmin(-1), UV-detection was at 245 nm. The analysis time was <11 min. A new SIC method was validated and compared with HPLC. The method was found to be useful for the routine analysis of the active compounds ambroxol and preservatives (methylparaben or benzoic acid) in various pharmaceutical syrups and drops.

Coatings of molecularly imprinted polymers based on polyhedral oligomeric silsesquioxane for open tubular capillary electrochromatography.

PubMed

Zhao, Qing-Li; Zhou, Jin; Zhang, Li-Shun; Huang, Yan-Ping; Liu, Zhao-Sheng

2016-05-15

Polyhedral oligomeric silsesquioxane (POSS) was successfully applied, for the first time, to prepare imprinted monolithic coating for capillary electrochromatography. The imprinted monolithic coating was synthesized with a mixture of PSS-(1-Propylmethacrylate)-heptaisobutyl substituted (MA 0702), S-amlodipine (template), methacrylic acid (functional monomer), and 2-methacrylamidopropyl methacrylate (crosslinker), in a porogenic mixture of toluene-isooctane. The influence of synthesis parameters on the imprinting effect and separation performance, including the amount of MA 0702, the ratio of template to monomer, and the ratio of monomer to crosslinker, was investigated. The greatest resolution for enantiomers separation on the imprinted monolithic column prepared with MA 0702 was up to 22.3, about 2 times higher than that prepared in absence of the POSS. Column efficiency on the POSS-based MIP coatings was beyond 30,000 plate m(-1). The comparisons between MIP coating synthesized with the POSS and without the POSS were made in terms of selectivity, column efficiency, and resolution. POSS-based MIP capillaries with naproxen or zopiclone was also prepared and separation of enantiomers can be achieved. Copyright © 2016 Elsevier B.V. All rights reserved.

Polymeric monolith column composited with multiwalled carbon nanotubes-β-cyclodextrin for the selective extraction of psoralen and isopsoralen.

PubMed

Ling, Xu; Zou, Li; Chen, Zilin

2017-09-01

A polymeric column that contains multiwalled carbon nanotubes-β-cyclodextrin composite was developed. The composite was wrapped into the poly(butyl methacrylate-ethylene dimethacrylate) monolith column (0.76 mm id and 10 cm in length). The column was then applied for the online solid-phase microextraction of psoralen and isopsoralen from Fructus Psoraleae. Following microextraction, the coumarins were quantified by high-performance liquid chromatography with C 18 separation column and UV detection. The effects of sample flow rate, sample volume, and pH value were optimized. The method showed low limits of detection (20 pg/mL, S/N = 3) for both psoralen and isopsoralen. Finally the method was successfully applied to the determination of psoralen and isopsoralen in spiked herb extracts and rat plasma where it gave recoveries that ranged between 93.2 and 102.1%. The empty hydrophobic cavities of β-cyclodextrin and the hydrophobicity of multiwalled carbon nanotubes provided specific extraction capability for psoralen and isopsoralen. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

High-performance liquid chromatography separation of unsaturated organic compounds by a monolithic silica column embedded with silver nanoparticles.

PubMed

Zhu, Yang; Morisato, Kei; Hasegawa, George; Moitra, Nirmalya; Kiyomura, Tsutomu; Kurata, Hiroki; Kanamori, Kazuyoshi; Nakanishi, Kazuki

2015-08-01

The optimization of a porous structure to ensure good separation performances is always a significant issue in high-performance liquid chromatography column design. Recently we reported the homogeneous embedment of Ag nanoparticles in periodic mesoporous silica monolith and the application of such Ag nanoparticles embedded silica monolith for the high-performance liquid chromatography separation of polyaromatic hydrocarbons. However, the separation performance remains to be improved and the retention mechanism as compared with the Ag ion high-performance liquid chromatography technique still needs to be clarified. In this research, Ag nanoparticles were introduced into a macro/mesoporous silica monolith with optimized pore parameters for high-performance liquid chromatography separations. Baseline separation of benzene, naphthalene, anthracene, and pyrene was achieved with the theoretical plate number for analyte naphthalene as 36,000 m(-1). Its separation function was further extended to cis/trans isomers of aromatic compounds where cis/trans stilbenes were chosen as a benchmark. Good separation of cis/trans-stilbene with separation factor as 7 and theoretical plate number as 76,000 m(-1) for cis-stilbene was obtained. The trans isomer, however, is retained more strongly, which contradicts the long- established retention rule of Ag ion chromatography. Such behavior of Ag nanoparticles embedded in a silica column can be attributed to the differences in the molecular geometric configuration of cis/trans stilbenes. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Influence of porogen nature on the kinetic and potential efficiencies of divinylbenzene-based monolithic sorbents in gas chromatography

NASA Astrophysics Data System (ADS)

Korolev, A. A.; Shiryaeva, V. E.; Popova, T. P.; Kanat'eva, A. Yu.; Kurganov, A. A.

2015-02-01

It has been shown that using Poppe curves for characterization of monolithic sorbents makes it possible to optimize conditions for both the synthesis of monoliths intended for high-speed analysis and achievement of the best separation efficiency. The influence of the nature of a porogen on the kinetic efficiency of monolithic sorbents in high-pressure gas chromatography has been considered. It has been found that the nature of the porogen alcohol determines to a considerable extent the structure of the monolith and its kinetic efficiency. The sorbents prepared with the use of octanol-1 and dodecanol-1 have shown the best kinetic characteristics; however, minimal HETP values have been observed for the columns prepared using hexanol-1 as a porogen.

Incorporation of ionic liquid into porous polymer monoliths to enhance the separation of small molecules in reversed-phase high-performance liquid chromatography.

PubMed

Wang, Jiafei; Bai, Ligai; Wei, Zhen; Qin, Junxiao; Ma, Yamin; Liu, Haiyan

2015-06-01

An ionic liquid was incorporated into the porous polymer monoliths to afford stationary phases with enhanced chromatographic performance for small molecules in reversed-phase high-performance liquid chromatography. The effect of the ionic liquid in the polymerization mixture on the performance of the monoliths was studied in detail. While monoliths without ionic liquid exhibited poor resolution and low efficiency, the addition of ionic liquid to the polymerization mixture provides highly increased resolution and high efficiency. The chromatographic performances of the monoliths were demonstrated by the separations of various small molecules including aromatic hydrocarbons, isomers, and homologues using a binary polar mobile phase. The present column efficiency reached 27 000 plates/m, which showed that the ionic liquid monoliths are alternative stationary phases in the separation of small molecules by high-performance liquid chromatography. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Sequence-specific sepsis-related DNA capture and fluorescent labeling in monoliths prepared by single-step photopolymerization in microfluidic devices.

PubMed

Knob, Radim; Hanson, Robert L; Tateoka, Olivia B; Wood, Ryan L; Guerrero-Arguero, Israel; Robison, Richard A; Pitt, William G; Woolley, Adam T

2018-05-21

Fast determination of antibiotic resistance is crucial in selecting appropriate treatment for sepsis patients, but current methods based on culture are time consuming. We are developing a microfluidic platform with a monolithic column modified with oligonucleotides designed for sequence-specific capture of target DNA related to the Klebsiella pneumoniae carbapenemase (KPC) gene. We developed a novel single-step monolith fabrication method with an acrydite-modified capture oligonucleotide in the polymerization mixture, enabling fast monolith preparation in a microfluidic channel using UV photopolymerization. These prepared columns had a threefold higher capacity compared to monoliths prepared in a multistep process involving Schiff-base DNA attachment. Conditions for denaturing, capture and fluorescence labeling using hybridization probes were optimized with synthetic 90-mer oligonucleotides. These procedures were applied for extraction of a PCR amplicon from the KPC antibiotic resistance gene in bacterial lysate obtained from a blood sample spiked with E. coli. The results showed similar eluted peak areas for KPC amplicon extracted from either hybridization buffer or bacterial lysate. Selective extraction of the KPC DNA was verified by real time PCR on eluted fractions. These results show great promise for application in an integrated microfluidic diagnostic system that combines upstream blood sample preparation and downstream single-molecule counting detection. Copyright © 2018 Elsevier B.V. All rights reserved.

DEVELOPMENT OF AN AFFINITY SILICA MONOLITH CONTAINING HUMAN SERUM ALBUMIN FOR CHIRAL SEPARATIONS

PubMed Central

Mallik, Rangan; Hage, David S.

2008-01-01

An affinity monolith based on silica and containing immobilized human serum albumin (HSA) was developed and evaluated in terms of its binding, efficiency and selectivity in chiral separations. The results were compared with data obtained for the same protein when used as a chiral stationary phase with HPLC-grade silica particles or a monolith based on a copolymer of glycidyl methacrylate (GMA) and ethylene dimethacrylate (EDMA). The surface coverage of HSA in the silica monolith was similar to values obtained with silica particles and a GMA/EDMA monolith. However, the higher surface area of the silica monolith gave a material that contained 1.3- to 2.2-times more immobilized HSA per unit volume when compared to silica particles or a GMA/EDMA monolith. The retention, efficiency and resolving power of the HSA silica monolith were evaluated using two chiral analytes: D/L-tryptophan and R/S-warfarin. The separation of R- and S-ibuprofen was also considered. The HSA silica monolith gave higher retention and higher or comparable resolution and efficiency when compared with HSA columns that contained silica particles or a GMA/EDMA monolith. The silica monolith also gave lower back pressures and separation impedances than these other materials. It was concluded that silica monoliths can be valuable alternatives to silica particles or GMA/EDMA monoliths when used with immobilized HSA as a chiral stationary phase. PMID:17475436

Kinetic efficiency of polar monolithic capillary columns in high-pressure gas chromatography.

PubMed

Kurganov, A A; Korolev, A A; Shiryaeva, V E; Popova, T P; Kanateva, A Yu

2013-11-08

Poppe plots were used for analysis of kinetic efficiency of monolithic sorbents synthesized in quartz capillaries for utilization in high-pressure gas chromatography. Values of theoretical plate time and maximum number of theoretical plates occurred to depend significantly on synthetic parameters such as relative amount of monomer in the initial polymerization mixture, temperature and polymerization time. Poppe plots let one to find synthesis conditions suitable either for high-speed separations or for maximal efficiency. It is shown that construction of kinetic Poppe curves using potential Van Deemter data demands compressibility of mobile phase to be taken into consideration in the case of gas chromatography. Model mixture of light hydrocarbons C1 to C4 was then used for investigation of influence of carrier gas nature on kinetic efficiency of polymeric monolithic columns. Minimal values of theoretical plate times were found for CO2 and N2O carrier gases. Copyright © 2013 Elsevier B.V. All rights reserved.

Novel beta-cyclodextrin derivative functionalized polymethacrylate-based monolithic columns for enantioselective separation of ibuprofen and naproxen enantiomers in capillary electrochromatography.

PubMed

Tian, Yun; Zhong, Cheng; Fu, Enqin; Zeng, Zhaorui

2009-02-06

A novel enantioselective polymethacrylate-based monolithic column for capillary electrochromatography was prepared by ring-opening reaction of epoxy groups from poly(glycidyl methacrylate-co-ethylene dimethacrylate) monolith with a novel beta-cyclodextrin derivative bearing 4-dimethylamino-1,8-naphthalimide functionalities. Conditions for the ring-opening reaction with respect to different reaction parameters were thoroughly optimized to obtain high electroosmotic flow, separation efficiency and enantioselectivity for the analytes. The nonaqueous mobile phase composition regarding acetonitrile-methanol ratio and the concentration of electrolyte were examined to manipulate the hydrophobic inclusion and anion-exchange interaction between the analytes and chiral stationary phase. It was observed that in addition to beta-cyclodextrin cavity, the electrostatic interaction exhibited pronounced influence on the enantioseparation of acidic analytes. Acidic enantiomers (ibuprofen and naproxen) could be separated with separation factor (alpha) values up to 1.08 and a maximum separation efficiency of 86000 plates/m could be achieved.

Monolithic silica spin column extraction and simultaneous derivatization of amphetamines and 3,4-methylenedioxyamphetamines in human urine for gas chromatographic-mass spectrometric detection.

PubMed

Nakamoto, Akihiro; Nishida, Manami; Saito, Takeshi; Kishiyama, Izumi; Miyazaki, Shota; Murakami, Katsunori; Nagao, Masataka; Namura, Akira

2010-02-19

A simple, sensitive, and specific method with gas chromatography-mass spectrometry was developed for simultaneous extraction and derivatization of amphetamines (APs) and 3,4-methylenedioxyamphetamines (MDAs) in human urine by using a monolithic silica spin column. All the procedures, such as sample loading, washing, and elution were performed by centrifugation. APs and MDAs in urine were adsorbed on the monolithic silica and derivatized with propyl chloroformate in the column. Methamphetamine-d(5) was used as an internal standard. The linear ranges were 0.01-5.0 microg mL(-1) for methamphetamine (MA) and 3,4-methylenedioxymethamphetamine (MDMA) and 0.02-5.0 microg mL(-1) for amphetamine (AP) and 3,4-methylenedioxyamphetamine (MDA) (coefficient of correlation > or = 0.995). The recovery of APs and MDAs in urine was 84-94%, and the relative standard deviation of the intra- and interday reproducibility for urine samples containing 0.1, 1.0, and 4.0 microg mL(-1) of APs and MDAs ranged from 1.4% to 13.6%. The lowest detection limit (signal-to-noise ratio > or = 3) in urine was 5 ng mL(-1) for MA and MDMA and 10 ng mL(-1) for AP and MDA. The proposed method can be used to perform simultaneous extraction and derivatization on spin columns that have been loaded with a small quantity of solvent by using centrifugation. Copyright 2009 Elsevier B.V. All rights reserved.

Porous polymer monolithic columns with gold nanoparticles as an intermediate ligand for the separation of proteins in reverse phase-ion exchange mixed mode

DOE PAGES

Terborg, Lydia; Masini, Jorge C.; Lin, Michelle; ...

2014-11-04

A new approach has been developed for the preparation of mixed-mode stationary phases to separate proteins. The pore surface of monolithic poly(glycidyl methacrylate- co-ethylene dimethacrylate) capillary columns was functionalized with thiols and coated with gold nanoparticles. The final mixed mode surface chemistry was formed by attaching, in a single step, alkanethiols, mercaptoalkanoic acids, and their mixtures on the free surface of attached gold nanoparticles. Use of these mixtures allowed fine tuning of the hydrophobic/hydrophilic balance. The amount of attached gold nanoparticles according to thermal gravimetric analysis was 44.8 wt.%. This value together with results of frontal elution enabled calculation ofmore » surface coverage with the alkanethiol and mercaptoalkanoic acid ligands. Interestingly, alkanethiols coverage in a range of 4.46–4.51 molecules/nm 2 significantly exceeded that of mercaptoalkanoic acids with 2.39–2.45 molecules/nm 2. The mixed mode character of these monolithic stationary phases was for the first time demonstrated in the separations of proteins that could be achieved in the same column using gradient elution conditions typical of reverse phase (using gradient of acetonitrile in water) and ion exchange chromatographic modes (applying gradient of salt in water), respectively.« less

Green approach using monolithic column for simultaneous determination of coformulated drugs.

PubMed

Yehia, Ali M; Mohamed, Heba M

2016-06-01

Green chemistry and sustainability is now entirely encompassed across the majority of pharmaceutical companies and research labs. Researchers' attention is careworn toward implementing the green analytical chemistry principles for more eco-friendly analytical methodologies. Solvents play a dominant role in determining the greenness of the analytical procedure. Using safer solvents, the greenness profile of the methodology could be increased remarkably. In this context, a green chromatographic method has been developed and validated for the simultaneous determination of phenylephrine, paracetamol, and guaifenesin in their ternary pharmaceutical mixture. The chromatographic separation was carried out using monolithic column and green solvents as mobile phase. The use of monolithic column allows efficient separation protocols at higher flow rates, which results in short time of analysis. Two-factor three-level experimental design was used to optimize the chromatographic conditions. The greenness profile of the proposed methodology was assessed using eco-scale as a green metrics and was found to be an excellent green method with regard to the usage and production of hazardous chemicals and solvents, energy consumption, and amount of produced waste. The proposed method improved the environmental impact without compromising the analytical performance criteria and could be used as a safer alternate for the routine analysis of the studied drugs. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Reversed-phase HPLC analysis of levetiracetam in tablets using monolithic and conventional C18 silica columns.

PubMed

Can, Nafiz O; Arli, Goksel

2010-01-01

Development and validation of an RP-HPLC method for determination of levetiracetam in pharmaceutical tablets is described. The separation and quantification of levetiracetam and caffeine (internal standard) were performed using a single analytical procedure with two different types of stationary phases, conventional Phenomenex Gemini C18 (100 x 4.6 mm, 5 microm) and Merck Chromolith Performance RP18e (100 x 4.6 mm, macropore size 2 mm, micropore size 13 nm) monolithic silica. Five-microliter aliquots of samples were injected into the system and eluted using water-acetonitrile (90 + 10, v/v) mobile phase pumped at the rate of 1 mL/min. The analyte peaks were detected at 200 nm using a diode array detector with adequate resolution. Validation studies were performed using the method recommended by the International Conference on Harmonization, the U.S. Pharmacopeia, and AOAC INTERNATIONAL, which includes accuracy, precision, range, limits, robustness, and system suitability parameters. Levetiracetam and caffeine were detected in about 7 min using the conventional column, whereas less than 5 min was required when the monolithic column was used. Calibration plots had r values close to unity in the range of 0.8-8.0 microg/mL. Assay of levetiracetam in a tablet formulation was demonstrated as an application to real samples.

CEC-atmospheric pressure ionization MS of pesticides using a surfactant-bound monolithic column.

PubMed

Gu, Congying; Shamsi, Shahab A

2010-04-01

A surfactant bound poly (11-acrylaminoundecanoic acid-ethylene dimethacrylate) monolithic column was simply prepared by in situ co-polymerization of 11-acrylaminoundecanoic acid and ethylene dimethacrylate with 1-propanol, 1,4-butanediol and water as porogens in 100 microm id fused-silica capillary in one step. This column was used in CEC-atmospheric pressure photoionization (APPI)-MS system for separation and detection of N-methylcarbamates pesticides. Numerous parameters are optimized for CEC-APPI-MS. After evaluation of the mobile phase composition, sheath liquid composition and the monolithic capillary outlet position, a fractional factorial design was selected as a screening procedure to identify factors of ionization source parameters, such as sheath liquid flow rate, drying gas flow rate, drying gas temperature, nebulizing gas pressure, vaporizer temperature and capillary voltage, which significantly influence APPI-MS sensitivity. A face-centered central composite design was further utilized to optimize the most significant parameters and predict the best sensitivity. Under optimized conditions, S/Ns around 78 were achieved for an injection of 100 ng/mL of each pesticide. Finally, this CEC-APPI-MS method was successfully applied to the analysis of nine N-methylcarbamates in spiked apple juice sample after solid phase extraction with recoveries in the range of 65-109%.

Property evaluations and application for separation of small molecules of a nanodiamond-polymer composite monolithic column.

PubMed

Wang, Fengqing; Wei, Aile; Wang, Xixi; Liu, Haiyan; Bai, Ligai; Yan, Hongyuan

2016-07-01

A nanodiamond-polymer composite monolithic column was first prepared successfully with modified nanodiamond (ND) as monomer, ethylene glycol dimethacrylate (EDMA) as cross-linker, 1-dodecanol as porogenic agent and benzoyl peroxide/dimethylacetamide (BPO/DMA) as initiator at 35°C for 2.5h. There was a sharp increase of specific surface area with ND added about 22 times from 0mg (3.90m(2)/g) to 7mg (81.2m(2)/g) determined with BET. Characterizations including scanning electron microscopy (SEM), fourier-transform infrared spectra (FIRT) and mercury intrusion porosimetry (MIP) were used to determine the microstructure, group composition, pore size distribution (≃1.56μm) and porosity (≃0.7484μm) of the monolith. An excellent column stability was confirmed by permeability (1.258x10(-10)cm(2)) and good linearity (R(2)=0.998) corresponding to backpressures measured at different flow rates. The highest swelling ability of the composite was about (5%) and classical RPLC of the column obtained occurred with the acetonitrile concentration increasing from 20% to 85% in the mobile phase, above which another retention model of normal-phase chromatography appeared. The items of the eddy dispersion and the absorption-release kinetics were the decisional factors of the composite column compared with the factors of longitudinal diffusion, and the skeleton-eluent mass transfer resistance due to the finite diffusivity. Good separation of neutral and basic small molecules was obtained (24,350 plates/m for neutral molecules and 22,300 plates/m for basic ones) with the hydrophobicity retention mechanism, but not for the acidic ones except to regulate the pH of the mobile phase. Copyright © 2016 Elsevier B.V. All rights reserved.

Synthesis and wear behavior of aluminum 6061 alloy reinforced with carbon nanotubes

NASA Astrophysics Data System (ADS)

Khalil, Abdullah

In the present work, Al6061 alloy was uniformly reinforced with 0.5, 0.75, 1 and 2 wt. % Carbon Nanotubes (CNTs) using two way dispersion method. For consolidation, Spark Plasma Sintering (SPS) was used which resulted in very high densification for the matrix as well as composite. Results showed that addition of CNTs lead to increased hardness of the material and maximum hardness was found for 1 wt. % CNTs. So this composition was selected for detailed wear analysis. Pin-on-disk wear tests were conducted for the monolithic Al6061 and the composite at a constant speed of 0.5 m/s with varying load from 5 N to 30 N under dry sliding conditions using AISI 4140 steel disk as a counterface. The composite displayed lower wear rate and friction coefficient at lower levels of applied stress (0.175 to 0.525 MPa). Under higher stresses (0.700 to 1.050 MPa), the increased brittleness and porosity of the composite caused severe fracturing and delamination resulting in excessive wear rate and friction coefficient for the composite as compared to monolithic Al6061. The transition from mild to severe wear regime in composite occurred also at lower stress as compared to monolith. Analysis of the worn surfaces revealed abrasion as the dominant wear mechanism for both the materials at lower stresses. At higher stress levels, adhesion was found to be dominant in monolithic Al6061 whereas in composite, excessive sub-surface fracturing and delamination was mainly observed.

Development of optically pumped DBR-free semiconductor disk lasers (Conference Presentation)

NASA Astrophysics Data System (ADS)

Yang, Zhou; Albrecht, Alexander R.; Cederberg, Jeffrey G.; Sheik-Bahae, Mansoor

2017-03-01

Semiconductor disk lasers (SDLs) are attractive for applications requiring good beam quality, wavelength versatility, and high output powers. Typical SDLs utilize the active mirror geometry, where a semiconductor DBR is integrated with the active region by growth or post-growth bonding. This imposes restrictions for the SDL design, like material system choice, thermal management, and effective gain bandwidth. In DBR-free geometry, these restrictions can be alleviated. An integrated gain model predicts DBR-free geometry with twice the gain bandwidth of typical SDLs, which has been experimentally verified with active regions near 1 μm and 1.15 μm. The lift-off and bonding technique enables the integration of semiconductor active regions with arbitrary high quality substrates, allowing novel monolithic geometries. Bonding an active region onto a straight side of a commercial fused silica right angle prism, and attaching a high reflectivity mirror onto the hypotenuse side, with quasi CW pumping at 780 nm, lasing operation was achieved at 1037 nm with 0.2 mW average power at 1.6 mW average pump power. Laser dynamics show that thermal lens generation in the active region bottlenecks the laser efficiency. Investigations on total internal reflection based monolithic ring cavities are ongoing. These geometries would allow the intracavity integration of 2D materials or other passive absorbers, which could be relevant for stable mode locking. Unlike typical monolithic microchip SDLs, with the evanescent wave coupling technique, these monolithic geometries allow variable coupling efficiency.

Preparation of polyhedral oligomeric silsesquioxane based hybrid monoliths by ring-opening polymerization for capillary LC and CEC.

PubMed

Lin, Hui; Zhang, Zhenbin; Dong, Jing; Liu, Zhongshan; Ou, Junjie; Zou, Hanfa

2013-09-01

A new organic-inorganic hybrid monolith was prepared by the ring-opening polymerization of octaglycidyldimethylsilyl polyhedral oligomeric silsesquioxane (POSS) with 1,4-butanediamine (BDA) using 1-propanol, 1,4-butanediol, and PEG 10,000 as a porogenic system. Benefiting from the moderate phase separation process, the resulting poly(POSS-co-BDA) hybrid monolith possessed a uniform microstructure and exhibited excellent performance in chromatographic applications. Neutral, acidic, and basic compounds were successfully separated on the hybrid monolith in capillary LC (cLC), and high column efficiencies were achieved in all of the separations. In addition, as the amino groups could generate a strong EOF, the hybrid monolith was also applied in CEC for the separation of neutral and polar compounds, and a satisfactory performance was obtained. These results demonstrate that the poly(POSS-co-BDA) hybrid monolith is a good separation media in chromatographic separations of various types of compounds by both cLC and CEC. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Behavior of short silica monolithic columns in high pressure gas chromatography.

PubMed

Maniquet, Adrien; Bruyer, Nicolas; Raffin, Guy; Baco-Antoniali, Franck; Demesmay, Claire; Dugas, Vincent; Randon, Jérôme

2016-08-19

In order to analyze light hydrocarbons mixtures with silica monolithic columns, a conventional gas chromatograph was modified to work with carrier gas pressure as high as 60bar. To understand hydrodynamic flow and retention with short columns (less than 30cm), special attention was required due to the temperature difference between the oven area and the FID detector which contain a significant length of the column. Efficiency and selectivity using various carrier gases (helium, nitrogen and carbon dioxide) at different inlet pressure for different oven temperature were studied. Carrier gas nature was a very significant parameter: on one side, linked to adsorption mechanism for gases like nitrogen and carbon dioxide onto the stationary phase modifying retention and selectivity, on the other side in relation to the minimum theoretical plate height which was as low as 15μm (66 000 platem(-1)) using carbon dioxide as carrier gas. The chromatographic system was then used to separate methane, ethane, ethylene, acetylene, propane, cyclopropane, and butane in less than 30s. Copyright © 2016 Elsevier B.V. All rights reserved.

High power disk lasers: advances and applications

NASA Astrophysics Data System (ADS)

Havrilla, David; Holzer, Marco

2011-02-01

Though the genesis of the disk laser concept dates to the early 90's, the disk laser continues to demonstrate the flexibility and the certain future of a breakthrough technology. On-going increases in power per disk, and improvements in beam quality and efficiency continue to validate the genius of the disk laser concept. As of today, the disk principle has not reached any fundamental limits regarding output power per disk or beam quality, and offers numerous advantages over other high power resonator concepts, especially over monolithic architectures. With well over 1000 high power disk lasers installations, the disk laser has proven to be a robust and reliable industrial tool. With advancements in running cost, investment cost and footprint, manufacturers continue to implement disk laser technology with more vigor than ever. This paper will explain important details of the TruDisk laser series and process relevant features of the system, like pump diode arrangement, resonator design and integrated beam guidance. In addition, advances in applications in the thick sheet area and very cost efficient high productivity applications like remote welding, remote cutting and cutting of thin sheets will be discussed.

Determination of nitrite, nitrate, bromide, and iodide in seawater by ion chromatography with UV detection using dilauryldimethylammonium-coated monolithic ODS columns and sodium chloride as an eluent.

PubMed

Ito, Kazuaki; Nomura, Ryosuke; Fujii, Takuya; Tanaka, Masahito; Tsumura, Tomoaki; Shibata, Hiroyuki; Hirokawa, Takeshi

2012-11-01

A method was developed for determination of inorganic anions, including nitrite (NO(2)(-)), nitrate (NO(3)(-)), bromide (Br(-)), and iodide (I(-)), in seawater by ion chromatography (IC). The IC system used two dilauryldimethylammonium bromide (DDAB)-coated monolithic ODS columns (50 × 4.6 mm i.d. and 100 × 4.6 mm i.d.) connected in series for separation of the ions. Aqueous NaCl (0.5 mol/L; flow rate, 3 mL/min) containing 5 mmol/L phosphate buffer (pH 5) was used as the eluent, and detection was with a UV detector at 225 nm. The monolithic ODS columns were coated and equilibrated with a 1-mmol/L DDAB solution (in H(2)O/methanol, 90:10 v/v). The hydrophilic ions (NO(2)(-), NO(3)(-), and Br(-)) were separated within 3 min and the retention time of I(-) was 16 min. No interferences from matrix ions, such as chloride and sulfate ions, were observed in 35 ‰ artificial seawater. The detection limits were 0.6 μg/L for NO(2)(-), 1.1 μg/L for NO(3)(-), 70 μg/L for Br(-), and 1.6 μg/L for I(-) with a 200-μL sample injection. The performance of the coated columns was maintained without addition of DDAB in the eluent. The IC system was successfully applied to real seawater samples with recovery rates of 94-108 % for all ions.

Multiplexed electrokinetic sample fractionation, preconcentration and elution for proteomics.

PubMed

Hua, Yujuan; Jemere, Abebaw B; Dragoljic, Jelena; Harrison, D Jed

2013-07-07

Both 6 and 8-channel integrated microfluidic sample pretreatment devices capable of performing "in space" sample fractionation, collection, preconcentration and elution of captured analytes via sheath flow assisted electrokinetic pumping are described. Coatings and monolithic polymer beds were developed for the glass devices to provide cationic surface charge and anodal electroosmotic flow for delivery to an electrospray emitter tip. A mixed cationic ([2-(methacryloyloxy)ethyl] trimethylammonium chloride) (META) and hydrophobic butyl methacrylate-based monolithic porous polymer, photopolymerized in the 6- or 8-fractionation channels, was used to capture and preconcentrate samples. A 0.45 wt% META loaded bed generated comparable anodic electroosmotic flow to the cationic polymer PolyE-323 coated channel segments in the device. The balanced electroosmotic flow allowed stable electrokinetic sheath flow to prevent cross contamination of separated protein fractions, while reducing protein/peptide adsorption on the channel walls. Sequential elution of analytes trapped in the SPE beds revealed that the monolithic columns could be efficiently used to provide sheath flow during elution of analytes, as demonstrated for neutral carboxy SNARF (residual signal, 0.08% RSD, n = 40) and charged fluorescein (residual signal, 2.5% n = 40). Elution from monolithic columns showed reproducible performance with peak area reproducibility of ~8% (n = 6 columns) in a single sequential elution and the run-to-run reproducibility was 2.4-6.7% RSD (n = 4) for elution from the same bed. The demonstrated ability of this device design and operation to elute from multiple fractionation beds into a single exit channel for sample analysis by fluorescence or electrospray mass spectrometry is a crucial component of an integrated fractionation and assay system for proteomics.

VOLATILE-RICH CIRCUMSTELLAR GAS IN THE UNUSUAL 49 CETI DEBRIS DISK

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

Roberge, Aki; Grady, Carol A.; Welsh, Barry Y.

2014-11-20

We present Hubble Space Telescope Space Telescope Imaging Spectrograph far-UV spectra of the edge-on disk around 49 Ceti, one of the very few debris disks showing submillimeter CO emission. Many atomic absorption lines are present in the spectra, most of which arise from circumstellar gas lying along the line-of-sight to the central star. We determined the line-of-sight C I column density, estimated the total carbon column density, and set limits on the O I column density. Surprisingly, no line-of-sight CO absorption was seen. We discuss possible explanations for this non-detection, and present preliminary estimates of the carbon abundances in themore » line-of-sight gas. The C/Fe ratio is much greater than the solar value, suggesting that 49 Cet harbors a volatile-rich gas disk similar to that of β Pictoris.« less

CO2 adsorption on modified carbon coated monolith: effect of surface modification by using alkaline solutions

NASA Astrophysics Data System (ADS)

Hosseini, Soraya; Marahel, Ehsan; Bayesti, Iman; Abbasi, Ali; Chuah Abdullah, L.; Choong, Thomas S. Y.

2015-01-01

A monolithic column was used to study the feasibility of modified carbon-coated monolith for recovery of CO2 from gaseous mixtures (He/CO2) in a variety of operating conditions. Carbon-coated monolith was prepared by dip-coating method and modified by two alkaline solutions, i.e. NH3 and KOH. The surface properties of the carbon-coated monolith were altered by functional groups via KOH and NH3 treatments. The comparative study of CO2 uptake by two different adsorbents, i.e. unmodified and modified carbon-coated monolith, demonstrated that the applied modification process had improved CO2 adsorption. The presence of nitrogen- and oxygen-containing functional groups on the surface of the carbon led to an improved level of microporosity on the synthesized carbon-coated monolith. The physical parameters such as higher surface area, lower pore diameter, and larger micropore volume of modified monoliths indicated direct influence on the adsorbed amount of CO2. In the present study, the Deactivation Model is applied to analyze the breakthrough curves. The adsorption capacity increased with an increase in pressure and concentration, while a reduction of CO2 adsorption capacity was occurred with increase in temperature. Ammonia (NH3) and potassium hydroxide (KOH)-modified carbon-coated monolith showed an increase of approximately 12 and 27% in CO2 adsorption, respectively, as compared to unmodified carbon-coated monolith.

Sequential Injection Chromatography with an Ultra-short Monolithic Column for the Low-Pressure Separation of α-Tocopherol and γ-Oryzanol in Vegetable Oils and Nutrition Supplements.

PubMed

Thaithet, Sujitra; Kradtap Hartwell, Supaporn; Lapanantnoppakhun, Somchai

2017-01-01

A low-pressure separation procedure of α-tocopherol and γ-oryzanol was developed based on a sequential injection chromatography (SIC) system coupled with an ultra-short (5 mm) C-18 monolithic column, as a lower cost and more compact alternative to the HPLC system. A green sample preparation, dilution with a small amount of hexane followed by liquid-liquid extraction with 80% ethanol, was proposed. Very good separation resolution (R s = 3.26), a satisfactory separation time (10 min) and a total run time including column equilibration (16 min) were achieved. The linear working range was found to be 0.4 - 40 μg with R 2 being more than 0.99. The detection limits of both analytes were 0.28 μg with the repeatability within 5% RSD (n = 7). Quantitative analyses of the two analytes in vegetable oil and nutrition supplement samples, using the proposed SIC method, agree well with the results from HPLC.

Approaches for enantioselective resolution of pharmaceuticals by miniaturised separation techniques with new chiral phases based on nanoparticles and monolithis.

PubMed

Sierra, Isabel; Marina, Maria Luisa; Pérez-Quintanilla, Damián; Morante-Zarcero, Sonia; Silva, Mariana

2016-10-01

This article discusses new developments in the preparation of nanoparticles and monoliths with emphasis upon their application as the stationary and pseudo-stationary phases for miniaturised liquid phase separation techniques, which have occurred in the last 10 years (from 2006 to the actuality). References included in this review represent current trends and state of the art in the application of these materials to the analysis, by EKC, CEC and miniaturised chromatography, of chiral compounds with environmental interest such as pharmaceuticals. Due to their extraordinary properties, columns prepared with these new chiral stationary or pseudo-stationary phases, based on materials such as gold nanoparticles, metal-organic frameworks, ordered mesoporous silicas, carbonaceous materials, polymeric-based and silica-based monoliths or molecularly imprinted materials, can usually show some improvements in the separation selectivity, column efficiency and chemical stability in comparison with conventional chiral columns available commercially. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Continuous flow immobilized enzyme reactor-tandem mass spectrometry for screening of AChE inhibitors in complex mixtures.

PubMed

Forsberg, Erica M; Green, James R A; Brennan, John D

2011-07-01

A method is described for identifying bioactive compounds in complex mixtures based on the use of capillary-scale monolithic enzyme-reactor columns for rapid screening of enzyme activity. A two-channel nanoLC system was used to continuously infuse substrate coupled with automated injections of substrate/small molecule mixtures, optionally containing the chromogenic Ellman reagent, through sol-gel derived acetylcholinesterase (AChE) doped monolithic columns. This is the first report of AChE encapsulated in monolithic silica for use as an immobilized enzyme reactor (IMER), and the first use of such IMERs for mixture screening. AChE IMER columns were optimized to allow rapid functional screening of compound mixtures based on changes in the product absorbance or the ratio of mass spectrometric peaks for product and substrate ions in the eluent. The assay had robust performance and produced a Z' factor of 0.77 in the presence of 2% (v/v) DMSO. A series of 52 mixtures consisting of 1040 compounds from the Canadian Compound Collection of bioactives was screened and two known inhibitors, physostigmine and 9-aminoacridine, were identified from active mixtures by manual deconvolution. The activity of the compounds was confirmed using the enzyme reactor format, which allowed determination of both IC(50) and K(I) values. Screening results were found to correlate well with a recently published fluorescence-based microarray screening assay for AChE inhibitors.

Monolithic metal-organic framework MIL-53(Al)-polymethacrylate composite column for the reversed-phase capillary liquid chromatography separation of small aromatics.

PubMed

Yusuf, Kareem; Badjah-Hadj-Ahmed, Ahmed Yacine; Aqel, Ahmad; ALOthman, Zeid Abdullah

2016-03-01

A monolithic capillary column containing a composite of metal-organic framework MIL-53(Al) incorporated into hexyl methacrylate-co-ethylene dimethacrylate was prepared to enhance the separation of mixtures of small aromatic compounds by using capillary liquid chromatography. The addition of 10 mg/mL MIL-53(Al) microparticles increased the micropore content in the monolithic matrix and increased the Brunauer-Emmett-Teller surface area from 26.92 to 85.12 m(2) /g. The presence of 1,4-benzenedicarboxylate moieties within the structure of MIL-53(Al) as an organic linker greatly influenced the separation of aromatic mixtures through π-π interactions. High-resolution separation was obtained for a series of alkylbenzenes (with resolution factors in the range 0.96-1.75) in less than 8 min, with 14 710 plates/m efficiency for propylbenzene, using a binary polar mobile phase of water/acetonitrile in isocratic mode. A reversed-phase separation mechanism was indicated by the increased retention factor and resolution as the water percentage in the mobile phase increased. A stability study on the composite column showed excellent mechanical stability under various conditions. The higher resolution and faster separation observed at increased temperature indicated an exothermic separation, whereas the negative values for the free energy change of transfer indicated a spontaneous process. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Seismic performance of interior precast concrete beam-column connections with T-section steel inserts under cyclic loading

NASA Astrophysics Data System (ADS)

Ketiyot, Rattapon; Hansapinyo, Chayanon

2018-04-01

An experimental investigation was conducted to study the performance of precast beam-column concrete connections using T-section steel inserts into the concrete beam and joint core, under reversed cyclic loading. Six 2/3-scale interior beam-column subassemblies, one monolithic concrete specimen and five precast concrete specimens were tested. One precast specimen was a simple connection for a gravity load resistant design. Other precast specimens were developed with different attributes to improve their seismic performance. The test results showed that the performance of the monolithic specimen M1 represented ductile seismic behavior. Failure of columns and joints could be prevented, and the failure of the frame occurred at the flexural plastic hinge formation at the beam ends, close to the column faces. For the precast specimens, the splitting crack along the longitudinal lapped splice was a major failure. The precast P5 specimen with double steel T-section inserts showed better seismic performance compared to the other precast models. However, the dowel bars connected to the steel inserts were too short to develop a bond. The design of the precast concrete beams with lap splice is needed for longer lap lengths and should be done at the beam mid span or at the low flexural stress region.

High-power disk lasers: advances and applications

NASA Astrophysics Data System (ADS)

Havrilla, David; Ryba, Tracey; Holzer, Marco

2012-03-01

Though the genesis of the disk laser concept dates to the early 90's, the disk laser continues to demonstrate the flexibility and the certain future of a breakthrough technology. On-going increases in power per disk, and improvements in beam quality and efficiency continue to validate the genius of the disk laser concept. As of today, the disk principle has not reached any fundamental limits regarding output power per disk or beam quality, and offers numerous advantages over other high power resonator concepts, especially over monolithic architectures. With about 2,000 high power disk lasers installations, and a demand upwards of 1,000 lasers per year, the disk laser has proven to be a robust and reliable industrial tool. With advancements in running cost, investment cost and footprint, manufacturers continue to implement disk laser technology with more vigor than ever. This paper will explain recent advances in disk laser technology and process relevant features of the laser, like pump diode arrangement, resonator design and integrated beam guidance. In addition, advances in applications in the thick sheet area and very cost efficient high productivity applications like remote welding, remote cutting and cutting of thin sheets will be discussed.

Vibration-tolerant narrow-linewidth semiconductor disk laser using novel frequency-stabilisation schemes

NASA Astrophysics Data System (ADS)

Hunter, Craig R.; Jones, Brynmor E.; Schlosser, Peter; Sørensen, Simon Toft; Strain, Michael J.; McKnight, Loyd J.

2018-02-01

This paper will present developments in narrow-linewidth semiconductor-disk-laser systems using novel frequencystabilisation schemes for reduced sensitivity to mechanical vibrations, a critical requirement for mobile applications. Narrow-linewidth single-frequency lasers are required for a range of applications including metrology and highresolution spectroscopy. Stabilisation of the laser was achieved using a monolithic fibre-optic ring resonator with free spectral range of 181 MHz and finesse of 52 to act as passive reference cavity for the laser. Such a cavity can operate over a broad wavelength range and is immune to a wide band of vibrational frequency noise due to its monolithic implementation. The frequency noise of the locked system has been measured and compared to typical Fabry-Perotlocked lasers using vibration equipment to simulate harsh environments, and analysed here. Locked linewidths of < 40 kHz have been achieved. These developments offer a portable, narrow-linewidth laser system for harsh environments that can be flexibly designed for a range of applications.

Preparation of a zeolite-modified polymer monolith for identification of synthetic colorants in lipsticks

NASA Astrophysics Data System (ADS)

Wang, Huiqi; Li, Zheng; Niu, Qian; Ma, Jiutong; Jia, Qiong

2015-10-01

A novel zeolite-modified poly(methacrylic acid-ethylenedimethacrylate) (zeolite@poly(MAA-EDMA)) monolithic column was prepared with the in situ polymerization method and employed in polymer monolith microextraction for the separation and preconcentration of synthetic colorants combined with high performance liquid chromatography. The polymer was characterized by scanning electronmicroscopy, Fourier-transform infrared spectroscopy, X-ray photoelectron spectroscopy, and thermo-gravimetric analysis. Various parameters affecting the extraction efficiency were investigated and optimized. Under the optimum experimental conditions, we obtained acceptable linearities, low limits of detection, and good intra-day/inter-day relative standard deviations. The method was applied to the determination of synthetic colorants in lipsticks with recoveries ranged from 70.7% to 109.7%. Compared with conventional methacrylic acid-based monoliths, the developed monolith exhibited high enrichment capacity because of the introduction of zeolites into the preparation process. The extraction efficiency followed the order: zeolite@poly(MAA-EDMA) > poly(MAA-EDMA) > direct HPLC analysis.

THE GAS/DUST RATIO OF CIRCUMSTELLAR DISKS: TESTING MODELS OF PLANETESIMAL FORMATION

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

Horne, David; Gibb, Erika; Rettig, Terrence W.

2012-07-20

We present high-resolution, near-infrared NIRSPEC observations of CO absorption toward six class II T Tauri stars: AA Tau, DG Tau, IQ Tau, RY Tau, CW Tau, and Haro 6-5b. {sup 12}CO overtone absorption lines originating from the circumstellar disk of each object were used to calculate line-of-sight gas column densities toward each source. We measured the gas/dust ratio as a function of disk inclination, utilizing measured visual extinctions and inclinations for each star. The majority of our sources show further evidence for a correlation between the gas/dust column density ratio and disk inclination similar to that found by Rettig etmore » al.« less

Preparation of acryloyl β-cyclodextrin-silica hybrid monolithic column and its application in pipette tip solid-phase extraction and HPLC analysis of methyl parathion and fenthion.

PubMed

Chen, Ling; Dang, Xueping; Ai, Youhong; Chen, Huaixia

2018-05-07

An acryloyl β-cyclodextrin-silica hybrid monolithic column for pipette tip solid-phase extraction and high-performance liquid chromatography determination of methyl parathion and fenthion have been prepared through a sol-gel polymerization method. The synthesis conditions, including the volume of cross-linker and the ratio of inorganic solution to organic solution, were optimized. The prepared monolithic column was characterized by thermogravimetric analysis, scanning electron microscopy and Fourier transform infrared spectroscopy. The eluent type, volume and flow rate, sample volume, flow rate, acidity and ionic strength were optimized in detail. Under the optimized conditions, a simple and sensitive pipette tip solid-phase extraction with high-performance liquid chromatography method was developed for the determination of methyl parathion and fenthion in lettuce. The method yielded a linear calibration curve in the concentration ranges of 15-400 μg/kg for methyl parathion and 20-400 μg/kg for fenthion with correlation coefficients of above 0.9957. The limits of detection were 4.5 μg/kg for methyl parathion and 6.0 μg/kg for fenthion, respectively. The recoveries of methyl parathion and fenthion spiked in lettuce ranged from 96.0 to 104.2% with relative standard deviations less than 8.4%. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

Comparative study of new shell-type, sub-2 micron fully porous and monolith stationary phases, focusing on mass-transfer resistance.

PubMed

Oláh, Erzsébet; Fekete, Szabolcs; Fekete, Jeno; Ganzler, Katalin

2010-06-04

Today sub-2 microm packed columns are very popular to conduct fast chromatographic separations. The mass-transfer resistance depends on the particle size but some practical limits exist not to reach the theoretically expected plate height and mass-transfer resistance. Another approach applies particles with shortened diffusion path to enhance the efficiency of separations. In this study a systematical evaluation of the possibilities of the separations obtained with 5 cm long narrow bore columns packed with new 2.6 microm shell particles (1.9 microm nonporous core surrounded by a 0.35 microm porous shell, Kinetex, Core-Shell), packed with other shell-type particles (Ascentis Express, Fused-Core), totally porous sub-2 microm particles and a 5 cm long narrow bore monolith column is presented. The different commercially available columns were compared by using van Deemter, Knox and kinetic plots. Theoretical Poppe plots were constructed for each column to compare their kinetic performance. Data are presented on polar neutral real-life analytes. Comparison of a low molecular weight compounds (MW=270-430) and a high molecular weight one (MW approximately 900) was conducted. This study proves that the Kinetex column packed with 2.6 microm shell particles is worthy of rivaling to sub-2 microm columns and other commercially available shell-type packings (Ascentis Express or Halo), both for small and large molecule separation. The Kinetex column offers a very flat C term. Utilizing this feature, high flow rates can be applied to accomplish very fast separations without significant loss in efficiency. Copyright 2010 Elsevier B.V. All rights reserved.

First detection of hydrogen in the β Pictoris gas disk

NASA Astrophysics Data System (ADS)

Wilson, P. A.; Lecavelier des Etangs, A.; Vidal-Madjar, A.; Bourrier, V.; Hébrard, G.; Kiefer, F.; Beust, H.; Ferlet, R.; Lagrange, A.-M.

2017-03-01

The young and nearby star β Pictoris (β Pic) is surrounded by a debris disk composed of dust and gas known to host a myriad evaporating exocomets, planetesimals and at least one planet. At an edge-on inclination, as seen from Earth, this system is ideal for debris disk studies providing an excellent opportunity to use absorption spectroscopy to study the planet forming environment. Using the Cosmic Origins Spectrograph (COS) instrument on the Hubble Space Telescope (HST) we observe the most abundant element in the disk, hydrogen, through the H I Lyman α (Ly-α) line. We present a new technique to decrease the contamination of the Ly-α line by geocoronal airglow in COS spectra. This Airglow Virtual Motion (AVM) technique allows us to shift the Ly-α line of the astrophysical target away from the contaminating airglow emission revealing more of the astrophysical line profile. This new AVM technique, together with subtraction of an airglow emission map, allows us to analyse the shape of the β Pic Ly-α emission line profile and from it, calculate the column density of neutral hydrogen surrounding β Pic. The column density of hydrogen in the β Pic stable gas disk at the stellar radial velocity is measured to be log (NH/ 1 cm2) ≪ 18.5. The Ly-α emission line profile is found to be asymmetric and we propose that this is caused by H I falling in towards the star with a bulk radial velocity of 41 ± 6 km s-1 relative to β Pic and a column density of log (NH/ 1 cm2) = 18.6 ± 0.1. The high column density of hydrogen relative to the hydrogen content of CI chondrite meteorites indicates that the bulk of the hydrogen gas does not come from the dust in the disk. This column density reveals a hydrogen abundance much lower than solar, which excludes the possibility that the detected hydrogen could be a remnant of the protoplanetary disk or gas expelled by the star. We hypothesise that the hydrogen gas observed falling towards the star arises from the dissociation of water originating from evaporating exocomets.

In-column immobilization of Cs-saturated crystalline silicotitanates using phenolic resins.

PubMed

Curi, Rodrigo F; Luca, Vittorio

2018-03-01

The in situ immobilization of granulated Cs-saturated crystalline silicotitanates (Cs-CST) in fixed-bed columns has been investigated using commercially available phenol formaldehyde (PF) resin as a binding agent. Two types of PF resin were investigated as part of this study both being prepared from resol polymer having a formaldehyde:phenol ratio of 3:1. However, one of the resol polymers had water as the primary solvent and the other ethanol. Both resol polymers were observed to completely infiltrate the space between the Cs-CST beads and also the pores within the beads themselves. PF resin monoliths prepared after curing the water-based resol at 180 °C were considerably less porous than the ethanol-based counterparts cured under the same conditions. The enhanced macroporosity of the resin prepared from the ethanol-based resol was presumably the result from enhanced gas bubble generation. Little or no micro- or mesoporosity was measured using nitrogen porosimetry. For both resins cured at 180 °C, intimate contacts with the Cs-CST beads were observed that were not modified even after complete immersion in water over long time frames. Little or no migration of Cs from Cs-CST to the resin binder was observed. The compressive strength of the Cs-CST-PF resin monoliths was measured and benchmarked against cement monoliths and was found to be two to three times higher than cement in the case of the water-based resin. Leaching of the monoliths was conducted in demineralized water at 90 °C. Normalized Cs mass losses of the order of 1.0 g/m 2 were measured after 30 days for the ethanol-based resin monoliths. For the less porous water-based monoliths, the normalized mass loss was one order of magnitude lower. The leaching of monoliths irradiated with a 2-MGy dose of γ radiation showed no difference in Cs mass loss suggesting that the ability to retain Cs of either the CST or PF resin was not affected. PF resins are capable of acting as a mechanically robust, radiation-resistant, and impermeable active secondary barrier reducing the likelihood of Cs entry into the biosphere.

Ionic liquid-regenerated macroporous cellulose monolith: Fabrication, characterization and its protein chromatography.

PubMed

Du, Kaifeng

2017-04-21

Macroporous cellulose monolith as chromatographic support was successfully fabricated from an ionic liquid dissolved cellulose solution by an emulsification method and followed by the cross-linking reaction and DEAE modification. With the physical characterization, the cellulose monolith featured by both the interconnected macropores in range of 0.5-2.5μm and the diffusion pores centered at about 10nm. Given the bimodal pore system, the monolith possessed the specific surface area of 36.4m 2 g -1 and the column permeability of about 7.45×10 -14 m 2 . After the DEAE modification, the anion cellulose monolith was evaluated for its chromatography performances. It demonstrated that the static and dynamic adsorption capacity of BSA reached about 66.7mgmL -1 and 43.9mgmL -1 at 10% breakthrough point, respectively. The results were comparable to other chromatographic adsorbent. In addition, the proteins mixture with different pI was well separated at high flow velocity (611.0cmh -1 ) and high protein recovery (over 97%), proving the macroporous cellulose monolith had excellent separation performance. In this way, the prepared cellulose monolith with bimodal pores system is expected for the potential application in high-speed chromatography. Copyright © 2017 Elsevier B.V. All rights reserved.

Preparation of hydrophilic monolithic capillary column by in situ photo-polymerization of N-vinyl-2-pyrrolidinone and acrylamide for highly selective and sensitive enrichment of N-linked glycopeptides.

PubMed

Jiang, Hao; Yuan, Huiming; Qu, Yanyan; Liang, Yu; Jiang, Bo; Wu, Qi; Deng, Nan; Liang, Zhen; Zhang, Lihua; Zhang, Yukui

2016-01-01

In this study, a novel kind of amide functionalized hydrophilic monolith was synthesized by the in situ photo-polymerization of N-vinyl-2-pyrrolidinone (NVP), acrylamide (AM), and N, N'-methylenebisacrylamide (MBA) in a UV transparent capillary, and successfully applied for hydrophilic interaction chromatography (HILIC) based enrichment of N-linked glycopeptides. With 2 μg of the tryptic digests of IgG as the sample, after enrichment, 18 glycopeptides could be identified by MALDI-TOF/TOF MS analysis. Furthermore, with the mixture of BSA and IgG digests (10,000:1, m/m) as the sample, 6 N-linked glycopeptides were unambiguously identified after enrichment, indicating the high selectivity and good specificity of such material. Moreover, such a monolithic capillary column was also applied for the N-glycosylation sites profiling of 6 μg protein digests from HeLa cells and 1 μL human serum. In total, 530 and 262 unique N-glycosylated peptides were identified, respectively, corresponding to 282 and 124N-glycoproteins, demonstrating its great potential for the large scale glycoproteomics analysis. Copyright © 2015 Elsevier B.V. All rights reserved.

Methods and system for subsurface stabilization using jet grouting

DOEpatents

Loomis, Guy G.; Weidner, Jerry R.; Farnsworth, Richard K.; Gardner, Bradley M.; Jessmore, James J.

1999-01-01

Methods and systems are provided for stabilizing a subsurface area such as a buried waste pit for either long term storage, or interim storage and retrieval. A plurality of holes are drilled into the subsurface area with a high pressure drilling system provided with a drill stem having jet grouting nozzles. A grouting material is injected at high pressure through the jet grouting nozzles into a formed hole while the drill stem is withdrawn from the hole at a predetermined rate of rotation and translation. A grout-filled column is thereby formed with minimal grout returns, which when overlapped with other adjacent grout-filled columns encapsulates and binds the entire waste pit area to form a subsurface agglomeration or monolith of grout, soil, and waste. The formed monolith stabilizes the buried waste site against subsidence while simultaneously providing a barrier against contaminate migration. The stabilized monolith can be left permanently in place or can be retrieved if desired by using appropriate excavation equipment. The jet grouting technique can also be utilized in a pretreatment approach prior to in situ vitrification of a buried waste site. The waste encapsulation methods and systems are applicable to buried waste materials such as mixed waste, hazardous waste, or radioactive waste.

Variable Circumstellar Disks of Classical Be Stars in Clusters

NASA Astrophysics Data System (ADS)

Gerhartz, C.; Bjorkman, K. S.; Bjorkman, J. E.; Wisniewski, J. P.

2016-11-01

Circumstellar disks are common among many stars, at most spectral types, and at different stages of their lifetimes. Among the near-main-sequence classical Be stars, there is growing evidence that these disks form, dissipate, and reform on timescales that differ from star to star. Using data obtained with the Large Monolithic Imager (LMI) at the Lowell Observatory Discovery Channel Telescope (DCT), along with additional complementary data obtained at the University of Toledo Ritter Observatory (RO), we have begun a long-term monitoring project of a well-studied set of galactic star clusters that are known to contain Be stars. Our goal is to develop a statistically significant sample of variable circumstellar disk systems over multiple timescales. With a robust multi-epoch study we can determine the relative fraction of Be stars that exhibit disk-loss or disk-renewal phases, and investigate the range of timescales over which these events occur. A larger sample will improve our understanding of the prevalence and nature of the disk variability, and may provide insight about underlying physical mechanisms.

A novel ionic liquid-modified organic-polymer monolith as the sorbent for in-tube solid-phase microextraction of acidic food additives.

PubMed

Wang, Ting-Ting; Chen, Yi-Hui; Ma, Jun-Feng; Hu, Min-Jie; Li, Ying; Fang, Jiang-Hua; Gao, Hao-Qi

2014-08-01

A novel ionic liquid-modified organic-polymer monolithic capillary column was prepared and used for in-tube solid-phase microextraction (SPME) of acidic food additives. The primary amino group of 1-aminopropyl-3-methylimidazolium chloride was reacted with the epoxide group of glycidyl methacrylate. The as-prepared new monomer was then copolymerized in situ with acrylamide and N,N'-methylenebisacrylamide in the presence of polyethylene glycol (PEG)-8000 and PEG-10,000 as porogens. The extraction performance of the developed monolithic sorbent was evaluated for benzoic acid, 3-hydroxybenzoic acid, cinnamic acid, 2,4-dichlorophenoxyacetic acid, and 3-(trifluoromethyl)-cinnamic acid. Such a sorbent, bearing hydrophobic and anion-exchange groups, had high extraction efficiency towards the test compounds. The adsorption capacities for the analytes dissolved in water ranged from 0.18 to 1.74 μg cm(-1). Good linear calibration curves (R(2) > 0.99) were obtained, and the limits of detection (S/N = 3) for the analytes were found to be in the range 1.2-13.5 ng mL(-1). The recoveries of five acidic food additives spiked in Coca-Cola beverage samples ranged from 85.4 % to 98.3 %, with RSD less than 6.9 %. The excellent applicability of the ionic liquid (IL)-modified monolithic column was further tested by the determination of benzoic acid content in Sprite samples, further illustrating its good potential for analyzing food additives in complex samples.

Amino Acid Bound Surfactants: A New Synthetic Family of Polymeric Monoliths Open Up Possibilities for Chiral Separations in Capillary Electrochromatography

PubMed Central

He, Jun; Wang, Xiaochun; Morrill, Mike; Shamsi, Shahab A.

2012-01-01

By combining a novel chiral amino-acid surfactant containing acryloyl amide tail, carbamate linker and leucine head group of different chain lengths with a conventional cross linker and a polymerization technique, a new “one-pot”, synthesis for the generation of amino-acid based polymeric monolith is realized. The method promises to open up the discovery of amino-acid based polymeric monolith for chiral separations in capillary electrochromatography (CEC). Possibility of enhanced chemoselectivity for simultaneous separation of ephedrine and pseudoephedrine containing multiple chiral centers, and the potential use of this amino-acid surfactant bound column for CEC and CEC coupled to mass spectrometric detection is demonstrated. PMID:22607448

DATA QUALITY OBJECTIVE SUMMARY REPORT FOR THE 105 K EAST ION EXCHANGE COLUMN MONOLITH

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

JOCHEN, R.M.

2007-08-02

The 105-K East (KE) Basin Ion Exchange Column (IXC) cells, lead caves, and the surrounding vault are to be removed as necessary components in implementing ''Hanford Federal Facility Agreement and Consent Order'' (Ecology et al. 2003) milestone M-034-32 (Complete Removal of the K East Basin Structure). The IXCs consist of six units located in the KE Basin, three in operating positions in cells and three stored in a lead cave. Methods to remove the IXCs from the KE Basin were evaluated in KBC-28343, ''Disposal of K East Basin Ion Exchange Column Evaluation''. The method selected for removal was grouting themore » six IXCs into a single monolith for disposal at the Environmental Restoration Disposal Facility (ERDF). Grout will be added to the IXC cells, IXC lead caves containing spent IXCs, and in the spaces between the lead cave walls and metal skin, to immobilize the contaminants, provide self-shielding, minimize void space, and provide a structurally stable waste form. The waste to be offered for disposal is the encapsulated monolith defined by the exterior surfaces of the vault and the lower surface of the underlying slab. This document presents summary of the data quality objective (DQO) process establishing the decisions and data required to support decision-making activities for the disposition of the IXC monolith. The DQO process is completed in accordance with the seven-step planning process described in EPA QA/G-4, ''Guidance for the Data Quality Objectives Process'', which is used to clarify and study objectives; define the appropriate type, quantity, and quality of data; and support defensible decision-making. The DQO process involves the following steps: (1) state the problem; (2) identify the decision; (3) identify the inputs to the decision; (4) define the boundaries of the study; (5) develop a decision rule (DR); (6) specify tolerable limits on decision errors; and (7) optimize the design for obtaining data.« less

Cascaded Brillouin lasing in monolithic barium fluoride whispering gallery mode resonators

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

Lin, Guoping, E-mail: guoping.lin@femto-st.fr; Diallo, Souleymane; Saleh, Khaldoun

2014-12-08

We report the observation of stimulated Brillouin scattering and lasing at 1550 nm in barium fluoride (BaF{sub 2}) crystal. Brillouin lasing was achieved with ultra-high quality (Q) factor monolithic whispering gallery mode mm-size disk resonators. Overmoded resonators were specifically used to provide cavity resonances for both the pump and all Brillouin Stokes waves. Single and multiple Brillouin Stokes radiations with frequency shift ranging from 8.2 GHz up to 49 GHz have been generated through cascaded Brillouin lasing. BaF{sub 2} resonator-based Brillouin lasing can find potential applications for high-coherence lasers and microwave photonics.

Gaseous Inner Disks

DTIC Science & Technology

2007-01-01

planetary systems (i.e., planetary masses, orbital radii, and eccentricities). For example, the lifetime of gas in the inner disk (limited by accretion onto...2002). Thus, understanding how inner disks dissipate may impact our understanding of the origin of planetary orbital radii. Similarly, residual gas...which the orbiting giant planet carves out a “ gap ” in the disk . Low column densities would also be characteristic of a dissipating disk . Thus, we should

Recent advances in micro-scale and nano-scale high-performance liquid-phase chromatography for proteome research.

PubMed

Tao, Dingyin; Zhang, Lihua; Shan, Yichu; Liang, Zhen; Zhang, Yukui

2011-01-01

High-performance liquid chromatography-electrospray ionization tandem mass spectrometry (HPLC-ESI-MS-MS) is regarded as one of the most powerful techniques for separation and identification of proteins. Recently, much effort has been made to improve the separation capacity, detection sensitivity, and analysis throughput of micro- and nano-HPLC, by increasing column length, reducing column internal diameter, and using integrated techniques. Development of HPLC columns has also been rapid, as a result of the use of submicrometer packing materials and monolithic columns. All these innovations result in clearly improved performance of micro- and nano-HPLC for proteome research.

Preparation of well-controlled three-dimensional skeletal hybrid monoliths via thiol-epoxy click polymerization for highly efficient separation of small molecules in capillary liquid chromatography.

PubMed

Lin, Hui; Chen, Lianfang; Ou, Junjie; Liu, Zhongshan; Wang, Hongwei; Dong, Jing; Zou, Hanfa

2015-10-16

Two kinds of hybrid monoliths were first prepared via thiol-epoxy click polymerization using a multi-epoxy monomer, octaglycidyldimethylsilyl POSS (POSS-epoxy), and two multi-thiols, trimethylolpropanetris(3-mercaptopropionate) (TPTM) and pentaerythritoltetrakis(3-mercaptopropionate) (PTM), respectively, as the precursors. The resulting two hybrid monoliths (assigned as POSS-epoxy-TPTM and POSS-epoxy-PTM) not only possessed high thermal, mechanical and chemical stabilities, but also exhibited well-controlled 3D skeletal microstructure and high efficiency in capillary liquid chromatography (cLC) separation of small molecules. The highest column efficiency reached 182,700N/m (for butylbenzene) on the monolith POSS-epoxy-PTM at the velocity of 0.75mm/s. Furthermore, the hybrid monolith POSS-epoxy-PTM was successfully applied for cLC separations of various samples, not only standard compounds such as alkylbenzenes, PAHs, phenols and dipeptides, as well as intact proteins, but also complex samples of EPA 610 and BSA digest. Copyright © 2015 Elsevier B.V. All rights reserved.

Preparation of a thermoresponsive polymer grafted polystyrene monolithic capillary for the separation of bioactive compounds.

PubMed

Koriyama, Takuya; Asoh, Taka-Aki; Kikuchi, Akihiko

2016-11-01

To develop aqueous microseparation columns for bioactive compounds, a thermoresponsive polymer grafted polymer monolith was prepared inside silica capillaries having an I.D. of 100μm by polymerization of styrene (St) with m/p-divinylbenzene (DVB) in the presence of polydimethylsiloxane as porogen, followed by surface-initiated atom transfer radical polymerization (SI-ATRP) of N-isopropylacrylamide (NIPAAm). SEM analysis indicated that the resulting poly(N-isopropylacrylamide) (PNIPAAm) grafted polystyrene monolith had a consecutive three-dimensionally interconnected structure and through-pores, similar to the base polystyrene (PSt) monolith. The elution behavior of steroids with different hydrophobicity was evaluated using micro-high-performance liquid chromatography in sole aqueous mobile phase. Temperature dependent interaction changes were observed between steroids and the PNIPAAm modified surfaces. Furthermore, the interaction between bioactive compounds and the PNIPAAm grafted PSt surfaces was controlled and eventually separate these molecules with different hydrophobicities by simple temperature modulation in aqueous environment. The PNIPAAm grafted PSt monolithic capillary showed improved separation properties of bioactive compounds, compared with a PNIPAAm grafted hollow capillary in aqueous environment. Copyright © 2016 Elsevier B.V. All rights reserved.

Effect of chromatographic conditions and plasmid DNA size on the dynamic binding capacity of a monolithic support.

PubMed

Bicho, Diana; Sousa, Ângela; Sousa, Fani; Queiroz, João; Tomaz, Cãndida

2014-09-01

DNA therapies are becoming recognized alternatives for the treatment and prevention of severe pathologies. Although most current trials have used plasmids <10 kbp, in the future larger plasmids would be required. The purpose of this work was to study the chromatographic behavior of nongrafted carbonyldiimidazole monolithic disks using plasmids with different sizes under hydrophobic conditions. Thereunto, the purification of several plasmids was performed. Higher size plasmids needed lower ammonium sulfate concentration, due to the greater number of interactions between the plasmids and monolith. The dynamic binding capacity experiments for the different plasmids revealed a lower capacity for bigger plasmids. It was also verified that the increase of salt concentration from 2.5 to 3 M of ammonium sulfate increased the capacity. At the highest salt concentration, a slight improvement in the capacity using lower flow rate was observed, possibly due to compaction of plasmid molecules and its better organization on the monolith channels. Finally, a low pH also had a positive effect on the capacity. So, this monolithic support proved to be appropriate to purify the supercoiled isoform of different plasmids with different sizes, providing a valuable instrument as a purification technique. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Iminodiacetic acid functionalised organopolymer monoliths: application to the separation of metal cations by capillary high-performance chelation ion chromatography.

PubMed

Moyna, Áine; Connolly, Damian; Nesterenko, Ekaterina; Nesterenko, Pavel N; Paull, Brett

2013-03-01

Lauryl methacrylate-co-ethylene dimethacrylate monoliths were polymerised within fused silica capillaries and subsequently photo-grafted with varying amounts of glycidyl methacrylate (GMA). The grafted monoliths were then further modified with iminodiacetic acid (IDA), resulting in a range of chelating ion-exchange monoliths of increasing capacity. The IDA functional groups were attached via ring opening of the epoxy group on the poly(GMA) structure. Increasing the amount of attached poly(GMA), via photo-grafting with increasing concentrations of GMA, from 15 to 35%, resulted in a proportional and controlled increase in the complexation capacity of the chelating monoliths. Scanning capacitively coupled contactless conductivity detection (sC(4)D) was used to characterise and verify homogenous distribution of the chelating ligand along the length of the capillaries non-invasively. Chelation ion chromatographic separations of selected transition and heavy metals were carried out, with retention factor data proportional to the concentration of grafted poly(GMA). Average peak efficiencies of close to 5,000 N/m were achieved, with the isocratic separation of Na, Mg(II), Mn(II), Co(II), Cd(II) and Zn(II) possible on a 250-mm-long monolith. Multiple monolithic columns produced to the same recipes gave RSD data for retention factors of <15% (averaged for several metal ions). The monolithic chelating ion-exchanger was applied to the separation of alkaline earth and transition metal ions spiked in natural and potable waters.

Automatic and integrated micro-enzyme assay (AIμEA) platform for highly sensitive thrombin analysis via an engineered fluorescence protein-functionalized monolithic capillary column.

PubMed

Lin, Lihua; Liu, Shengquan; Nie, Zhou; Chen, Yingzhuang; Lei, Chunyang; Wang, Zhen; Yin, Chao; Hu, Huiping; Huang, Yan; Yao, Shouzhuo

2015-04-21

Nowadays, large-scale screening for enzyme discovery, engineering, and drug discovery processes require simple, fast, and sensitive enzyme activity assay platforms with high integration and potential for high-throughput detection. Herein, a novel automatic and integrated micro-enzyme assay (AIμEA) platform was proposed based on a unique microreaction system fabricated by a engineered green fluorescence protein (GFP)-functionalized monolithic capillary column, with thrombin as an example. The recombinant GFP probe was rationally engineered to possess a His-tag and a substrate sequence of thrombin, which enable it to be immobilized on the monolith via metal affinity binding, and to be released after thrombin digestion. Combined with capillary electrophoresis-laser-induced fluorescence (CE-LIF), all the procedures, including thrombin injection, online enzymatic digestion in the microreaction system, and label-free detection of the released GFP, were integrated in a single electrophoretic process. By taking advantage of the ultrahigh loading capacity of the AIμEA platform and the CE automatic programming setup, one microreaction column was sufficient for many times digestion without replacement. The novel microreaction system showed significantly enhanced catalytic efficiency, about 30 fold higher than that of the equivalent bulk reaction. Accordingly, the AIμEA platform was highly sensitive with a limit of detection down to 1 pM of thrombin. Moreover, the AIμEA platform was robust and reliable to detect thrombin in human serum samples and its inhibition by hirudin. Hence, this AIμEA platform exhibits great potential for high-throughput analysis in future biological application, disease diagnostics, and drug screening.

Gas in the Terrestrial Planet Region of Disks: CO Fundamental Emission from T Tauri Stars

DTIC Science & Technology

2003-06-01

planetary systems: protoplanetary disks — stars: variables: other 1. INTRODUCTION As the likely birthplaces of planets, the inner regions of young...both low column density regions, such as disk gaps , and temperature inversion regions in disk atmospheres can produce significant emission. The esti...which planetary systems form. The moti- vation to study inner disks is all the more intense today given the discovery of planets outside the solar system

Miniaturized monolithic columns for the electrochromatographic separation and SERS detection of molecules of exobiological interest

NASA Astrophysics Data System (ADS)

Carbonnier, Benjamin; Guerrouache, Mohamed

Development of miniaturized separation and detection media represents one of the major challenges in the field of modern analytical chemistry dedicated to space exploration. To date, gas chromatography-mass spectrometry has been selected as the method of choice for exobiology flight experiments for seeking for organic molecules and especially potential chemical indicators of life. [1] Liquid phase separation methods have also been developed with for instance, the so-called Mars Organic Analyzer (MOA) capillary electrophoresis (CE) microchip.[2] Although CE offers the advantages of easy miniaturization and high separation efficiency it suffers from a lack of selectivity towards a broad range of analytes with varied chemical nature. In this respect, we propose the use of capillary columns filled with monolithic stationary phases for the electrochromatographic separation of organic molecules of exobiology interest. Polymer monoliths have attracted a great deal of interest in analytical science over the last years as (electro)chromatographic stationary phases [3], immunosensors [4]. Beyond the intrinsic properties of monolithic polymers, i.e. fast mass transport between the monolithic support and the surrounding fluid and high permeability, other major advantages are their easy in situ preparation and tuning of surface functionality. Indeed, monoliths can be simply prepared through free radical copolymerization of a homogeneous mixture made of monomers, cross-linkers, porogenic solvents and initiator. UV-initiation process has been exploited to the synthesis of a discrete section of monolith as a flow-through active element within the confines of micro channels [5,6] while two-step strategies have been reported for the design of varied adsorbent starting with a generic monolith [7,8]. Although a nearly limitless range of monolithic supports can be prepared by this traditional method, the resulting monoliths exhibit unique function. In this contribution, we describe an elegant strategy for preparing multifunctional monoliths through spatially controlled surface functionalization.[9] Photochemical initiation affords spatial control over the reaction site, i.e. site-specific immobilization of ligands on the pore surface of the monolith. Hydrophobic and hydrophilic molecular entities were successfully grafted and the obtained monoliths were applied to electrochromatographic separation application under reversed-phase and hydrophilic interaction electrochromatography modes, respectively. The panel of successfully analyzed analytes ranges from hydrophobic polycyclic aromatic hydrocarbons to life markers such as amino acids and peptides. Our approach was extended to the local design of chelating interface for the site-specific immobilisation of gold nanoparticles. Taking advantage of the unique properties of supported nano-gold, it was possible to perform surface enhanced Raman spectroscopy (SERS) sensing of organic molecules at the sub-nanomolar level. This work is funded by the French Space Agency (CNES) References [1] M.C. Pietrogrande, M.G. Zampolli, F. Dondi, C. Szopa, R. Sternberg, A. Buch, J.F. Raulin, J. Chromatogr. A 1071 (2005) 255. [2] A. M. Stockton, T.M. Chiesl, J.M. Scherer, R. A. Mathies, Anal. Chem. 81 (2009) 790 [3] B. Carbonnier, M. Guerrouache, R. Denoyel, M. C. Millot, J. Sep. Sci. 30 (2007) 3000. [4] J.k. Liu, C.F. Chen, C.W. Chang, D.L. DeVoe, Biosensors Bioelectron. 26 (2010) 182. [5] J. Krenkova, F. Svec, J. Sep. Sci. 32 (2009) 706. [6] F. Svec, J. Chromatogr. B 841 (2004) 52 [7] M. Guerrouache, M. C. Millot, B. Carbonnier, Macromol. Rapid. Commun, 30 (2009) 109. [8] M. Guerrouache, B. Carbonnier, C. Vidal-Madjar, M.C. Millot, J. Chromatogr A, 1149 (2007) 368. [9] M. Guerrouache, S. Mahouche Chergui, M.M. Chehimi, B. Carbonnier. Chem. Commun. 48 (2012) 7486.

An easily regenerable enzyme reactor prepared from polymerized high internal phase emulsions

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

Ruan, Guihua, E-mail: guihuaruan@hotmail.com; Guangxi Collaborative Innovation Center for Water Pollution Control and Water Safety in Karst Area, Guilin University of Technology, Guilin 541004; Wu, Zhenwei

A large-scale high-efficient enzyme reactor based on polymerized high internal phase emulsion monolith (polyHIPE) was prepared. First, a porous cross-linked polyHIPE monolith was prepared by in-situ thermal polymerization of a high internal phase emulsion containing styrene, divinylbenzene and polyglutaraldehyde. The enzyme of TPCK-Trypsin was then immobilized on the monolithic polyHIPE. The performance of the resultant enzyme reactor was assessed according to the conversion ability of N{sub α}-benzoyl-L-arginine ethyl ester to N{sub α}-benzoyl-L-arginine, and the protein digestibility of bovine serum albumin (BSA) and cytochrome (Cyt-C). The results showed that the prepared enzyme reactor exhibited high enzyme immobilization efficiency and fast andmore » easy-control protein digestibility. BSA and Cyt-C could be digested in 10 min with sequence coverage of 59% and 78%, respectively. The peptides and residual protein could be easily rinsed out from reactor and the reactor could be regenerated easily with 4 M HCl without any structure destruction. Properties of multiple interconnected chambers with good permeability, fast digestion facility and easily reproducibility indicated that the polyHIPE enzyme reactor was a good selector potentially applied in proteomics and catalysis areas. - Graphical abstract: Schematic illustration of preparation of hypercrosslinking polyHIPE immobilized enzyme reactor for on-column protein digestion. - Highlights: • A reactor was prepared and used for enzyme immobilization and continuous on-column protein digestion. • The new polyHIPE IMER was quite suit for protein digestion with good properties. • On-column digestion revealed that the IMER was easy regenerated by HCl without any structure destruction.« less

Approximate transient and long time limit solutions for the band broadening induced by the thin sidewall-layer in liquid chromatography columns.

PubMed

Broeckhoven, Ken; Desmet, Gert

2007-11-16

Using a combination of both analytical and numerical techniques, approximate analytical expressions have been established for the transient and long time limit band broadening, originating from the presence of a thin disturbed sidewall layer in liquid chromatography columns, including packed, monolithic as well as microfabricated columns. The established expressions can be used to compare the importance of a thin disturbed sidewall layer with that of other radial heterogeneity effects (such as transcolumn packing density variations due to the relief of packing stresses). The expressions are independent of the actual velocity profile inside the layer as long as the disturbed sidewall layer occupies less than 2.5% of the column width.

Tentacle-type immobilized metal affinity cryogel for invertase purification from Saccharomyces cerevisiae.

PubMed

Çetin, Kemal; Perçin, Işık; Denizli, Fatma; Denizli, Adil

2017-11-01

The aim of this study is to investigate the usability of cryogel columns for the purification of invertase from Saccharomyces cerevisiae. Poly(2-hydroxyethyl methacrylate) monolithic columns were produced via cryogelation. Ester groups of the poly(2-hydroxyethyl methacrylate) structure were then converted to imine groups by the reaction with poly(ethylene imine) in the presence of NaHCO 3 . Transition metal ions, Cu(II), Co(II), and Ni(II), were chelated on the PEI-modified cryogel columns. Purification of invertase from natural source namely S. cerevisiae was also studied, and the purification fold values were obtained as 41.350, 44.714, and 30.302 for Cu(II)-chelated, Co(II)-chelated, and Ni(II)-chelated PHEMA/PEI columns, respectively.

Professional Resources

ERIC Educational Resources Information Center

Haddix, Marcelle M.

2015-01-01

In educational research, policies and practices, African American male youth are often portrayed as a monolithic demographic of uneducable, criminalized, deviant students. This column reviews the works of two African American male scholars, Tyrone D. Howard's (2014) "Black Male(d)" and David E. Kirkland's (2013) "A Search…

Structure for monolithic optical circuits

NASA Technical Reports Server (NTRS)

Evanchuk, Vincent L. (Inventor)

1984-01-01

A method for making monolithic optical circuits, with related optical devices as required or desired, on a supporting surface (10) consists of coating the supporting surface with reflecting metal or cladding resin, spreading a layer of liquid radiation sensitive plastic (12) on the surface, exposing the liquid plastic with a mask (14) to cure it in a desired pattern of light conductors (16, 18, 20), washing away the unexposed liquid plastic, and coating the conductors thus formed with reflective metal or cladding resin. The index of refraction for the cladding (22) is selected to be lower than for the conductors so that light in the conductors will be reflected by the interface with the cladding. For multiple level conductors, as where one conductor must cross over another, the process may be repeated to fabricate a bridge with columns (24, 26) of conductors to the next level, and conductor (28) between the columns. For more efficient transfer of energy over the bridge, faces at 45.degree. may be formed to reflect light up and across the bridge.

Warm H2O and OH Disk Emission in V1331 Cyg

NASA Astrophysics Data System (ADS)

Doppmann, Greg W.; Najita, Joan R.; Carr, John S.; Graham, James R.

2011-09-01

We present high-resolution (R = 24, 000) L-band spectra of the young intermediate-mass star V1331 Cyg obtained with NIRSPEC on the Keck II telescope. The spectra show strong, rich emission from water and OH that likely arises from the warm surface region of the circumstellar disk. We explore the use of the new BT2 water line list in fitting the spectra, and we find that it does a much better job than the well-known HITRAN water line list in the observed wavelength range and for the warm temperatures probed by our data. By comparing the observed spectra with synthetic disk emission models, we find that the water and OH emission lines have similar widths (FWHM ~= 18 km s-1). If the line widths are set by disk rotation, the OH and water emission lines probe a similar range of disk radii in this source. The water and OH emission are consistent with thermal emission for both components at a temperature ~1500 K. The column densities of the emitting water and OH are large, ~1021 cm-2 and ~1020 cm-2, respectively. Such a high column density of water is more than adequate to shield the disk midplane from external UV irradiation in the event of complete dust settling out of the disk atmosphere, enabling chemical synthesis to continue in the midplane despite a harsh external UV environment. The large OH-to-water ratio is similar to expectations for UV irradiated disks, although the large OH column density is less easily accounted for. Data presented herein were obtained at the W. M. Keck Observatory from telescope time allocated to the National Aeronautics and Space Administration through the agency's scientific partnership with the California Institute of Technology and the University of California. The Observatory was made possible by the generous financial support of the W. M. Keck Foundation.

In-tube solid-phase microextraction based on NH2-MIL-53(Al)-polymer monolithic column for online coupling with high-performance liquid chromatography for directly sensitive analysis of estrogens in human urine.

PubMed

Luo, Xialin; Li, Gongke; Hu, Yufei

2017-04-01

In this work, a novel NH 2 -MIL-53(Al) incorporated poly(styrene-divinylbenzene-methacrylic acid) (poly(St-DVB-MAA)) monolith was prepared via chemical fabrication. Moreover, it has been efficiently applied to the in-tube solid-phase microextraction (SPME) for online coupling with high-performance liquid chromatography (HPLC) to the direct determination of five estrogens in human urine samples. The NH 2 -MIL-53(Al)-polymer monolith was suitable for in-tube SPME owing to its good permeability, high extraction efficiency, chemical stability, good reproducibility and long lifetime. The extraction conditions including extraction solvent, pH of sample solution, flow rate of extraction and desorption, and desorption volume were investigated. Under the optimum conditions, the enrichment factors were 180-304 and saturated amounts of extraction were 2326-21393 pmol for estriol, 17β-estradiol, estrone, ethinyl estradiol and progesterone, respectively. The adsorption mechanism was also explored which contributed to its strong extraction to target compounds. The proposed method had low limit of detection (2.0-40ng/L) and good linearity (with R 2 between 0.9908 and 0.9978). Four endogenous estrogens were detected in urine samples and the recoveries of all five analytes were ranged from 75.1-120% with relative standard deviations (RSDs) less than 8.7%. The results showed that the proposed online SPME-HPLC method based on NH 2 -MIL-53(Al)-polymer monolithic column was highly sensitive for directly monitoring trace amount of estrogens in human urine sample. Copyright © 2016 Elsevier B.V. All rights reserved.

Physical reconstruction of packed beds and their morphological analysis: core-shell packings as an example.

PubMed

Bruns, Stefan; Tallarek, Ulrich

2011-04-08

We report a fast, nondestructive, and quantitative approach to characterize the morphology of packed beds of fine particles by their three-dimensional reconstruction from confocal laser scanning microscopy images, exemplarily shown for a 100μm i.d. fused-silica capillary packed with 2.6μm-sized core-shell particles. The presented method is generally applicable to silica-based capillary columns, monolithic or particulate, and comprises column pretreatment, image acquisition, image processing, and statistical analysis of the image data. It defines a unique platform for fundamental comparisons of particulate and monolithic supports using the statistical measures derived from their reconstructions. Received morphological data are column cross-sectional porosity profiles and chord length distributions from the interparticle macropore space, which are a descriptor of local density and can be characterized by a simplified k-gamma distribution. This distribution function provides a parameter of location and a parameter of dispersion which can be correlated to individual chromatographic band broadening processes (i.e., to transchannel and short-range interchannel contributions to eddy dispersion, respectively). Together with the transcolumn porosity profile the presented approach allows to analyze and quantify the packing microstructure from pore to column scale and therefore holds great promise in a comparative study of packing conditions and particle properties, particularly for characterizing and minimizing the packing process-specific heterogeneities in the final bed structure. Copyright © 2011 Elsevier B.V. All rights reserved.

[Monolithic column-gold composite substrate preparation and application to SERS detection of pigment].

PubMed

Xie, Yun-Fei; Li, Yan; Yu, Hui; Qian, He; Yao, Wei-Rong

2014-03-01

In the present study, we developed a novel SERS substrate with the porous monolith material combined with classic gold nanoparticles, and erythrosine as the research object, by adjusting the different experimental conditions for optimal SERS enhancements, including system pH and mixing time, and ultimately selected the optimum pH value 5.06 and mixing time 25 min. Compared with the traditional gold plastic substrate enhancement effect, the experimental conditions were applied to the monolith substrate SERS detection of dye erythrosine, different concentrations of samples were used for erythrosine SERS detection, and the detection limit reached 0.1 g x mL(-1). The method uses the payload of gold nanoparticles in mesoporous materials to effectively enhance the SERS signal. And this method has the advantages of simpleness and good stability, which provides a favorable theoretical basis for the rapid prohibited colorings screening.

Novel polymeric monolith materials with a β-cyclodextrin-graphene composite for the highly selective extraction of methyl jasmonate.

PubMed

Yu, Xinhong; Ling, Xu; Zou, Li; Chen, Zilin

2017-04-01

A novel polymeric monolith column with a  β-cyclodextrin-graphene composite was prepared for extraction of methyl jasmonate. A simple, sensitive, and effective polymeric monolith microextraction with high-performance liquid chromatography method has been presented for the determination. To carry out the best microextraction efficiency, several parameters such as sample flow rate, sample volume, and sample pH value were systematically optimized. In addition, the method validation showed a wide linear range of 5-2000 ng/mL, with a good linearity and low limits of detection for methyl jasmonate. The proposed method was successfully applied for the determination of methyl jasmonate in wintersweet flowers with recoveries of 90.67%. The result was confirmed by high-performance liquid chromatography with mass spectrometry. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Quantitative determination of p-aminosalicylic acid and its degradation product m-aminophenol in pellets by ion-pair high-performance liquid chromatography applying the monolithic Chromolith Speedrod RP-18e column.

PubMed

Vasbinder, E; Van der Weken, G; Vander Heyden, Y; Baeyens, W R G; Debunne, A; Remon, J P; García-Campaña, A M

2004-01-01

An ion-pair high performance liquid chromatographic method was developed for the simultaneous determination of p-aminosalicylic acid (PAS) and its degradation product m-aminophenol (MAP) in a newly developed multiparticular drug delivery system. Owing to the concentration differences of PAS and MAP, acetanilide and sulfanilic acid were used as internal standards, respectively. The separation was performed on a Chromolith SpeedROD RP-18e column, a new packing material consisting of monolithic rods of highly porous silica. The mobile phase composition was of 20 mm phosphate buffer, 20 mm tetrabutylammonium hydrogen sulphate and 16% (v/v) methanol adjusted to pH 6.8, at a flow-rate of 1.0 mL/min, resulting in a run-time of about 6 min. Detection was by UV at 233 nm. The method was validated and proved to be useful for stability testing of the new dosage form. Separation efficiency was compared between the new packing material Chromolith SpeedROD RP-18e and the conventional reversed-phase cartridge LiChroCART 125-4 (5 microm). A robustness test was carried out on both columns and different separation parameters (retention, resolution, run time, temperature) were determined. Copyright 2004 John Wiley & Sons, Ltd.

Temperature-Modulated Array High-Performance Liquid Chromatography

PubMed Central

Premstaller, Andreas; Xiao, Wenzhong; Oberacher, Herbert; O'Keefe, Matthew; Stern, David; Willis, Thomas; Huber, Christian G.; Oefner, Peter J.

2001-01-01

Using novel monolithic poly(styrene-divinylbenzene) capillary columns with an internal diameter of 0.2 mm, we demonstrate for the first time the feasibility of constructing high-performance liquid chromatography arrays for the detection of mutations by heteroduplex analysis under partially denaturing conditions. In one embodiment, such an array can be used to analyze one sample simultaneously at different temperatures to maximize the detection of mutations in DNA fragments containing multiple discrete melting domains. Alternatively, one may inject different samples onto columns kept at the same effective temperature. Further improvements in throughput can be obtained by means of laser-induced fluorescence detection and the differential labeling of samples with up to four different fluorophores. Major advantages of monolithic capillary high-performance liquid chromatographic arrays over their capillary electrophoretic analogs are the chemical inertness of the poly(styrene-divinylbenzene) stationary phase, the physical robustness of the column bed due to its covalent linkage to the inner surface of the fused silica capillary, and the feasibility to modify the stationary phase thereby allowing the separation of compounds not only on the principle of size exclusion, but also adsorption, distribution, and ion exchange. Analyses times are on the order of a few minutes and turnaround time is extremely short as there is no need for the replenishment of the separation matrix between runs. PMID:11691859

Rapid determination of amino acids in biological samples using a monolithic silica column.

PubMed

Song, Yanting; Funatsu, Takashi; Tsunoda, Makoto

2012-05-01

A high-performance liquid chromatography method in which fluorescence detection is used for the simultaneous determination of 21 amino acids is proposed. Amino acids were derivatized with 4-fluoro-7-nitro-2,1,3-benzoxadiazole (NBD-F) and then separated on a monolithic silica column (MonoClad C18-HS, 150 mm×3 mm i.d.). A mixture of 25 mM citrate buffer containing 25 mM sodium perchlorate (pH 5.5) and acetonitrile was used as the mobile phase. We found that the most significant factor in the separation was temperature, and a linear temperature gradient from 30 to 49°C was used to control the column temperature. The limits of detection and quantification for all amino acids ranged from 3.2 to 57.2 fmol and 10.8 to 191 fmol, respectively. The calibration curves for the NBD-amino acid had good linearity within the range of 40 fmol to 40 pmol when 6-aminocaproic acid was used as an internal standard. Using only conventional instruments, the 21 amino acids could be analyzed within 10 min. This method was found to be suitable for the quantification of the contents of amino acids in mouse plasma and adrenal gland samples.

Coupling of metal-organic frameworks-containing monolithic capillary-based selective enrichment with matrix-assisted laser desorption ionization-time-of-flight mass spectrometry for efficient analysis of protein phosphorylation.

PubMed

Li, Daojin; Yin, Danyang; Chen, Yang; Liu, Zhen

2017-05-19

Protein phosphorylation is a major post-translational modification, which plays a vital role in cellular signaling of numerous biological processes. Mass spectrometry (MS) has been an essential tool for the analysis of protein phosphorylation, for which it is a key step to selectively enrich phosphopeptides from complex biological samples. In this study, metal-organic frameworks (MOFs)-based monolithic capillary has been successfully prepared as an effective sorbent for the selective enrichment of phosphopeptides and has been off-line coupled with matrix-assisted laser desorption ionization-time-of-flight mass spectrometry (MALDI-TOF MS) for efficient analysis of phosphopeptides. Using š-casein as a representative phosphoprotein, efficient phosphorylation analysis by this off-line platform was verified. Phosphorylation analysis of a nonfat milk sample was also demonstrated. Through introducing large surface areas and highly ordered pores of MOFs into monolithic column, the MOFs-based monolithic capillary exhibited several significant advantages, such as excellent selectivity toward phosphopeptides, superb tolerance to interference and simple operation procedure. Because of these highly desirable properties, the MOFs-based monolithic capillary could be a useful tool for protein phosphorylation analysis. Copyright © 2016 Elsevier B.V. All rights reserved.

Arginine homopeptides for plasmid DNA purification using monolithic supports.

PubMed

Cardoso, Sara; Sousa, Ângela; Queiroz, João A; Azzoni, Adriano R; Sousa, Fani

2018-06-15

Purification of plasmid DNA targeting therapeutic applications still presents many challenges, namely on supports and specific ligand development. Monolithic supports have emerged as interesting approaches for purifying pDNA due to its excellent mass transfer properties and higher binding capacity values. Moreover, arginine ligands were already described to establish specific and preferential interactions with pDNA. Additionally, some studies revealed the ability of arginine based cationic peptides to condense plasmid DNA, which increased lengthening can result in strongest interactions with higher binding capacities for chromatographic purposes of large molecules such as pDNA. In this work, arginine homopeptides were immobilized in monolithic supports and their performance was evaluated and compared with a single arginine monolithic column regarding supercoiled (sc) plasmid DNA purification. Specific interactions of arginine based peptides with several nucleic acids present in a clarified Escherichia coli lysate sample showed potential for the sc pDNA purification. Effectively, the immobilization of the arginine homopeptides became more functional compared with the single arginine amino acid, showing higher binding capacities, which was also reflected in the intensity of the interactions. The combination of structural versatilities of monoliths with the specificity of arginine peptides raised as a promising strategy for sc pDNA purification. Copyright © 2018 Elsevier B.V. All rights reserved.

Depletion of human serum albumin in embryo culture media for in vitro fertilization using monolithic columns with immobilized antibodies.

PubMed

Tarasova, Irina A; Lobas, Anna A; Černigoj, Urh; Solovyeva, Elizaveta M; Mahlberg, Barbara; Ivanov, Mark V; Panić-Janković, Tanja; Nagy, Zoltan; Pridatchenko, Marina L; Pungor, Andras; Nemec, Blaž; Vidic, Urška; Gašperšič, Jernej; Krajnc, Nika Lendero; Vidič, Jana; Gorshkov, Mikhail V; Mitulović, Goran

2016-09-01

Affinity depletion of abundant proteins such as HSA is an important stage in routine sample preparation prior to MS/MS analysis of biological samples with high range of concentrations. Due to the charge competition effects in electrospray ion source that results in discrimination of the low-abundance species, as well as limited dynamic range of MS/MS, restricted typically by three orders of magnitude, the identification of low-abundance proteins becomes a challenge unless the sample is depleted from high-concentration compounds. This dictates a need for developing efficient separation technologies allowing fast and automated protein depletion. In this study, we performed evaluation of a novel immunoaffinity-based Convective Interaction Media analytical columns (CIMac) depletion column with specificity to HSA (CIMac-αHSA). Because of the convective flow-through channels, the polymethacrylate CIMac monoliths afford flow rate independent binding capacity and resolution that results in relatively short analysis time compared with traditional chromatographic supports. Seppro IgY14 depletion kit was used as a benchmark to control the results of depletion. Bottom-up proteomic approach followed by label-free quantitation using normalized spectral indexes were employed for protein quantification in G1/G2 and cleavage/blastocyst in vitro fertilization culture media widely utilized in clinics for embryo growth in vitro. The results revealed approximately equal HSA level of 100 ± 25% in albumin-enriched fractions relative to the nondepleted samples for both CIMac-αHSA column and Seppro kit. In the albumin-free fractions concentrated 5.5-fold by volume, serum albumin was identified at the levels of 5-30% and 20-30% for the CIMac-αHSA and Seppro IgY14 spin columns, respectively. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Characterization of the efficiency of microbore liquid chromatography columns by van Deemter and kinetic plot analysis.

PubMed

Hetzel, Terence; Loeker, Denise; Teutenberg, Thorsten; Schmidt, Torsten C

2016-10-01

The efficiency of miniaturized liquid chromatography columns with inner diameters between 200 and 300 μm has been investigated using a dedicated micro-liquid chromatography system. Fully porous, core-shell and monolithic commercially available stationary phases were compared applying van Deemter and kinetic plot analysis. The sub-2 μm fully porous as well as the 2.7 μm core-shell particle packed columns showed superior efficiency and similar values for the minimum reduced plate heights (2.56-2.69) before correction for extra-column contribution compared to normal-bore columns. Moreover, the influence of extra-column contribution was investigated to demonstrate the difference between apparent and intrinsic efficiency by replacing the column by a zero dead volume union to determine the band spreading caused by the system. It was demonstrated that 72% of the intrinsic efficiency could be reached. The results of the kinetic plot analysis indicate the superior performance of the sub-2 μm fully porous particle packed column for ultra-fast liquid chromatography. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Supercoiled plasmid DNA purification by integrating membrane technology with a monolithic chromatography.

PubMed

Nunes, Catherine; Sousa, Angela; Nunes, José C; Morão, António M; Sousa, Fani; Queiroz, João A

2014-06-01

The present study describes the integration of membrane technology with monolithic chromatography to obtain plasmid DNA with high quality. Isolation and clarification of plasmid DNA lysate were first conducted by a microfiltration step, by using a hydrophilic nylon microfiltration membrane, avoiding the need of centrifugation. For the total elimination of the remaining impurities, a suitable purification step is required. Monolithic stationary phases have been successfully applied as an alternative to conventional supports. Thus, the sample recovered from the membrane process was applied into a nongrafted CarbonylDiImidazole disk. Throughout the global procedure, a reduced level of impurities such as proteins and RNA was obtained, and no genomic DNA was detectable in the plasmid DNA sample. The chromatographic process demonstrated an efficient performance on supercoiled plasmid DNA purity and recovery (100 and 84.44%, respectively). Thereby, combining the membrane technology to eliminate some impurities from lysate sample with an efficient chromatographic strategy to purify the supercoiled plasmid DNA arises as a powerful approach for industrial-scale systems aiming at plasmid DNA purification. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Facet joint geometry and intervertebral disk degeneration in the L5-S1 region of the vertebral column in German Shepherd dogs.

PubMed

Seiler, Gabriela S; Häni, Hansjürg; Busato, André R; Lang, Johann

2002-01-01

To evaluate the possible association between facet joint geometry and intervertebral disk degeneration in German Shepherd Dogs. 25 German Shepherd Dogs and 11 control dogs of similar body weight and condition. Facet joint angles in the caudal portion of the lumbar region of the vertebral column (L5-S1) were measured by use of computed tomography, and the intervertebral discs were evaluated microscopically. The relationship between facet joint geometry and disk degeneration was evaluated by use of statistical methods. German Shepherd Dogs had significantly more facet joint tropism than control dogs, but an association with disk degeneration was not found. However, German Shepherd Dogs had a different facet joint conformation, with more sagittally oriented facet joints at L5-L6 and L6-L7 and a larger angle difference between the lumbar and lumbosacral facet joints, compared with control dogs. A large difference between facet joint angles at L6-L7 and L7-S1 in German Shepherd Dogs may be associated with the frequent occurrence of lumbosacral disk degeneration in this breed.

Method of making and structure for monolithic optical circuits

NASA Technical Reports Server (NTRS)

Evanchuk, Vincent L. (Inventor)

1983-01-01

A method for making monolithic optical circuits, with related optical devices as required or desired, on a supporting surface (10) consists of coating the supporting surface with reflecting metal or cladding resin, spreading a layer of liquid radiation senstivie plastic (12) on the surface, exposing the liquid plastic with a mask (14) to cure it in a desired pattern of light conductors (16, 18, 20), washing away the unexposed liquid plastic, and coating the conductors thus formed with reflective metal or cladding resin. The index of refraction for the cladding (22) is selected to be lower than for the conductors so that light in the conductors will be reflected by the interface with the cladding. For multiple level conductors, as where one conductor must cross over another, the process may be repeated to fabricate a bridge with columns (24, 26) of conductors to the next level, and conductor (28) between the columns. For more efficient transfer of energy over the bridge, faces at 45.degree. may be formed to reflect light up and across the bridge.

Rapid tea catechins and caffeine determination by HPLC using microwave-assisted extraction and silica monolithic column.

PubMed

Rahim, A A; Nofrizal, S; Saad, Bahruddin

2014-03-15

A rapid reversed-phase high performance liquid chromatographic method using a monolithic column for the determination of eight catechin monomers and caffeine was developed. Using a mobile phase of water:acetonitrile:methanol (83:6:11) at a flow rate of 1.4 mL min(-1), the catechins and caffeine were isocratically separated in about 7 min. The limits of detection and quantification were in the range of 0.11-0.29 and 0.33-0.87 mg L(-1), respectively. Satisfactory recoveries were obtained (94.2-105.2 ± 1.8%) for all samples when spiked at three concentrations (5, 40 and 70 mg L(-1)). In combination with microwave-assisted extraction (MAE), the method was applied to the determination of the catechins and caffeine in eleven tea samples (6 green, 3 black and 2 oolong teas). Relatively high levels of caffeine were found in black tea, but higher levels of the catechins, especially epigallocatechin gallate (EGCG) were found in green teas. Copyright © 2013 Elsevier Ltd. All rights reserved.

Simultaneous determination of tylosin and josamycin residues in muscles, liver, eggs and milk by MLC with a monolithic column and time-programmed UV detection: application to baby food and formulae

PubMed Central

2014-01-01

Background Tylosin and Josamycin are macrolide antibiotics. They are used in the treatment of pneumonia, arthritis and mastitis in cattle, and mycoplasma infections in poultry. The incorrect use of antibiotics has lead to the presence of antibiotic residues in foods. The residues cause toxic effects on consumers. Results A simple and sensitive method was optimized and validated for the analysis of tylosin and josamycin residues in food samples. Analytical separation was performed in less than 10 min using a RP C18 monolithic column with time-programmed UV detection at 287 nm and 232 nm and a micellar solution of 0.17 M sodium dodecyl sulphate, 14% methanol and 0.3% triethylamine in 0.02 M phosphoric acid buffered at pH 4 as the mobile phase. The method was fully validated in accordance with ICH guidelines. The micellar method was successfully applied to quantitatively determine tylosin and josamycin residues in spiked chicken muscles, chicken liver, bovine muscles, liver, milk and eggs. It was also extended to the determination of tylosin and josamycin residues in chicken-based baby food and baby formulae. The compounds were separated by a monolithic column which, on account of its particular structure, could bear higher flow rates than usually found for this kind of analysis. High extraction efficiency for tylosin and josamycin was obtained without matrix interference in the extraction process and in the subsequent chromatographic determination. No organic solvent was used during the pretreatment step. Hence, it is considered an interesting technique for “green” chemistry. Conclusion The proposed method was validated and successfully applied for the determination of tylosin and josamycin residues in spiked chicken muscles, chicken liver, bovine muscles, liver, milk and eggs. It was also extended to the determination of tylosin and josamycin residues in chicken-based baby food and baby formulae. PMID:24976860

Affinity monolith chromatography: A review of general principles and applications.

PubMed

Li, Zhao; Rodriguez, Elliott; Azaria, Shiden; Pekarek, Allegra; Hage, David S

2017-11-01

Affinity monolith chromatography, or AMC, is a liquid chromatographic method in which the support is a monolith and the stationary phase is a biological-binding agent or related mimic. AMC has become popular for the isolation of biochemicals, for the measurement of various analytes, and for studying biological interactions. This review will examine the principles and applications of AMC. The materials that have been used to prepare AMC columns will be discussed, which have included various organic polymers, silica, agarose, and cryogels. Immobilization schemes that have been used in AMC will also be considered. Various binding agents and applications that have been reported for AMC will then be described. These applications will include the use of AMC for bioaffinity chromatography, immunoaffinity chromatography, dye-ligand affinity chromatography, and immobilized metal-ion affinity chromatography. The use of AMC with chiral stationary phases and as a tool to characterize biological interactions will also be examined. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

III-nitride nanowire LEDs and diode lasers: monolithic light sources on (001) Si emitting in the 600-1300nm range

NASA Astrophysics Data System (ADS)

Bhattacharya, P.; Hazari, A.; Jahangir, S.

2018-02-01

GaN-based nanowire heterostructure arrays epitaxially grown on (001)Si substrates have unique properties and present the potential to realize useful devices. The active light-emitting region in the nanowire heterostructures are usually InGaN disks, whose composition can be varied to tune the emission wavelength. We have demonstrated light emitting diodes and edgeemitting diode lasers with power outputs 10mW with emission in the 600-1300nm wavelength range. These light sources are therefore useful for a variety of applications, including silicon photonics. Molecular beam epitaxial growth of the nanowire heterostructure arrays on (001)Si substrates and the characteristics of 1.3μm nanowire array edge emitting lasers, guided wave photodiodes and a monolithic photonic integrated circuit designed for 1.3μm operation are described.

Benchmark Design and Installation: A synthesis of Existing Information.

DTIC Science & Technology

1987-07-01

casings (15 ft deep) drilled to rock and filled with concrete. Disks - 1 . Set on vertically stable structures (e.g., dam monoliths). 2 . Set in rock ...Structural movement survey 1 . Rock outcrops (first choice) -- chiseled square on high point. 2 . Massive concrete structure (second choice) - cut square on...bolt marker (type 2 ). 58,. % %--"% %I 1 ± 4 -I,.- Table Cl. Recomnded benchmarks. Type of condition or terrain Type of markert Bedrock, rock outcrops

Pedestal substrate for coated optics

DOEpatents

Hale, Layton C.; Malsbury, Terry N.; Patterson, Steven R.

2001-01-01

A pedestal optical substrate that simultaneously provides high substrate dynamic stiffness, provides low surface figure sensitivity to mechanical mounting hardware inputs, and constrains surface figure changes caused by optical coatings to be primarily spherical in nature. The pedestal optical substrate includes a disk-like optic or substrate section having a top surface that is coated, a disk-like base section that provides location at which the substrate can be mounted, and a connecting cylindrical section between the base and optics or substrate sections. The connecting cylindrical section may be attached via three spaced legs or members. However, the pedestal optical substrate can be manufactured from a solid piece of material to form a monolith, thus avoiding joints between the sections, or the disk-like base can be formed separately and connected to the connecting section. By way of example, the pedestal optical substrate may be utilized in the fabrication of optics for an extreme ultraviolet (EUV) lithography imaging system, or in any optical system requiring coated optics and substrates with reduced sensitivity to mechanical mounts.

Experimental study of the stability and flow characteristics of floating liquid columns confined between rotating disks

NASA Technical Reports Server (NTRS)

Fowle, A. A.; Soto, L.; Strong, P. F.; Wang, C. A.

1980-01-01

A low Bond number simulation technique was used to establish the stability limits of cylindrical and conical floating liquid columns under conditions of isorotation, equal counter rotation, rotation of one end only, and parallel axis offset. The conditions for resonance in cylindrical liquid columns perturbed by axial, sinusoidal vibration of one end face are also reported. All tests were carried out under isothermal conditions with water and silicone fluids of various viscosities. A technique for the quantitative measurement of stream velocity within a floating, isothermal, liquid column confined between rotatable disks was developed. In the measurement, small, light scattering particles were used as streamline markers in common arrangement, but the capability of the measurement was extended by use of stereopair photography system to provide quantitative data. Results of velocity measurements made under a few selected conditions, which established the precision and accuracy of the technique, are given. The general qualitative features of the isothermal flow patterns under various conditions of end face rotation resulting from both still photography and motion pictures are presented.

Sorption of DNA by diatomite-Zn(II) embedded supermacroporous monolithic p(HEMA) cryogels.

PubMed

Tozak, Kabil Özcan; Erzengin, Mahmut; Sargin, Idris; Ünlü, Nuri

2013-01-01

In this study, the DNA sorption performance of diatomite-Zn(II) embedded supermacroporous monolithic p(HEMA) cryogels were investigated for the purpose of designing a novel adsorbent that can be utilized for DNA purification, separation and immunoadsorption studies such as removal of anti-dsDNA antibodies from systemic lupus erythematosus (SLE) patient plasma. Poly(2-hydroxyethyl methacrylate) [p(HEMA)]-based monolithic cryogel column embedded with Zn(2+)-diatomite particles was prepared by free radical cryo-copolymerization of 2-hydroxyethyl methacrylate (HEMA) with N,N'-methylene-bis-acrylamide (MBAAm). The polymerization reaction was initiated by N,N,N',N'-tetramethylene diamine (TEMED) and ammonium persulfate (APS) pair in an ice bath. After thawing, the monolithic composite cryogels were used for affinity sorption and then subsequent desorption of DNA molecules from aqueous solutions. Diatomite (DA) particles were characterized by XRF and BET method. The characterization of composite cryogel was done through SEM imaging. The effects of pH of the solution, initial DNA concentration, ionic strength, temperature and flow rates on adsorption were investigated to determine the optimum conditions for adsorption/desorption experiments. The particle embedding procedure was shown to yield significantly enhanced adsorption of DNA on the adsorbent. Furthermore, considering its excellent bio-compatibility, p(HEMA) cryogels are promising a candidate for further DNA sorption studies.

Sorption of DNA by diatomite-Zn(II) embedded supermacroporous monolithic p(HEMA) cryogels

PubMed Central

Tozak, Kabil Özcan; Erzengin, Mahmut; Sargin, Idris; Ünlü, Nuri

2013-01-01

In this study, the DNA sorption performance of diatomite-Zn(II) embedded supermacroporous monolithic p(HEMA) cryogels were investigated for the purpose of designing a novel adsorbent that can be utilized for DNA purification, separation and immunoadsorption studies such as removal of anti-dsDNA antibodies from systemic lupus erythematosus (SLE) patient plasma. Poly(2-hydroxyethyl methacrylate) [p(HEMA)]-based monolithic cryogel column embedded with Zn2+-diatomite particles was prepared by free radical cryo-copolymerization of 2-hydroxyethyl methacrylate (HEMA) with N,N'-methylene-bis-acrylamide (MBAAm). The polymerization reaction was initiated by N,N,N',N'-tetramethylene diamine (TEMED) and ammonium persulfate (APS) pair in an ice bath. After thawing, the monolithic composite cryogels were used for affinity sorption and then subsequent desorption of DNA molecules from aqueous solutions. Diatomite (DA) particles were characterized by XRF and BET method. The characterization of composite cryogel was done through SEM imaging. The effects of pH of the solution, initial DNA concentration, ionic strength, temperature and flow rates on adsorption were investigated to determine the optimum conditions for adsorption/desorption experiments. The particle embedding procedure was shown to yield significantly enhanced adsorption of DNA on the adsorbent. Furthermore, considering its excellent bio-compatibility, p(HEMA) cryogels are promising a candidate for further DNA sorption studies. PMID:26600734

Affinity chromatography on monolithic supports for simultaneous and high-throughput isolation of immunoglobulins from human serum.

PubMed

Martinović, Tamara; Andjelković, Uroš; Klobučar, Marko; Černigoj, Urh; Vidič, Jana; Lučić, Marina; Pavelić, Krešimir; Josić, Djuro

2017-11-01

Posttranslational modifications of immunoglobulins have been a topic of great interest and have been repeatedly reported as a major factor in disease pathology. Cost-effective, reproducible, and high-throughput (HTP) isolation of immunoglobulins from human serum is vital for studying the changes in protein structure and the following understanding of disease development. Although there are many methods for the isolation of specific immunoglobulin classes, only a few of them are applicable for isolation of all subtypes and variants. Here, we present the development of a scheme for fast and simultaneous affinity purification of α (A), γ (G), and μ (M) immunoglobulins from human serum through affinity monolith chromatography. Affinity-based monolithic columns with immobilized protein A, G, or L were used for antibody isolation. Monolithic stationary phases have a high surface accessibility of binding sites, large flow-through channels, and can be operated at high flow rates, making them the ideal supports for HTP isolation of biopolymers. The presented method can be used for HTP screening of human serum in order to simultaneously isolate all three above-mentioned immunoglobulins and determine their concentration and changes in their glycosylation pattern as potential prognostic and diagnostic disease biomarkers. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Mixed mode HILIC/anion exchange separations on latex coated silica monoliths.

PubMed

Ibrahim, Mohammed E A; Lucy, Charles A

2012-10-15

Bare silica monoliths do not possess anion exchange sites hence they show low retention for anions. Moreover, bare silica monoliths show low retention in hydrophilic interaction liquid chromatography (HILIC). Coating the silica surface with cationic nanoparticles e.g. AS9-SC (latex A), AS12A (latex B) and DNApac (latex C) increases the thickness of the water layer on the Onyx silica monolith 8-10 times enabling HILIC retention when a high % acetonitrile (ACN) mobile phase is used. The formed water layer by itself is not sufficient to perform good separation of the studied anions (acetate, formate, nitrate, bromate, thiocyanate and iodide). On the other hand, the latex nanoparticles introduce positively charged sites, making anion exchange chromatography possible, with the anion exchange capacity varying with the latex adsorbed (44.1 ± 0.2, 4.4 ± 0.1 and 14.0 ± 0.7 μeq/column for latex A, B and C, respectively). Latex A nanoparticles which provided the highest ion exchange capacity separated all tested anions with reasonable resolution. Fast separation (2.5 min) of acetate, formate, nitrate, bromate, thiocyanate and iodide was performed using the latex A coated silica monolith. The obtained efficiencies are 13,000-50,000 plates/m at 3 mL/min with a minimum resolution of 0.85. Retention is mixed mode under HILIC conditions with HILIC dominating for the kosmotropic anions and ion exchange dominating for the chaotropic anions. The two different brands of silica monoliths (Merck Chromolith and Phenomenex Onyx) coated with the same latex A nanoparticles displayed similar water layer volumes, ion exchange capacity and selectivity. Copyright © 2012 Elsevier B.V. All rights reserved.

The Distribution and Excitation of CH3CN in a Solar Nebula Analog

NASA Astrophysics Data System (ADS)

Loomis, Ryan A.; Cleeves, L. Ilsedore; Öberg, Karin I.; Aikawa, Yuri; Bergner, Jennifer; Furuya, Kenji; Guzman, V. V.; Walsh, Catherine

2018-06-01

Cometary studies suggest that the organic composition of the early Solar Nebula was rich in complex nitrile species such CH3CN. Recent ALMA detections in protoplanetary disks suggest that these species may be common during planet and comet formation, but connecting gas-phase measurements to cometary abundances first requires constraints on formation chemistry and distributions of these species. We present here the detection of seven spatially resolved transitions of CH3CN in the protoplanetary disk around the T-Tauri star TW Hya. Using a rotational diagram analysis, we find a disk-averaged column density of {N}T={1.45}-0.15+0.19× {10}12 cm‑2 and a rotational temperature of {T}rot}={32.7}-3.4+3.9 K. A radially resolved rotational diagram shows the rotational temperature to be constant across the disk, suggesting that the CH3CN emission originates from a layer at z/r ∼ 0.3. Through comparison of the observations with predictions from a disk chemistry model, we find that grain-surface reactions likely dominate CH3CN formation and that in situ disk chemistry is sufficient to explain the observed CH3CN column density profile without invoking inheritance from the protostellar phase. However, the same model fails to reproduce a solar system cometary abundance of CH3CN relative to H2O in the midplane, suggesting that either vigorous vertical mixing or some degree of inheritance from interstellar ices occurred in the Solar Nebula.

NuSTAR Observations of Water Megamaser AGN

NASA Technical Reports Server (NTRS)

Masini, A.; Comastri, A.; Balokvic, M.; Zaw, I.; Puccetti, S.; Ballantyne, D. R.; Bauer, F. E.; Boggs, S. E.; Brandt, W. N.; Zhang, William W.

2016-01-01

Aims. We study the connection between the masing disk and obscuring torus in Seyfert 2 galaxies. Methods. We present a uniform X-ray spectral analysis of the high energy properties of 14 nearby megamaser active galactic nuclei observed by NuSTAR. We use a simple analytical model to localize the maser disk and understand its connection with the torus by combining NuSTAR spectral parameters with the available physical quantities from VLBI mapping.Results. Most of the sources that we analyzed are heavily obscured, showing a column density in excess of approx.10(exp 23) cm(exp -2); in particular, 79% are Compton-thick [NH is greater than 1.5 x 10(exp 24) cm(exp -2)]. When using column densities measured by NuSTAR with the assumption that the torus is the extension of the maser disk, and further assuming a reasonable density profile, we can predict the torus dimensions. They are found to be consistent with mid-IR interferometry parsec-scale observations of Circinus and NGC 1068. In this picture, the maser disk is intimately connected to the inner part of the torus. It is probably made of a large number of molecular clouds that connect the torus and the outer part of the accretion disk, giving rise to a thin disk rotating in most cases in Keplerian or sub-Keplerian motion. This toy model explains the established close connection between water megamaser emission and nuclear obscuration as a geometric effect.

Raman-Scattering Line Profiles of the Symbiotic Star AG Peg

NASA Astrophysics Data System (ADS)

Lee, Seong-Jae; Hyung, Siek

2017-06-01

The high dispersion Hα and Hβ line profiles of the Symbiotic star AG Peg consist of top double Gaussian and bottom components. We investigated the formation of the broad wings with Raman scattering mechanism. Adopting the same physical parameters from the photo-ionization study of Kim and Hyung (2008) for the white dwarf and the ionized gas shell, Monte Carlo simulations were carried out for a rotating accretion disk geometry of non-symmetrical latitude angles from -7° < θ < +7° to -16° < θ < +16°. The smaller latitude angle of the disk corresponds to the approaching side of the disk responsible for weak blue Gaussian profile, while the wider latitude angle corresponds to the other side of the disk responsible for the strong red Gaussian profile. We confirmed that the shell has the high gas density ˜ 109.85 cm-3 in the ionized zone of AG Peg derived in the previous photo-ionization model study. The simulation with various HI shell column densities (characterized by a thickness ΔD × gas number density nH) shows that the HI gas shell with a column density Hhi ≈ 3 - 5 × 1019 cm-2 fits the observed line profiles well. The estimated rotation speed of the accretion disk shell is in the range of 44 - 55 kms-1. We conclude that the kinematically incoherent structure involving the outflowing gas from the giant star caused an asymmetry of the disk and double Gaussian profiles found in AG Peg.

On the Origin of the High Column Density Turnover in the HI Column Density Distribution

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

Erkal, Denis; Gnedin, Nickolay Y.; Kravtsov, Andrey V.

We study the high column density regime of the HI column density distribution function and argue that there are two distinct features: a turnover at NHI ~ 10^21 cm^-2 which is present at both z=0 and z ~ 3, and a lack of systems above NHI ~ 10^22 cm^-2 at z=0. Using observations of the column density distribution, we argue that the HI-H2 transition does not cause the turnover at NHI ~ 10^21 cm^-2, but can plausibly explain the turnover at NHI > 10^22 cm^-2. We compute the HI column density distribution of individual galaxies in the THINGS sample andmore » show that the turnover column density depends only weakly on metallicity. Furthermore, we show that the column density distribution of galaxies, corrected for inclination, is insensitive to the resolution of the HI map or to averaging in radial shells. Our results indicate that the similarity of HI column density distributions at z=3 and z=0 is due to the similarity of the maximum HI surface densities of high-z and low-z disks, set presumably by universal processes that shape properties of the gaseous disks of galaxies. Using fully cosmological simulations, we explore other candidate physical mechanisms that could produce a turnover in the column density distribution. We show that while turbulence within GMCs cannot affect the DLA column density distribution, stellar feedback can affect it significantly if the feedback is sufficiently effective in removing gas from the central 2-3 kpc of high-redshift galaxies. Finally, we argue that it is meaningful to compare column densities averaged over ~ kpc scales with those estimated from quasar spectra which probe sub-pc scales due to the steep power spectrum of HI column density fluctuations observed in nearby galaxies.« less

Depleted fully monolithic CMOS pixel detectors using a column based readout architecture for the ATLAS Inner Tracker upgrade

NASA Astrophysics Data System (ADS)

Wang, T.; Barbero, M.; Berdalovic, I.; Bespin, C.; Bhat, S.; Breugnon, P.; Caicedo, I.; Cardella, R.; Chen, Z.; Degerli, Y.; Egidos, N.; Godiot, S.; Guilloux, F.; Hemperek, T.; Hirono, T.; Krüger, H.; Kugathasan, T.; Hügging, F.; Marin Tobon, C. A.; Moustakas, K.; Pangaud, P.; Schwemling, P.; Pernegger, H.; Pohl, D.-L.; Rozanov, A.; Rymaszewski, P.; Snoeys, W.; Wermes, N.

2018-03-01

Depleted monolithic active pixel sensors (DMAPS), which exploit high voltage and/or high resistivity add-ons of modern CMOS technologies to achieve substantial depletion in the sensing volume, have proven to have high radiation tolerance towards the requirements of ATLAS in the high-luminosity LHC era. DMAPS integrating fast readout architectures are currently being developed as promising candidates for the outer pixel layers of the future ATLAS Inner Tracker, which will be installed during the phase II upgrade of ATLAS around year 2025. In this work, two DMAPS prototype designs, named LF-Monopix and TJ-Monopix, are presented. LF-Monopix was fabricated in the LFoundry 150 nm CMOS technology, and TJ-Monopix has been designed in the TowerJazz 180 nm CMOS technology. Both chips employ the same readout architecture, i.e. the column drain architecture, whereas different sensor implementation concepts are pursued. The paper makes a joint description of the two prototypes, so that their technical differences and challenges can be addressed in direct comparison. First measurement results for LF-Monopix will also be shown, demonstrating for the first time a fully functional fast readout DMAPS prototype implemented in the LFoundry technology.

Monolithically Integrated Dual-Wavelength Self-Sustained Pulsating Laser Diodes with Real Refractive Index Guided Self-Aligned Structure

NASA Astrophysics Data System (ADS)

Onishi, Toshikazu; Imafuji, Osamu; Fukuhisa, Toshiya; Mochida, Atsunori; Kobayashi, Yasuhiro; Yuri, Masaaki; Itoh, Kunio; Shimizu, Hirokazu

2001-11-01

Monolithically integrated 780-nm-band and 650-nm-band self-sustained pulsating (SSP) lasers, which are desirable for simplified optical pickups in digital versatile disk (DVD) systems, have been developed for the first time. The real refractive index guided self-aligned (RISA) waveguide structure is adapted to reduce absorption loss in the current blocking layers. In order to obtain stable SSP, a saturable absorber formed in the active layer outside the current stripe, and a saturable absorbing layer above the active layer are utilized for the 780-nm-band and 650-nm-band laser diodes (LDs), respectively. Relative intensity noise less than -130 dB/Hz is maintained at temperatures of up to 80°C at an output power of 7 mW for the 650 nm band and 10 mW for the 780 nm band, which suggests that stable SSP operations have been realized.

Silica-based monolithic column with evaporative light scattering detector for HPLC analysis of bacosides and apigenin in Bacopa monnieri.

PubMed

Bhandari, Pamita; Kumar, Neeraj; Singh, Bikram; Singh, Virendra; Kaur, Inderjeet

2009-08-01

A high performance liquid chromatographic method using a silica-based monolithic column coupled with evaporative light scattering detector (HPLC-ELSD) was developed and validated for simultaneous quantification of bacosides (bacoside A, bacopaside I, bacoside A(3), bacopaside II, bacopaside X, bacopasaponin C) and apigenin in Bacopa monnieri. The chromatographic resolution was achieved on a Chromolith RP-18 (100x4.6 mm) column with acetonitrile/water (30:70) as mobile phase in isocratic elution at a flow rate of 0.7 mL/min. The drift tube temperature of the ELSD was set to 95 degrees C, and the nitrogen flow rate was 2.0 SLM (standard liter per minute). The calibration curves revealed a good linear relationship (r(2) > 0.9988) within the test ranges. The detection limits (S/N = 3) and the quantification limits (S/N = 10) for the compounds were in the range of 0.54-6.06 and 1.61-18.78 microg/mL, respectively. Satisfactory average recovery was observed in the range of 95.8-99.0%. The method showed good reproducibility for the quantification of these compounds in B. monnieri with intra- and inter-day precision of less than 0.69 and 0.67%, respectively. The validated method was successfully applied to quantify analytes in nine accessions of B. monnieri and thus provides a new basis for overall quality assessment of B. monnieri.

Behavior of wet precast beam column connections under progressive collapse scenario: an experimental study

NASA Astrophysics Data System (ADS)

Nimse, Rohit B.; Joshi, Digesh D.; Patel, Paresh V.

2014-12-01

Progressive collapse denotes a failure of a major portion of a structure that has been initiated by failure of a relatively small part of the structure such as failure of any vertical load carrying element (typically columns). Failure of large part of any structure will results into substantial loss of human lives and natural resources. Therefore, it is important to prevent progressive collapse which is also known as disproportionate collapse. Nowadays, there is an increasing trend toward construction of buildings using precast concrete. In precast concrete construction, all the components of structures are produced in controlled environment and they are being transported to the site. At site such individual components are connected appropriately. Connections are the most critical elements of any precast structure, because in past major collapse of precast structure took place because of connection failure. In this study, behavior of three different 1/3rd scaled wet precast beam column connections under progressive collapse scenario are studied and its performance is compared with monolithic connection. Precast connections are constructed by adopting different connection detailing at the junction by considering reinforced concrete corbel for two specimens and steel billet for one specimen. Performance of specimen is evaluated on the basis of ultimate load carrying capacity, maximum deflection and deflection measured along the span of the beam. From the results, it is observed that load carrying capacity and ductility of precast connections considered in this study are more than that of monolithic connections.

Damping and impact properties of laminated scaffolds and glass columns evaluated through the use of computational methods

NASA Astrophysics Data System (ADS)

Nieves, Ian

Dynamic finite element analysis (FEA) was used to verify the ability of a novel percussion instrument to characterize the composition and structure of laminated materials and glass columns and to elucidate key facets of this process. Initial simulations modeling the percussion process with varying probe geometries were performed to access which configuration most accurately represented in situ diagnostic activity. Percussion testing of monoliths and laminated duplex scaffolds consisting of PTFE and 6061 Al was simulated to assess the ability of the numeric methodology to model intrinsic damping in laminated scaffolds and determine the potential contributions of size effects, gripping configurations, and probe friction to the loading response of the material being tested. Percussion testing of laminated scaffolds and monoliths composed of either PMMA or PLGA was modeled to investigate the effects of defects on the impact response and to evaluate promising strategies for enhancing damping that promotes tissue regeneration in biomedical materials. Percussion testing of virgin and cracked glass columns was modeled and the resulting probe acceleration predictions compared to corresponding experimental findings to evaluate the overall accuracy of the methodology and to discern its capacity for elucidating facets of defect detection in rigid materials. Overall, the modeling the results validated the effectiveness of the numeric methodology for modeling and elucidating the mechanics of percussion testing and suggested strategies whereby this procedure can facilitate the development of innovative biomedical materials designed to promote tissue regeneration.

Two-dimensional liquid chromatography consisting of twelve second-dimension columns for comprehensive analysis of intact proteins.

PubMed

Ren, Jiangtao; Beckner, Matthew A; Lynch, Kyle B; Chen, Huang; Zhu, Zaifang; Yang, Yu; Chen, Apeng; Qiao, Zhenzhen; Liu, Shaorong; Lu, Joann J

2018-05-15

A comprehensive two-dimensional liquid chromatography (LCxLC) system consisting of twelve columns in the second dimension was developed for comprehensive analysis of intact proteins in complex biological samples. The system consisted of an ion-exchange column in the first dimension and the twelve reverse-phase columns in the second dimension; all thirteen columns were monolithic and prepared inside 250 µm i.d. capillaries. These columns were assembled together through the use of three valves and an innovative configuration. The effluent from the first dimension was continuously fractionated and sequentially transferred into the twelve second-dimension columns, while the second-dimension separations were carried out in a series of batches (six columns per batch). This LCxLC system was tested first using standard proteins followed by real-world samples from E. coli. Baseline separation was observed for eleven standard proteins and hundreds of peaks were observed for the real-world sample analysis. Two-dimensional liquid chromatography, often considered as an effective tool for mapping proteins, is seen as laborious and time-consuming when configured offline. Our online LCxLC system with increased second-dimension columns promises to provide a solution to overcome these hindrances. Copyright © 2018 Elsevier B.V. All rights reserved.

Evolving Gravitationally Unstable Disks over Cosmic Time: Implications for Thick Disk Formation

NASA Astrophysics Data System (ADS)

Forbes, John; Krumholz, Mark; Burkert, Andreas

2012-07-01

Observations of disk galaxies at z ~ 2 have demonstrated that turbulence driven by gravitational instability can dominate the energetics of the disk. We present a one-dimensional simulation code, which we have made publicly available, that economically evolves these galaxies from z ~ 2 to z ~ 0 on a single CPU in a matter of minutes, tracking column density, metallicity, and velocity dispersions of gaseous and multiple stellar components. We include an H2-regulated star formation law and the effects of stellar heating by transient spiral structure. We use this code to demonstrate a possible explanation for the existence of a thin and thick disk stellar population and the age-velocity-dispersion correlation of stars in the solar neighborhood: the high velocity dispersion of gas in disks at z ~ 2 decreases along with the cosmological accretion rate, while at lower redshift the dynamically colder gas forms the low velocity dispersion stars of the thin disk.

General Relativistic Radiation MHD Simulations of Supercritical Accretion onto a Magnetized Neutron Star: Modeling of Ultraluminous X-Ray Pulsars

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

Takahashi, Hiroyuki R.; Ohsuga, Ken, E-mail: takahashi@cfca.jp, E-mail: ken.ohsuga@nao.ac.jp

By performing 2.5-dimensional general relativistic radiation magnetohydrodynamic simulations, we demonstrate supercritical accretion onto a non-rotating, magnetized neutron star, where the magnetic field strength of dipole fields is 10{sup 10} G on the star surface. We found the supercritical accretion flow consists of two parts: the accretion columns and the truncated accretion disk. The supercritical accretion disk, which appears far from the neutron star, is truncated at around ≃3 R {sub *} ( R {sub *} = 10{sup 6} cm is the neutron star radius), where the magnetic pressure via the dipole magnetic fields balances with the radiation pressure of themore » disks. The angular momentum of the disk around the truncation radius is effectively transported inward through magnetic torque by dipole fields, inducing the spin up of a neutron star. The evaluated spin-up rate, ∼−10{sup −11} s s{sup −1}, is consistent with the recent observations of the ultraluminous X-ray pulsars. Within the truncation radius, the gas falls onto a neutron star along the dipole fields, which results in a formation of accretion columns onto the northern and southern hemispheres. The net accretion rate and the luminosity of the column are ≃66 L {sub Edd}/ c {sup 2} and ≲10 L {sub Edd}, where L {sub Edd} is the Eddington luminosity and c is the light speed. Our simulations support a hypothesis whereby the ultraluminous X-ray pulsars are powered by the supercritical accretion onto the magnetized neutron stars.« less

Noninvasive monitoring of plasma L-dopa concentrations using sweat samples in Parkinson's disease.

PubMed

Tsunoda, Makoto; Hirayama, Masaaki; Tsuda, Takao; Ohno, Kinji

2015-03-10

L-dopa (l-3,4-dihydroxyphenylalanine) is commonly used for treating Parkinson's disease (PD). However, regardless of its prominent effect, therapeutic range of L-dopa narrows down with disease progression, which leads to development of motor complications including wearing off and dyskinesias. In addition, intestinal absorption of L-dopa is inversely correlated with the amount of oral protein intake, and shows intra- and inter-day variability. Hence, frequent monitoring of plasma L-dopa concentrations is beneficial, but frequent venipuncture imposes physical and psychological burdens on patients with PD. We investigated the usefulness of sweat samples instead of plasma samples for monitoring L-dopa concentrations. With a monolithic silica disk-packed spin column and the high-performance liquid chromatography-electrochemical detection system, L-dopa in sweat samples was successfully quantified and analyzed in 23 PD patients. We found that the Pearson's correlation coefficient of the plasma and sweat l-dopa concentrations was 0.678. Although the disease durations and severities were not correlated with the deviation of the actual sweat L-dopa concentrations from the fitted line, acquisition of the sweat samples under a stable condition was technically difficult in severely affected patients. The deviations may also be partly accounted for by skin permeability of L-dopa. Measuring L-dopa concentrations in sweat is suitable to get further insights into the L-dopa metabolism. Copyright © 2015 Elsevier B.V. All rights reserved.

Smooth H I Low Column Density Outskirts in Nearby Galaxies

NASA Astrophysics Data System (ADS)

Ianjamasimanana, R.; Walter, Fabian; de Blok, W. J. G.; Heald, George H.; Brinks, Elias

2018-06-01

The low column density gas at the outskirts of galaxies as traced by the 21 cm hydrogen line emission (H I) represents the interface between galaxies and the intergalactic medium, i.e., where galaxies are believed to get their supply of gas to fuel future episodes of star formation. Photoionization models predict a break in the radial profiles of H I at a column density of ∼5 × 1019 cm‑2 due to the lack of self-shielding against extragalactic ionizing photons. To investigate the prevalence of such breaks in galactic disks and to characterize what determines the potential edge of the H I disks, we study the azimuthally averaged H I column density profiles of 17 nearby galaxies from the H I Nearby Galaxy Survey and supplemented in two cases with published Hydrogen Accretion in LOcal GAlaxieS data. To detect potential faint H I emission that would otherwise be undetected using conventional moment map analysis, we line up individual profiles to the same reference velocity and average them azimuthally to derive stacked radial profiles. To do so, we use model velocity fields created from a simple extrapolation of the rotation curves to align the profiles in velocity at radii beyond the extent probed with the sensitivity of traditional integrated H I maps. With this method, we improve our sensitivity to outer-disk H I emission by up to an order of magnitude. Except for a few disturbed galaxies, none show evidence of a sudden change in the slope of the H I radial profiles: the alleged signature of ionization by the extragalactic background.

Structural analysis for a 40-story building

NASA Technical Reports Server (NTRS)

Hua, L.

1972-01-01

NASTRAN was chosen as the principal analytical tool for structural analysis of the Illinois Center Plaza Hotel Building in Chicago, Illinois. The building is a 40-story, reinforced concrete structure utilizing a monolithic slab-column system. The displacements, member stresses, and foundation loads due to wind load, live load, and dead load were obtained through a series of NASTRAN runs. These analyses and the input technique are described.

Line formation in the hot spot region of cataclysmic variable accretion disks

NASA Technical Reports Server (NTRS)

Elitzur, Moshe; Clarke, John T.; Kallman, T. R.

1988-01-01

The paper presents a theoretical analysis of the emission lines observed in the cataclysmic variable A0 Psc (=H2252-035), including detailed modeling of the hydrogen Balmer line emission. The analysis makes it possible to deduce the physical conditions in the so called 'hot spot', or 'bulge' region where the accretion column hits the rim of the accretion disk. It is concluded that the bulge is optically thick to the ionizing disk radiation. Consequently, its disk illuminated face is fully ionized whereas the side facing away from the disk is neutral, resulting in modulation of the observed emission lines with the orbital period. The density in the hot spot is about 5 x 10 to the 12th to 10 to the 13th/cu cm.

Spiral Countercurrent Chromatography

PubMed Central

Ito, Yoichiro; Knight, Martha; Finn, Thomas M.

2013-01-01

For many years, high-speed countercurrent chromatography conducted in open tubing coils has been widely used for the separation of natural and synthetic compounds. In this method, the retention of the stationary phase is solely provided by the Archimedean screw effect by rotating the coiled column in the centrifugal force field. However, the system fails to retain enough of the stationary phase for polar solvent systems such as the aqueous–aqueous polymer phase systems. To address this problem, the geometry of the coiled channel was modified to a spiral configuration so that the system could utilize the radially acting centrifugal force. This successfully improved the retention of the stationary phase. Two different types of spiral columns were fabricated: the spiral disk assembly, made by stacking multiple plastic disks with single or four interwoven spiral channels connected in series, and the spiral tube assembly, made by inserting the tetrafluoroethylene tubing into a spiral frame (spiral tube support). The capabilities of these column assemblies were successfully demonstrated by separations of peptides and proteins with polar two-phase solvent systems whose stationary phases had not been well retained in the earlier multilayer coil separation column for high-speed countercurrent chromatography. PMID:23833207

Preparation of 2,4-dichlorophenoxyacetic acid imprinted organic-inorganic hybrid monolithic column and application to selective solid-phase microextraction.

PubMed

Liu, Xiaofang; Zhu, Quanfei; Chen, Huaixia; Zhou, Liuzi; Dang, Xueping; Huang, Jianlin

2014-03-01

An organic-inorganic hybrid molecular imprinting monolith (HMIM) has been prepared, characterized and applied for the determination of 2,4-dichlorophenoxyacetic acid (2,4-D) in rice with high-performance liquid chromatography-photodiodes array detector (HPLC-PAD). By optimizing the polymerization conditions, such as the volume ratio of the inorganic alcoholysate and organic part, the 2,4-D-HMIM was synthesized in a micro pipette tip using acrylamide as the functional monomer, ethylene dimethacrylate as the cross-linker and methanol as the porogenic solvent. The morphology of the monolith was studied by scanning electronmicroscopy and Fourier transform infrared spectra. The imprinted factor of the monolith for 2,4-D reached 3.29. A simple, rapid and sensitive method for the determination of 2,4-D in rice using the HMIM microextraction combined with high-performance liquid chromatography-photodiodes array detector was developed. Some parameters affecting the sample pretreatment were investigated, including the type and volume of eluent, the flow rate and volume of sample solution. The assay exhibited a linear dynamic range of 167-4167μg/kg with the correlation coefficient above 0.9972. The detection limit (at S/N=3) was 50μg/kg. The proposed method was successfully applied for the selective determination of 2,4-D in rice. Copyright © 2014 Elsevier B.V. All rights reserved.

Monolithic poly[(trimethylsilyl-4-methylstyrene)-co- bis(4-vinylbenzyl)dimethylsilane] stationary phases for the fast separation of proteins and oligonucleotides.

PubMed

Jakschitz, Thomas A E; Huck, Christian W; Lubbad, Said; Bonn, Günther K

2007-04-13

In this paper the synthesis, optimisation and application of a silane based monolithic copolymer for the rapid separation of proteins and oligonucleotides is described. The monolith was prepared by thermal initiated in situ copolymerisation of trimethylsilyl-4-methylstyrene (TMSiMS) and bis(4-vinylbenzyl)dimethylsilane (BVBDMSi) in a silanised 200 microm I.D. fused silica column. Different ratios of monomer and crosslinker, as well as different ratios of micro- (toluene) and macro-porogen (2-propanol) were used for optimising the physical properties of the stationary phase regarding separation efficiency. The prepared monolithic stationary phases were characterised by measurement of permeability with different solvents, determination of pore size distribution by mercury intrusion porosimetry (MIP). Morphology was studied by scanning electron microscopy (SEM). Applying optimised conditions, a mixture comprised of five standard proteins ribunuclease A, cytochrome c, alpha-lactalbumine, myoglobine and ovalbumine was separated within 1 min by ion-pair reversed-phase liquid chromatography (IP-RPLC) obtaining half-height peak widths between 1.8 and 2.4 s. Baseline separation of oligonucleotides d(pT)(12-18) was achieved within 1.8 min obtaining half-height peak widths between 3.6 and 5.4 s. The results demonstrate the high potential of this stationary phase for fast separation of high-molecular weight biomolecules such as oligonucleotides and proteins.

Spin-on doping of germanium-on-insulator wafers for monolithic light sources on silicon

NASA Astrophysics Data System (ADS)

Al-Attili, Abdelrahman Z.; Kako, Satoshi; Husain, Muhammad K.; Gardes, Frederic Y.; Arimoto, Hideo; Higashitarumizu, Naoki; Iwamoto, Satoshi; Arakawa, Yasuhiko; Ishikawa, Yasuhiko; Saito, Shinichi

2015-05-01

High electron doping of germanium (Ge) is considered to be an important process to convert Ge into an optical gain material and realize a monolithic light source integrated on a silicon chip. Spin-on doping is a method that offers the potential to achieve high doping concentrations without affecting crystalline qualities over other methods such as ion implantation and in-situ doping during material growth. However, a standard spin-on doping recipe satisfying these requirements is not yet available. In this paper we examine spin-on doping of Ge-on-insulator (GOI) wafers. Several issues were identified during the spin-on doping process and specifically the adhesion between Ge and the oxide, surface oxidation during activation, and the stress created in the layers due to annealing. In order to mitigate these problems, Ge disks were first patterned by dry etching followed by spin-on doping. Even by using this method to reduce the stress, local peeling of Ge could still be identified by optical microscope imaging. Nevertheless, most of the Ge disks remained after the removal of the glass. According to the Raman data, we could not identify broadening of the lineshape which shows a good crystalline quality, while the stress is slightly relaxed. We also determined the linear increase of the photoluminescence intensity by increasing the optical pumping power for the doped sample, which implies a direct population and recombination at the gamma valley.

Ion chromatographic determination of hydroxide ion on monolithic reversed-phase silica gel columns coated with nonionic and cationic surfactants.

PubMed

Xu, Qun; Mori, Masanobu; Tanaka, Kazuhiko; Ikedo, Mikaru; Hu, Wenzhi; Haddad, Paul R

2004-07-02

The determination of hydroxide by ion chromatography (IC) is demonstrated using a monolithic octadecylsilyl (ODS)-silica gel column coated first with a nonionic surfactant (polyoxyethylene (POE)) and then with a cationic surfactant (cetyltrimethylammonium bromide (CTAB)). This stationary phase, when used in conjunction with a 10 mmol/l sodium sulfate eluent at pH 8.2, was found to be suitable for the rapid and efficient separation of hydroxide from some other anions, based on a conventional ion-exchange mechanism. The peak directions and detection responses for these ions were in agreement with their known limiting equivalent ionic conductance values. Under these conditions, a linear calibration plot was obtained for hydroxide ion over the range 16 micromol/l to 15 mmol/l, and the detection limit determined at a signal-to-noise ratio of 3 was 6.4 micromol/l. The double-coated stationary phase described above was shown to be superior to a single coating of cetyltrimethylammonium bromide alone, in terms of separation efficiency and stability of the stationary phase. A range of samples comprising solutions of some strong and weak bases was analyzed by the proposed method and the results obtained were in good agreement with those obtained by conventional potentiometric pH measurement.

Development of monolithic pixel detector with SOI technology for the ILC vertex detector

NASA Astrophysics Data System (ADS)

Yamada, M.; Ono, S.; Tsuboyama, T.; Arai, Y.; Haba, J.; Ikegami, Y.; Kurachi, I.; Togawa, M.; Mori, T.; Aoyagi, W.; Endo, S.; Hara, K.; Honda, S.; Sekigawa, D.

2018-01-01

We have been developing a monolithic pixel sensor for the International Linear Collider (ILC) vertex detector with the 0.2 μm FD-SOI CMOS process by LAPIS Semiconductor Co., Ltd. We aim to achieve a 3 μm single-point resolution required for the ILC with a 20×20 μm2 pixel. Beam bunch crossing at the ILC occurs every 554 ns in 1-msec-long bunch trains with an interval of 200 ms. Each pixel must record the charge and time stamp of a hit to identify a collision bunch for event reconstruction. Necessary functions include the amplifier, comparator, shift register, analog memory and time stamp implementation in each pixel, and column ADC and Zero-suppression logic on the chip. We tested the first prototype sensor, SOFIST ver.1, with a 120 GeV proton beam at the Fermilab Test Beam Facility in January 2017. SOFIST ver.1 has a charge sensitive amplifier and two analog memories in each pixel, and an 8-bit Wilkinson-type ADC is implemented for each column on the chip. We measured the residual of the hit position to the reconstructed track. The standard deviation of the residual distribution fitted by a Gaussian is better than 3 μm.

Development of an image converter of radical design. [employing solid state electronics towards the production of an advanced engineering model camera system

NASA Technical Reports Server (NTRS)

Irwin, E. L.; Farnsworth, D. L.

1972-01-01

A long term investigation of thin film sensors, monolithic photo-field effect transistors, and epitaxially diffused phototransistors and photodiodes to meet requirements to produce acceptable all solid state, electronically scanned imaging system, led to the production of an advanced engineering model camera which employs a 200,000 element phototransistor array (organized in a matrix of 400 rows by 500 columns) to secure resolution comparable to commercial television. The full investigation is described for the period July 1962 through July 1972, and covers the following broad topics in detail: (1) sensor monoliths; (2) fabrication technology; (3) functional theory; (4) system methodology; and (5) deployment profile. A summary of the work and conclusions are given, along with extensive schematic diagrams of the final solid state imaging system product.

A comparative study of progressive wear of four dental monolithic, veneered glass-ceramics.

PubMed

Zhang, Zhenzhen; Yi, Yuanping; Wang, Xuesong; Guo, Jiawen; Li, Ding; He, Lin; Zhang, Shaofeng

2017-10-01

This study evaluated the wear performance and wear mechanisms of four dental glass-ceramics, based on the microstructure and mechanical properties in the progressive wear process. Bar (N = 40, n = 10) and disk (N = 32, n = 8) specimens were prepared from (A) lithium disilicate glass-ceramic (LD), (B) leucite reinforced glass-ceramic (LEU), (C) feldspathic glass-ceramic (FEL), and (D) fluorapatite glass-ceramic (FLU). The bar specimens were tested for three-point flexural strength, hardness, fracture toughness and elastic modulus. The disk specimens paired with steatite antagonists were tested in a pin-on-disk tribometer with 10N up to 1000,000 wear cycles. The wear analysis of glass-ceramics was performed using a 3D profilometer after every 200,000 wear cycles. Wear loss of steatite antagonists was calculated by measuring the weight and density using sensitive balance and Archimedes' method. Wear morphologies and microstructures were analyzed by scanning electron microscopy (SEM). The crystalline phase compositions were determined using X-ray diffraction (XRD). One-way analysis of variance (ANOVA) was used to analyze the data. Multiple pair-wise comparison of means was performed by Tukey's post-hoc test. LD showed the highest fracture toughness, flexural strength, elastic modulus and crystallinity, followed by LEU and FEL, and FLU showed the lowest. However, the hardness of LD was lower than all the other three types of ceramics. For steatite antagonists, LD produced the least wear loss of antagonist, followed by LEU and FEL, and FLU had the most wear loss. For glass-ceramic materials, LD exhibited similar wear loss as LEU, but more than FLU and FEL did. Moreover, fracture occurred on the wear surface of FLU. In the progressive wear process, veneering porcelains showed better wear resistance but fluorapatite veneering porcelains appeared fracture surface. Monolithic lithium disilicate glass-ceramics with higher mechanical properties showed more wear loss, however, they did not fracture and produced less wear loss of antagonists. Copyright © 2017 Elsevier Ltd. All rights reserved.

Intervertebral disk (image)

MedlinePlus

... are filled with a gelatinous substance, called the nucleus pulposus, which provides cushioning to the spinal column. ... fibrosus is a fibrocartilaginous ring that surrounds the nucleus pulposus, which keeps the nucleus pulposus in tact ...

Quantification of the association between intervertebral disk calcification and disk herniation in Dachshunds.

PubMed

Jensen, Vibeke F; Beck, Sarah; Christensen, Knud A; Arnbjerg, Jens

2008-10-01

To quantify the association between intervertebral disk calcification and disk herniation in Dachshunds. Longitudinal study. 61 Dachshunds that had been radiographically screened for calcification of intervertebral disks at 2 years of age in other studies. Thirty-seven of the dogs had survived to the time of the present study and were > or = 8 years of age; 24 others had not survived. Radiographic examination of 36 surviving dogs was performed, and information on occurrence of disk calcification at 2 years of age were obtained from records of all 61 Dachshunds. Information on occurrence of disk herniation between 2 and 8 years of age was obtained from owners via questionnaire. Associations between numbers of calcified disks and disk herniation were analyzed via maximum likelihood logistic regression. Disk calcification at 2 years of age was a significant predictor of clinical disk herniation (odds ratio per calcified disk, 1.42; 95% confidence interval, 1.19 to 1.81). Number of calcified disks in the full vertebral column was a better predictor than number of calcified disks between vertebrae T10 and L3. Numbers of calcified disks at > or = 8 years of age and at 2 years of age were significantly correlated. Number of calcified disks at 2 years of age was a good predictor of clinical disk herniation in Dachshunds. Because of the high heritability of disk calcification, it is possible that an effective reduction in occurrence of severe disk herniation in Dachshunds could be obtained by selective breeding against high numbers of calcified disks at 2 years of age.

Status of HVCMOS developments for ATLAS

NASA Astrophysics Data System (ADS)

Perić, I.; Blanco, R.; Casanova Mohr, R.; Ehrler, F.; Guezzi Messaoud, F.; Krämer, C.; Leys, R.; Prathapan, M.; Schimassek, R.; Schöning, A.; Vilella Figueras, E.; Weber, A.; Zhang, H.

2017-02-01

This paper describes the status of the developments made by ATLAS HVCMOS and HVMAPS collaborations. We have proposed two HVCMOS sensor concepts for ATLAS pixels—the capacitive coupled pixel detector (CCPD) and the monolithic detector. The sensors have been implemented in three semiconductor processes AMS H18, AMS H35 and LFoundry LFA15. Efficiency of 99.7% after neutron irradiation to 1015 neq/cm2W has been measured with the small area CCPD prototype in AMS H18 technology. About 84% of the particles are detected with a time resolution better than 25 ns. The sensor was implemented on a low resistivity substrate. The large area demonstrator sensor in AMS H35 process has been designed, produced and successfully tested. The sensor has been produced on different high resistivity substrates ranging from 80 Ωcm to more than 1 kΩ. Monolithic- and hybrid readout are both possible. In August 2016, six different monolithic pixel matrices for ATLAS with a total area of 1 cm2 have been submitted in LFoundry LFA15 process. The matrices implement column drain and triggered readout as well as waveform sampling capability on pixel level. Design details will be presented.

Tracking the Disk Wind Behavior of MAXI J1305-704

NASA Astrophysics Data System (ADS)

Sinclair, Kimberly Poppy; Miller, Jon M.

2017-01-01

There is still much to be understood about black hole accretion disks and their relationship to black hole disk winds. In an attempt to better understand these relationships, we have analyzed the x-ray transient black hole binary MAXI J1305-704 during its outburst in 2012 in order to draw conclusions about the parameters of its disk. The source showed strong absorption signs, as detected by Chandra, on April 21, 2012. From this date on, we analyzed SWIFT observations of the source, using XSPEC from HEASOFT, in order to find strong signals of absorption. By modeling 67 successive observations over the period of 74 days, we were able to closely track the evolution of various disk properties, from inner disk temperature, to power law index, to column density. We could also analyze various parameter relationships in order to determine if there is a statistically significant correlation between any of the properties of a disk. We found that there are strong linear relationships between disk temperature & ionization, photon index & disk temperature, and photon index & ionization. These relationships seem to imply that the corona, in addition to the disk, may be driving the wind properties. Additionally, the counterintuitive relationship between disk temperature and ionization, where disk temperature increases as ionization decreases, seems to imply that there are mechanisms at play in the disk system that are not yet fully understood.

The Disk-Jet Connection in Radio-Loud AGN: The X-Ray Perspective

NASA Technical Reports Server (NTRS)

Sambruna, Rita

2008-01-01

Unification schemes assume that radio-loud active galactic nuclei (AGN) contain an accretion disk and a relativistic jet perpendicular to the disk, and an obscuring molecular torus. The jet dominance decreases with larger viewing angles from blazars to Broad-Line and Narrow-Line Radio Galaxies. A fundamental question is how accretion and ejecta are related. The X-rays provide a convenient window to study these issues, as they originate in the innermost nuclear regions and penetrate large obscuring columns. I review the data, using observations by Chandra but also from other currently operating high-energy experiments. Synergy with the upcoming GLAST mission will also be highlighted.

Reliability of macroscopic grading of intervertebral disk degeneration in dogs by use of the Thompson system and comparison with low-field magnetic resonance imaging findings.

PubMed

Bergknut, Niklas; Grinwis, Guy; Pickee, Emile; Auriemma, Edoardo; Lagerstedt, Anne-Sofie; Hagman, Ragnvi; Hazewinkel, Herman A W; Meij, Björn P

2011-07-01

To evaluate the reliability of the Thompson system for use in grading the gross pathological changes of intervertebral disk (IVD) degeneration in dogs and to investigate the agreement between gross pathological findings and low-field (0.2-T) magnetic resonance imaging (MRI) findings. Vertebral columns from cadavers of 19 dogs of various ages, breeds, and origins. 182 intervertebral segments were collected from 19 canine cadavers. Sagittal T2-weighted MRI of the T11 through S1 portion of the vertebral column was performed within 24 hours after the dogs were euthanized. The vertebral columns were subsequently divided in the midsagittal plane, and high-resolution photographs were obtained of each intervertebral segment (end plate-disk-end plate). The MRI images and photographs were graded separately in a blinded manner by 4 observers who used both Pfirrmann and Thompson grading criteria. The interobserver agreement for Thompson scores ranged from 0.76 to 0.88, and the intraobserver agreement ranged from 0.88 to 0.94 (Cohen weighted κ analysis). Agreement between scores for the Pfirrmann and Thompson grading criteria was κ = 0.70. Grading of IVD degeneration in dogs by use of the Thompson system resulted in high interobserver and intraobserver agreement, and scores for the Thompson system had substantial agreement with low-field MRI findings graded by use of the Pfirrmann system. This suggested that low-field MRI can be used to diagnose IVD degeneration in dogs.

Performance of a SiPM based semi-monolithic scintillator PET detector

NASA Astrophysics Data System (ADS)

Zhang, Xianming; Wang, Xiaohui; Ren, Ning; Kuang, Zhonghua; Deng, Xinhan; Fu, Xin; Wu, San; Sang, Ziru; Hu, Zhanli; Liang, Dong; Liu, Xin; Zheng, Hairong; Yang, Yongfeng

2017-10-01

A depth encoding PET detector module using semi-monolithic scintillation crystal single-ended readout by a SiPM array was built and its performance was measured. The semi-monolithic scintillator detector consists of 11 polished LYSO slices measuring 1  ×  11.6  ×  10 mm3. The slices are glued together with enhanced specular reflector (ESR) in between and outside of the slices. The bottom surface of the slices is coupled to a 4  ×  4 SiPM array with a 1 mm light guide and silicon grease between them. No reflector is used on the top surface and two sides of the slices to reduce the scintillation photon reflection. The signals of the 4  ×  4 SiPM array are grouped along rows and columns separately into eight signals. Four SiPM column signals are used to identify the slices according to the center of the gravity of the scintillation photon distribution in the pixelated direction. Four SiPM row signals are used to estimate the y (monolithic direction) and z (depth of interaction) positions according to the center of the gravity and the width of the scintillation photon distribution in the monolithic direction, respectively. The detector was measured with 1 mm sampling interval in both the y and z directions with electronic collimation by using a 0.25 mm diameter 22Na point source and a 1  ×  1  ×  20 mm3 LYSO crystal detector. An average slice based energy resolution of 14.9% was obtained. All slices of 1 mm thick were clearly resolved and a detector with even thinner slices could be used. The y positions calculated with the center of gravity method are different for interactions happening at the same y, but different z positions due to depth dependent edge effects. The least-square minimization and the maximum likelihood positioning algorithms were developed and both methods improved the spatial resolution at the edges of the detector as compared with the center of gravity method. A mean absolute error (MAE) which is defined as the probability-weighted mean of the absolute value of the positioning error is used to evaluate the spatial resolution. An average MAE spatial resolution of ~1.15 mm was obtained in both y and z directions without rejection of the multiple scattering events. The average MAE spatial resolution was ~0.7 mm in both y and z directions after the multiple scattering events were rejected. The timing resolution of the detector is 575 ps. In the next step, long rectangle detector will be built to reduce edge effects and improve the spatial resolution of the semi-monolithic detector. Thick detector up to 20 mm will be explored and the positioning algorithms will be further optimized.

Performance of a SiPM based semi-monolithic scintillator PET detector.

PubMed

Zhang, Xianming; Wang, Xiaohui; Ren, Ning; Kuang, Zhonghua; Deng, Xinhan; Fu, Xin; Wu, San; Sang, Ziru; Hu, Zhanli; Liang, Dong; Liu, Xin; Zheng, Hairong; Yang, Yongfeng

2017-09-21

A depth encoding PET detector module using semi-monolithic scintillation crystal single-ended readout by a SiPM array was built and its performance was measured. The semi-monolithic scintillator detector consists of 11 polished LYSO slices measuring 1  ×  11.6  ×  10 mm 3 . The slices are glued together with enhanced specular reflector (ESR) in between and outside of the slices. The bottom surface of the slices is coupled to a 4  ×  4 SiPM array with a 1 mm light guide and silicon grease between them. No reflector is used on the top surface and two sides of the slices to reduce the scintillation photon reflection. The signals of the 4  ×  4 SiPM array are grouped along rows and columns separately into eight signals. Four SiPM column signals are used to identify the slices according to the center of the gravity of the scintillation photon distribution in the pixelated direction. Four SiPM row signals are used to estimate the y (monolithic direction) and z (depth of interaction) positions according to the center of the gravity and the width of the scintillation photon distribution in the monolithic direction, respectively. The detector was measured with 1 mm sampling interval in both the y and z directions with electronic collimation by using a 0.25 mm diameter 22 Na point source and a 1  ×  1  ×  20 mm 3 LYSO crystal detector. An average slice based energy resolution of 14.9% was obtained. All slices of 1 mm thick were clearly resolved and a detector with even thinner slices could be used. The y positions calculated with the center of gravity method are different for interactions happening at the same y, but different z positions due to depth dependent edge effects. The least-square minimization and the maximum likelihood positioning algorithms were developed and both methods improved the spatial resolution at the edges of the detector as compared with the center of gravity method. A mean absolute error (MAE) which is defined as the probability-weighted mean of the absolute value of the positioning error is used to evaluate the spatial resolution. An average MAE spatial resolution of ~1.15 mm was obtained in both y and z directions without rejection of the multiple scattering events. The average MAE spatial resolution was ~0.7 mm in both y and z directions after the multiple scattering events were rejected. The timing resolution of the detector is 575 ps. In the next step, long rectangle detector will be built to reduce edge effects and improve the spatial resolution of the semi-monolithic detector. Thick detector up to 20 mm will be explored and the positioning algorithms will be further optimized.

ROSAT survey of emission from Be stars

NASA Technical Reports Server (NTRS)

Grady, Carol

1993-01-01

ROSAT pointed observations of bright, classical Be stars have demonstrated that detection of soft x-rays at a level expected for normal B stars of comparable T(sub eff) and luminosity is anti-correlated with the presence of episodes of enhanced mass ejection and formation of a dense, moderately ionized equatorial circumstellar disk. At epochs of lower than average disk column density, x-ray flaring has been detected in 2 Be stars, lambda Eri and pi Aqr.

Modeling X-ray Absorbers in AGNs with MHD-Driven Accretion-Disk Winds

NASA Astrophysics Data System (ADS)

Fukumura, Keigo; Kazanas, D.; Shrader, C. R.; Tombesi, F.; Contopoulos, J.; Behar, E.

2013-04-01

We have proposed a systematic view of the observed X-ray absorbers, namely warm absorbers (WAs) in soft X-ray and highly-ionized ultra-fast outflows (UFOs), in the context of magnetically-driven accretion-disk wind models. While potentially complicated by variability and thermal instability in these energetic outflows, in this simplistic model we have calculated 2D kinematic field as well as density and ionization structure of the wind with density profile of 1/r corresponding to a constant column distribution per decade of ionization parameter. In particular we show semi-analytically that the inner layer of the disk-wind manifests itself as the strongly-ionized fast outflows while the outer layer is identified as the moderately-ionized absorbers. The computed characteristics of these two apparently distinct absorbers are consistent with X-ray data (i.e. a factor of ~100 difference in column and ionization parameters as well as low wind velocity vs. near-relativistic flow). With the predicted contour curves for these wind parameters one can constrain allowed regions for the presence of WAs and UFOs.The model further implies that the UFO's gas pressure is comparable to that of the observed radio jet in 3C111 suggesting that the magnetized disk-wind with density profile of 1/r is a viable agent to help sustain such a self-collimated jet at small radii.

Development of radiation tolerant monolithic active pixel sensors with fast column parallel read-out

NASA Astrophysics Data System (ADS)

Koziel, M.; Dorokhov, A.; Fontaine, J.-C.; De Masi, R.; Winter, M.

2010-12-01

Monolithic active pixel sensors (MAPS) [1] (Turchetta et al., 2001) are being developed at IPHC—Strasbourg to equip the EUDET telescope [2] (Haas, 2006) and vertex detectors for future high energy physics experiments, including the STAR upgrade at RHIC [3] (T.S. Collaboration, 2005) and the CBM experiment at FAIR/GSI [4] (Heuser, 2006). High granularity, low material budget and high read-out speed are systematically required for most applications, complemented, for some of them, with high radiation tolerance. A specific column-parallel architecture, implemented in the MIMOSA-22 sensor, was developed to achieve fast read-out MAPS. Previous studies of the front-end architecture integrated in this sensor, which includes in-pixel amplification, have shown that the fixed pattern noise increase consecutive to ionizing radiation can be controlled by means of a negative feedback [5] (Hu-Guo et al., 2008). However, an unexpected rise of the temporal noise was observed. A second version of this chip (MIMOSA-22bis) was produced in order to search for possible improvements of the radiation tolerance, regarding this type of noise. In this prototype, the feedback transistor was tuned in order to mitigate the sensitivity of the pixel to ionizing radiation. The performances of the pixels after irradiation were investigated for two types of feedback transistors: enclosed layout transistor (ELT) [6] (Snoeys et al., 2000) and "standard" transistor with either large or small transconductance. The noise performance of all test structures was studied in various conditions (expected in future experiments) regarding temperature, integration time and ionizing radiation dose. Test results are presented in this paper. Based on these observations, ideas for further improvement of the radiation tolerance of column parallel MAPS are derived.

Sub-1min separation in sequential injection chromatography for determination of synthetic water-soluble dyes in pharmaceutical formulation.

PubMed

Davletbaeva, Polina; Chocholouš, Petr; Bulatov, Andrey; Šatínský, Dalibor; Solich, Petr

2017-09-05

Sequential Injection Chromatography (SIC) evolved from fast and automated non-separation Sequential Injection Analysis (SIA) into chromatographic separation method for multi-element analysis. However, the speed of the measurement (sample throughput) is due to chromatography significantly reduced. In this paper, a sub-1min separation using medium polar cyano monolithic column (5mm×4.6mm) resulted in fast and green separation with sample throughput comparable with non-separation flow methods The separation of three synthetic water-soluble dyes (sunset yellow FCF, carmoisine and green S) was in a gradient elution mode (0.02% ammonium acetate, pH 6.7 - water) with flow rate of 3.0mLmin -1 corresponding with sample throughput of 30h -1 . Spectrophotometric detection wavelengths were set to 480, 516 and 630nm and 10Hz data collection rate. The performance of the separation was described and discussed (peak capacities 3.48-7.67, peak symmetries 1.72-1.84 and resolutions 1.42-1.88). The method was represented by validation parameters: LODs of 0.15-0.35mgL -1 , LOQs of 0.50-1.25mgL -1 , calibration ranges 0.50-150.00mgL -1 (r>0.998) and repeatability at 10.0mgL -1 of RSD≤0.98% (n=6). The method was used for determination of the dyes in "forest berries" colored pharmaceutical cough-cold formulation. The sample matrix - pharmaceuticals and excipients were not interfering with vis determination because of no retention in the separation column and colorless nature. The results proved the concept of fast and green chromatography approach using very short medium polar monolithic column in SIC. Copyright © 2017 Elsevier B.V. All rights reserved.

Reversible entrapment of plasmid deoxyribonucleic acid on different chromatographic supports.

PubMed

Gabor, Boštjan; Černigoj, Urh; Barut, Miloš; Štrancar, Aleš

2013-10-11

HPLC based analytical assay is a powerful technique that can be used to efficiently monitor plasmid DNA (pDNA) purity and quantity throughout the entire purification process. Anion exchange monolithic and non-porous particle based stationary phases were used to study the recovery of the different pDNA isoforms from the analytical column. Three differently sized pDNA molecules of 3.0kbp, 5.2kbp and 14.0kbp were used. Plasmid DNA was injected onto columns under the binding conditions and the separation of the isoforms took place by increasing the ionic strength of the elution buffer. While there was no substantial decrease of the recovered supercoiled and linear isoforms of the pDNA with the increase of the plasmid size and with the increase of the flow rate (recoveries in all cases larger than 75%), a pronounced decrease of the oc isoform recovery was observed. The entrapment of the oc pDNA isoform occurred under non-binding conditions as well. The partial oc isoform elution from the column could be achieved by decreasing the flow rate of the elution mobile phase. The results suggested a reversible entrapment of the oc isoform in the restrictions within the pores of the monolithic material as well as within the intra-particle space of the non-porous particles. This phenomenon was observed on both types of the stationary phase morphologies and could only be connected to the size of a void space through which the pDNA needs to migrate. A prediction of reversible pDNA entrapment was successfully estimated with the calculation of Peclet numbers, Pe, which defines the ratio between a convective and diffusive mass transport. Copyright © 2013 Elsevier B.V. All rights reserved.

CO AND H{sub 2} ABSORPTION IN THE AA TAURI CIRCUMSTELLAR DISK

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

France, Kevin; Burgh, Eric B.; Schindhelm, Eric

2012-01-01

The direct study of molecular gas in inner protoplanetary disks is complicated by uncertainties in the spatial distribution of the gas, the time variability of the source, and the comparison of observations across a wide range of wavelengths. Some of these challenges can be mitigated with far-ultraviolet spectroscopy. Using new observations obtained with the Hubble Space Telescope Cosmic Origins Spectrograph, we measure column densities and rovibrational temperatures for CO and H{sub 2} observed on the line of sight through the AA Tauri circumstellar disk. CO A - X absorption bands are observed against the far-UV continuum. The CO absorption ismore » characterized by log{sub 10}(N({sup 12}CO)) = 17.5 {+-} 0.5 cm{sup -2} and T{sub rot}(CO) = 500{sup +500}{sub -200} K, although this rotational temperature may underestimate the local kinetic temperature of the CO-bearing gas. We also detect {sup 13}CO in absorption with an isotopic ratio of {approx}20. We do not observe H{sub 2} absorption against the continuum; however, hot H{sub 2} (v > 0) is detected in absorption against the Ly{alpha} emission line. We measure the column densities in eight individual rovibrational states, determining a total log{sub 10}(N(H{sub 2})) = 17.9{sup +0.6}{sub -0.3} cm{sup -2} with a thermal temperature of T(H{sub 2}) = 2500{sup +800}{sub -700} K. The high temperature of the molecules, the relatively small H{sub 2} column density, and the high inclination of the AA Tauri disk suggest that the absorbing gas resides in an inner disk atmosphere. If the H{sub 2} and CO are cospatial within a molecular layer {approx}0.6 AU thick, this region is characterized by {approx} 10{sup 5} cm{sup -3} with an observed (CO/H{sub 2}) ratio of {approx}0.4. We also find evidence for a departure from a purely thermal H{sub 2} distribution, suggesting that excitation by continuum photons and H{sub 2} formation may be altering the level populations in the molecular gas.« less

Molecular diagnostics of FUV and accretion-related heating in protoplanetary disks

NASA Astrophysics Data System (ADS)

Adamkovics, Mate; Najita, Joan R.

2017-10-01

Emission lines from the terrestrial planet forming regions of disks are diagnostic of both the physical processes that heat the gas and the chemistry that determines the inventory of nebular material available during the epoch of planet formation. Interpreting emission spectra is informed by models of radiative, thermal, physical, and chemical processes, such as: (i) the radiation transfer of X-rays and FUV --- both continuum and Ly-alpha, (ii) direct and indirect heating processes such as the photoelectric effect and photochemical heating, (iii) heating related to turbulent processes and viscous dissipation, and (iv) gas phase chemical reaction kinetics. Many of these processes depend on a the spatial distribution of dust grains and their properties, which temporally evolve during the lifetime of the disk and the formation of planets. Studies of disks atmospheres often predict a layered structure of hot (a few thousand K) atomic gas overlying warm (a few hundred K) molecular gas, which is generally consistent with the isothermal slab emission models that are used to interpret emission spectra. However, detailed comparison between observed spectra and models (e.g., comparing the total columns and the radial extent of warm emitting species) is rare.We present results including the implementation of Ly-alpha scattering, which is an important part of the photochemical heating and FUV heating radiation budget. By including these processes we find a new component of the disk atmosphere; hot molecular gas at ~2000K within radial distances of ~0.5AU, which is consistent with observations of UV-fluorescent H2 emission (Ádámkovics, Najita & Glassgold, 2016). Constraining the most optimistic contribution of radiative heating mechanisms via X-rays and FUV together with a favorable comparison to observations, allows us to explore and evaluate additional heating mechanisms. We find that the total columns of warm (90-400K) emitting molecules such as CO, arising directly below the irradiated molecular layer, are diagnostic of the role of turbulent (viscous) mechanical heating. We discuss how the total columns of warm molecules in this layer may be diagnostic of the magnetorotational instability (Najita & Ádámkovics, 2017).

Integrated enzyme reactor and high resolving chromatography in "sub-chip" dimensions for sensitive protein mass spectrometry.

PubMed

Hustoft, Hanne Kolsrud; Brandtzaeg, Ole Kristian; Rogeberg, Magnus; Misaghian, Dorna; Torsetnes, Silje Bøen; Greibrokk, Tyge; Reubsaet, Léon; Wilson, Steven Ray; Lundanes, Elsa

2013-12-16

Reliable, sensitive and automatable analytical methodology is of great value in e.g. cancer diagnostics. In this context, an on-line system for enzymatic cleavage of proteins, subsequent peptide separation by liquid chromatography (LC) with mass spectrometric detection has been developed using "sub-chip" columns (10-20 μm inner diameter, ID). The system could detect attomole amounts of isolated cancer biomarker progastrin-releasing peptide (ProGRP), in a more automatable fashion compared to previous methods. The workflow combines protein digestion using an 20 μm ID immobilized trypsin reactor with a polymeric layer of 2-hydroxyethyl methacrylate-vinyl azlactone (HEMA-VDM), desalting on a polystyrene-divinylbenzene (PS-DVB) monolithic trap column, and subsequent separation of resulting peptides on a 10 μm ID (PS-DVB) porous layer open tubular (PLOT) column. The high resolution of the PLOT columns was maintained in the on-line system, resulting in narrow chromatographic peaks of 3-5 seconds. The trypsin reactors provided repeatable performance and were compatible with long-term storage.

Simultaneous Liquid Chromatographic Determination of 10 Ultra-Violet Filters in Sunscreens.

PubMed

Wharton, Mary; Geary, Michael; O'Connor, Niamh; Curtin, Laura; Ketcher, Krystal

2015-09-01

A rapid HPLC method was developed for the simultaneous determination of 10 UV filters found in sunscreen. The following UV filters were analyzed in this method; 2-phenylbenzimidazole-5-sulfonic acid, benzophenone-3, isoamyl p-methoxycinnamate, 4-methylbenzylidene camphor, octocrylene, ethylhexyl dimethyl 4-aminobenzoic acid, ethylhexyl methoxycinnamate, butyl methoxydibenzoylmethane, ethylhexyl salicylate and homosalate. The method was developed on two columns; a Thermo Hypersil C18 BDS, 3 µm column (4.6 × 100 mm) and a Chromolith RP-18e Monolithic column (4.6 × 100 mm). The same mobile phase of ethanol and 1% acetic acid (70:30, v/v) was employed for both columns. The separation of the 10 UV filters was carried out successfully on both columns; the optimal resolution was obtained on the Thermo Scientific Hypersil column in a time frame of 7 min. An isocratic elution utilizing ethanol and acetic acid (70:30, v/v) at a temperature of 35°C was employed. The method was applied to a number of commercial samples of sunscreen and lotions and was validated according to International Conference on Harmonisation guidelines for selectivity, linearity, accuracy, precision and robustness. A comparison of the performances of both columns was also carried out. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Binding mechanisms for histamine and agmatine ligands in plasmid deoxyribonucleic acid purifications.

PubMed

Sousa, Ângela; Pereira, Patrícia; Sousa, Fani; Queiroz, João A

2014-10-31

Histamine and agmatine amino acid derivatives were immobilized into monolithic disks, in order to combine the specificity and selectivity of the ligand with the high mass transfer and binding capacity offered by monolithic supports, to purify potential plasmid DNA biopharmaceuticals. Different elution strategies were explored by changing the type and salt concentration, as well as the pH, in order to understand the retention pattern of different plasmids isoforms The pVAX1-LacZ supercoiled isoform was isolated from a mixture of pDNA isoforms by using NaCl increasing stepwise gradient and also by ammonium sulfate decreasing stepwise gradient, in both histamine and agmatine monoliths. Acidic pH in the binding buffer mainly strengthened ionic interactions with both ligands in the presence of sodium chloride. Otherwise, for histamine ligand, pH values higher than 7 intensified hydrophobic interactions in the presence of ammonium sulfate. In addition, circular dichroism spectroscopy studies revealed that the binding and elution chromatographic conditions, such as the combination of high ionic strength with extreme pH values can reversibly influence the structural stability of the target nucleic acid. Therefore, ascending sodium chloride gradients with pH manipulation can be preferable chromatographic conditions to be explored in the purification of plasmid DNA biopharmaceuticals, in order to avoid the environmental impact of ammonium sulfate. Copyright © 2014. Published by Elsevier B.V.

Preparation of open tubular capillary columns by in situ ring-opening polymerization and their applications in cLC-MS/MS analysis of tryptic digest.

PubMed

Wang, Hongwei; Yao, Yating; Li, Ya; Ma, Shujuan; Peng, Xiaojun; Ou, Junjie; Ye, Mingliang

2017-08-01

An open tubular (OT) column (25 μm i.d.) was prepared by in situ ring-opening polymerization of octaglycidyldimethylsilyl polyhedral oligomeric silsesquioxanes (POSS-epoxy) with 4-aminophenyl disulfide (APDS) in a binary porogenic system of ethanol/H 2 O. It was found that porogenic composition played an important role in the formation of OT stationary phases. The ratio of ethanol/H 2 O at 6/1 (v/v) would lead to the fabrication of hybrid monoliths, while the ratio of ethanol/H 2 O at 13/1 (v/v) would result in the synthesis of OT phases. In addition, the effects of precursor content and reaction duration on the thickness of OT stationary phases were investigated. Either lower precursor content or shorter reaction duration would produce thinner layer of OT column. The repeatability of OT columns was evaluated through relative standard deviation (RSD%) with benzene as the analyte. The run-to-run, column-to-column and batch-to-batch repeatabilities were 1.7%, 4.8% and 5.6%, respectively, exhibiting satisfactory repeatability of the OT column. Then tryptic digest of mouse liver proteins was used to evaluate the performance of the resulting OT columns (25 μm i.d. × 2.5 m in length) by cLC-MS/MS analysis, demonstrating their potential in proteome analysis. Copyright © 2017 Elsevier B.V. All rights reserved.

YOUNG STARS IN AN OLD BULGE: A NATURAL OUTCOME OF INTERNAL EVOLUTION IN THE MILKY WAY

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

Ness, M.; Debattista, Victor P.; Cole, D. R.

2014-06-01

The center of our disk galaxy, the Milky Way, is dominated by a boxy/peanut-shaped bulge. Numerous studies of the bulge based on stellar photometry have concluded that the bulge stars are exclusively old. The perceived lack of young stars in the bulge strongly constrains its likely formation scenarios, providing evidence that the bulge is a unique population that formed early and separately from the disk. However, recent studies of individual bulge stars using the microlensing technique have reported that they span a range of ages, emphasizing that the bulge may not be a monolithic structure. In this Letter we demonstratemore » that the presence of young stars that are located predominantly nearer to the plane is expected for a bulge that has formed from the disk via dynamical instabilities. Using an N-body+ smoothed particle hydrodynamics simulation of a disk galaxy forming out of gas cooling inside a dark matter halo and forming stars, we find a qualitative agreement between our model and the observations of younger metal-rich stars in the bulge. We are also able to partially resolve the apparent contradiction in the literature between results that argue for a purely old bulge population and those that show a population comprised of a range in ages; the key is where to look.« less

Water and Solute Mass Transport in Soils Developed on glacial Drift: A Br Tracer Investigation Using Instrumented Soil Monoliths at an Agricultural Long Term Ecological Research Site (Kellogg Biological Station, Hickory Corners, Southern Michigan)

NASA Astrophysics Data System (ADS)

Jin, L.; Hamilton, S. K.; Walter, L. M.

2004-12-01

Hydrologic processes control the residence time of water in the soil column. This is of central importance in understanding mineral weathering rates in terms of reaction kinetics and solute transport. In order to better quantify the coupling between water and solute mass transport and to better define controls on carbonate and aluminosilicates weathering rates, we have conducted bromide-tracer introduction experiments at four replicate soil monoliths (4 m3 volume) instrumented and managed by the KBS-LTER. Monolith soils are developed on the pitted outwash plain of the morainic system left by the last retreat of the Wisconsin glaciation, around 12,000 years ago. Soil profiles from the monolith sections extend to 200 cm and they were sampled and characterized texturally and mineralogically. Quartz and feldspar are dominant throughout the soil profile, while carbonates and hornblende occur only in deeper soil horizons. The four replicate monoliths are instrumented with gas and soil water sampling devices (Prenart tension lysimeters) at various depths. The monoliths also have a large capacity tray at the bottom, which permits collection of water for weight and chemical determinations. A bromide tracer solution (as lithium bromide) was applied to coincide as closely as possible with a major snowmelt event (2/27/04). The saturated and unsaturated transport of bromide through the four monoliths was followed as a function of time and soil profile depth for the duration of the snowmelt as well as intermittent rain events. Because the soil was saturated at the time of bromide application, the bromide solution is expected to move rapidly through macropores, followed by slower movement into micropores. The unsaturated transport of bromide is largely controlled by the intensity and duration of the rains if it is dominated by piston flow as opposed to preferential channel flow. In general, the tracer moved through the shallow soils very quickly, which is shown by early sharp peaks in bromide concentrations. Transport of bromide into deeper soil horizons, however, differs markedly among the four monoliths. Even within a given monolith, waters sampled at the same depth by different tension lysimeters show a very different pattern of bromide transport over time with some lyimeters suggesting piston flow, while others in the same monolith suggest preferential channel flow. These differences are likely driven by heterogeneous soil textures. The water recovered from the monolith trays over the first three months of the study period is between 80 and 90 percent of the total precipitation recorded at the LTER site. This recovery is reasonable given the fact that temperature was low and crops were not yet actively growing. The recovery of bromide is different among the monoliths and in general is less than 50 percent, which means more than 50 percent of tracer is still in the soils even after three months. Residence time of water has been calculated after some assumptions on the breakthrough curve. The water mass transport constraints imposed by the bromide tracer study will be utilized in concert with additional data on soil water geochemistry.

A study of extreme-ultraviolet emission from cataclysmic variables

NASA Technical Reports Server (NTRS)

Polidan, Ronald S.; Mauche, Christopher W.; Wade, Richard A.

1990-01-01

Voyager far- and extreme UV spectrophotometric observations of five cataclysmic variables (the dwarf novae SS Cyg and VW Hyi and the novalike variables V3885 Sgr, RW Sex, and IX Vel) are combined with neutral hydrogen column densities derived from the curve-of-growth analysis of interstellar absorption lines in high-resolution IUE spectra to place upper limits on the emitted flux in the 600-700 A EUV band. The Voyager observations of VW Hyi were obtained during both normal and superoutbursts. Detailed accretion disk model calculations show that most of the 600-700 A flux in these systems should originate in the inner accretion disk rather than in the boundary layer. For VW Hyi, the low neutral hydrogen column and excellent Voyager superoutburst data place the observed upper limit to the 600-700 A flux well below the expected EUV flux from the model calculations.

Signatures of Hot Molecular Hydrogen Absorption from Protoplanetary Disks. I. Non-thermal Populations

NASA Astrophysics Data System (ADS)

Hoadley, Keri; France, Kevin; Arulanantham, Nicole; Loyd, R. O. Parke; Kruczek, Nicholas

2017-09-01

The environment around protoplanetary disks (PPDs) regulates processes that drive the chemical and structural evolution of circumstellar material. We perform a detailed empirical survey of warm molecular hydrogen (H2) absorption observed against H I-Lyα (Lyα: λ1215.67) emission profiles for 22 PPDs, using archival Hubble Space Telescope ultraviolet (UV) spectra to identify H2 absorption signatures and quantify the column densities of H2 ground states in each sightline. We compare thermal equilibrium models of H2 to the observed H2 rovibrational level distributions. We find that, for the majority of targets, there is a clear deviation in high-energy states (T exc ≳ 20,000 K) away from thermal equilibrium populations (T(H2) ≳ 3500 K). We create a metric to estimate the total column density of non-thermal H2 (N(H2)nLTE) and find that the total column densities of thermal (N(H2)) and N(H2)nLTE correlate for transition disks and targets with detectable C IV-pumped H2 fluorescence. We compare N(H2) and N(H2)nLTE to circumstellar observables and find that N(H2)nLTE correlates with X-ray and far-UV luminosities, but no correlations are observed with the luminosities of discrete emission features (e.g., Lyα, C IV). Additionally, N(H2) and N(H2)nLTE are too low to account for the H2 fluorescence observed in PPDs, so we speculate that this H2 may instead be associated with a diffuse, hot, atomic halo surrounding the planet-forming disk. We create a simple photon-pumping model for each target to test this hypothesis and find that Lyα efficiently pumps H2 levels with T exc ≥ 10,000 K out of thermal equilibrium.

Simultaneous separation of inorganic anions and metal-citrate complexes on a zwitterionic stationary phase with on-column complexation.

PubMed

Nesterenko, Ekaterina P; Nesterenko, Pavel N; Paull, Brett

2008-12-05

The retention and separation selectivity of inorganic anions and on-column derivatised negatively charged citrate or oxalate metal complexes on reversed-phase stationary phases dynamically coated with N-(dodecyl-N,N-dimethylammonio)undecanoate (DDMAU) has been investigated. The retention mechanism for the metal-citrate complexes was predominantly anion exchange, although the amphoteric/zwitterionic nature of the stationary phase coating undoubtedly also contributed to the unusual separation selectivity shown. A mixture of 10 inorganic anions and metal cations was achieved using a 20 cm monolithic DDMAU modified column and a 1 mM citrate eluent, pH 4.0, flow rate equal to 0.8 mL/min. Selectivity was found to be strongly pH dependent, allowing additional scope for manipulation of solute retention, and thus application to complex samples. This is illustrated with the analysis of an acidic mine drainage sample with a range of inorganic anions and transition metal cations, varying significantly in their concentrations levels.

Chromato-panning: an efficient new mode of identifying suitable ligands from phage display libraries

PubMed Central

Noppe, Wim; Plieva, Fatima; Galaev, Igor Yu; Pottel, Hans; Deckmyn, Hans; Mattiasson, Bo

2009-01-01

Background Phage Display technology is a well established technique for high throughput screening of affinity ligands. Here we describe a new compact chromato-panning procedure for selection of suitable binders from a phage peptide display library. Results Both phages and E. coli cells pass non-hindered through the interconnected pores of macroporous gel, so called cryogel. After coupling a ligand to a monolithic cryogel column, the phage library was applied on the column and non-bound phages were washed out. The selection of strong phage-binders was achieved already after the first panning cycle due to the efficient separation of phage-binders from phage-non-binders in chromatographic mode rather than in batch mode as in traditional biopanning procedures. E. coli cells were applied on the column for infection with the specifically bound phages. Conclusion Chromato-panning allows combining several steps of the panning procedure resulting in 4–8 fold decrease of total time needed for phage selection. PMID:19292898

InGaN/GaN dot-in-nanowire monolithic LEDs and lasers on (001) silicon

NASA Astrophysics Data System (ADS)

Bhattacharya, P.; Hazari, A.; Jahangir, S.

2017-02-01

GaN-based nanowire arrays have been grown on (001)Si substrate by plasma-assisted molecular beam epitaxy and their structural and optical properties have been determined. InxGa1-xN disks inserted in the nanowires behave as quantum dots with emission ranging from visible to near-infrared. We have exploited these nanowire heterostructure arrays to realize light-emitting diodes and diode lasers in which the quantum dots form the active light emitting media. The fabrication and characteristics of 630nm light-emitting diodes and 1.3μm edge-emitting diode lasers are described.

Wear of human enamel opposing monolithic zirconia, glass ceramic, and composite resin: an in vitro study.

PubMed

Sripetchdanond, Jeerapa; Leevailoj, Chalermpol

2014-11-01

Demand is increasing for ceramic and composite resin posterior restorations. However, ceramics are recognized for their high abrasiveness to opposing dental structure. The purpose of this study was to investigate the wear of enamel as opposed to dental ceramics and composite resin. Twenty-four test specimens (antagonists), 6 each of monolithic zirconia, glass ceramic, composite resin, and enamel, were prepared into cylindrical rods. Enamel specimens were prepared from 24 extracted human permanent molar teeth. Enamel specimens were abraded against each type of antagonist with a pin-on-disk wear tester under a constant load of 25 N at 20 rpm for 4800 cycles. The maximum depth of wear (Dmax), mean depth of wear (Da), and mean surface roughness (Ra) of the enamel specimens were measured with a profilometer. All data were statistically analyzed by 1-way ANOVA, followed by the Tukey test (α=.05). A paired t test was used to compare the Ra of enamel at baseline and after testing. The wear of both the enamel and antagonists was evaluated qualitatively with scanning electron microscopic images. No significant differences were found in enamel wear depth (Dmax, Da) between monolithic zirconia (2.17 ±0.80, 1.83 ±0.75 μm) and composite resin (1.70 ±0.92, 1.37 ±0.81 μm) or between glass ceramic (8.54 ±2.31, 7.32 ±2.06 μm) and enamel (10.72 ±6.31, 8.81 ±5.16 μm). Significant differences were found when the enamel wear depth caused by monolithic zirconia and composite resin was compared with that of glass ceramic and enamel (P<.001). The Ra of enamel specimens increased significantly after wear tests with monolithic zirconia, glass ceramic, and enamel (P<.05); however, no difference was found among these materials. Within the limitations of this in vitro study, monolithic zirconia and composite resin resulted in less wear depth to human enamel compared with glass ceramic and enamel. All test materials except composite resin similarly increased the enamel surface roughness after wear testing. Copyright © 2014 Editorial Council for the Journal of Prosthetic Dentistry. Published by Elsevier Inc. All rights reserved.

Stress-strain state of the structure in the service area of underground railway

NASA Astrophysics Data System (ADS)

Barabash, M.; Bashinsky, Y.; Korjakins, A.

2017-10-01

The paper focuses on numerical study how vibration due to underground trains influences the load-bearing building structures. Diagrams of vibration levels for monolithic floor slab depending on frequency are obtained. Levels of vibrations on floor slabs and columns are measured. The simulation of dynamic load from underground railway onto load-bearing building structures is presented as an example with account of load transmission through the soil. Recommendations for generation of design model in dynamic analysis of structure are provided.

Comparison of various types of stationary phases in non-aqueous reversed-phase high-performance liquid chromatography-mass spectrometry of glycerolipids in blackcurrant oil and its enzymatic hydrolysis mixture.

PubMed

Lísa, Miroslav; Holcapek, Michal; Sovová, Helena

2009-11-20

The selection of column packing during the development of high-performance liquid chromatography method is a crucial step to achieve sufficient chromatographic resolution of analyzed species in complex mixtures. Various stationary phases are tested in this paper for the analysis of complex mixture of triacylglycerols (TGs) in blackcurrant oil using non-aqueous reversed-phase (NARP) system with acetonitrile-2-propanol mobile phase. Conventional C(18) column in the total length of 45 cm is used for the separation of TGs according to their equivalent carbon number, the number and positions of double bonds and acyl chain lengths. The separation of TGs and their more polar hydrolysis products after the partial enzymatic hydrolysis of blackcurrant oil in one chromatographic run is achieved using conventional C(18) column. Retention times of TGs are reduced almost 10 times without the loss of the chromatographic resolution using ultra high-performance liquid chromatography with 1.7 microm C(18) particles. The separation in NARP system on C(30) column shows an unusual phenomenon, because the retention order of TGs changes depending on the column temperature, which is reported for the first time. The commercial monolithic column modified with C(18) is used for the fast analysis of TGs to increase the sample throughput but at cost of low resolution.

Analysis of the activation of acetylcholinesterase by carbon nanoparticles using a monolithic immobilized enzyme microreactor: role of the water molecules in the active site gorge.

PubMed

Ibrahim, Firas; Andre, Claire; Iutzeler, Anne; Guillaume, Yves Claude

2013-10-01

A biochromatographic system was used to study the direct effect of carbon nanoparticles (CNPs) on the acetylcholinesterase (AChE) activity. The AChE enzyme was covalently immobilized on a monolithic CIM-disk via its NH2 residues. Our results showed an increase in the AChE activity in presence of CNPs. The catalytic constant (k(cat)) was increased while the Michaelis constant (K(m)) was slightly decreased. This indicated an increase in the enzyme efficiency with increase of the substrate affinity to the active site. The thermodynamic data of the activation mechanism of the enzyme, i.e. ΔH* and ΔS*, showed no change in the substrate interaction mechanism with the anionic binding site. The increase of the enthalpy (ΔH*) and the entropy (ΔS*) with decrease in the free energy of activation (Ea) was related to structural conformation change in the active site gorge. This affected the stability of water molecules in the active site gorge and facilitated water displacement by substrate for entering to the active site of the enzyme.

Evaluation of punching shear strength of flat slabs supported on rectangular columns

NASA Astrophysics Data System (ADS)

Filatov, Valery

2018-03-01

The article presents the methodology and results of an analytical study of structural parameters influence on the value of punching force for the joint of columns and flat reinforced concrete slab. This design solution is typical for monolithic reinforced concrete girderless frames, which have a wide application in the construction of high-rise buildings. As the results of earlier studies show the punching shear strength of slabs at rectangular columns can be lower than at square columns with a similar length of the control perimeter. The influence of two structural parameters on the punching strength of the plate is investigated - the ratio of the side of the column cross-section to the effective depth of slab C/d and the ratio of the sides of the rectangular column Cmax/Cmin. According to the results of the study, graphs of reduction the control perimeter depending on the structural parameters are presented for columns square and rectangular cross-sections. Comparison of results obtained by proposed approach and MC2010 simplified method are shown, that proposed approach gives a more conservative estimate of the influence of the structural parameters. A significant influence of the considered structural parameters on punching shear strength of reinforced concrete slabs is confirmed by the results of experimental studies. The results of the study confirm the necessity of taking into account the considered structural parameters when calculating the punching shear strength of flat reinforced concrete slabs and further development of code design methods.

A reversed phase high performance liquid chromatography method for the determination of fumonisins B1 and B2 in food and feed using monolithic column and positive confirmation by liquid chromatography/tandem mass spectrometry.

PubMed

Khayoon, Wejdan Shakir; Saad, Bahruddin; Salleh, Baharuddin; Ismail, Nor Azliza; Abdul Manaf, Normaliza Hj; Abdul Latiff, Aishah

2010-10-29

The development of a reversed phase high performance liquid chromatography fluorescence method for the determination of the mycotoxins fumonisin B(1) and fumonisin B(2) by using silica-based monolithic column is described. The samples were first extracted using acetonitrile:water (50:50, v/v) and purified by using a C(18) solid phase extraction-based clean-up column. Then, pre-column derivatization for the analyte using ortho-phthaldialdehyde in the presence of 2-mercaptoethanol was carried out. The developed method involved optimization of mobile phase composition using methanol and phosphate buffer, injection volume, temperature and flow rate. The liquid chromatographic separation was performed using a reversed phase Chromolith(®) RP-18e column (100 mm × 4.6 mm) at 30 °C and eluted with a mobile phase of a mixture of methanol and phosphate buffer pH 3.35 (78:22, v/v) at a flow rate of 1.0 mL min(-1). The fumonisins separation was achieved in about 4 min, compared to approximately 20 min by using a C(18) particle-packed column. The fluorescence excitation and emission were at 335 nm and 440 nm, respectively. The limits of detections were 0.01-0.04 μg g(-1) fumonisin B(1) and fumonisin B(2), respectively. Good recoveries were found for spiked samples (0.1, 0.5, 1.5 μg g(-1) fumonisins B(1) and B(2)), ranging from 84.0 to 106.0% for fumonisin B(1) and from 81.0 to 103.0% for fumonisin B(2). Fifty-three samples were analyzed including 39 food and feeds and 14 inoculated corn and rice. Results show that 12.8% of the food and feed samples were contaminated with fumonisin B(1) (range, 0.01-0.51 μg g(-1)) and fumonisin B(2) (0.05 μg g(-1)). The total fumonisins in these samples however, do not exceed the legal limits established by the European Union of 0.8 μg g(-1). Of the 14 inoculated samples, 57.1% contained fumonisin B(1) (0.16-41.0 μg g(-1)) and fumonisin B(2) (range, 0.22-50.0 μg g(-1)). Positive confirmation of selected samples was carried out using liquid chromatography-tandem mass spectrometry, using triple quadrupole analyzer and operated in the multiple reaction monitoring mode. Copyright © 2010 Elsevier B.V. All rights reserved.

Nanoporous Gold Nanocomposites as a Versatile Platform for Plasmonic Engineering and Sensing

PubMed Central

Zhao, Fusheng; Zeng, Jianbo; Shih, Wei-Chuan

2017-01-01

Plasmonic metal nanostructures have shown great potential in sensing applications. Among various materials and structures, monolithic nanoporous gold disks (NPGD) have several unique features such as three-dimensional (3D) porous network, large surface area, tunable plasmonic resonance, high-density hot-spots, and excellent architectural integrity and environmental stability. They exhibit a great potential in surface-enhanced spectroscopy, photothermal conversion, and plasmonic sensing. In this work, interactions between smaller colloidal gold nanoparticles (AuNP) and individual NPGDs are studied. Specifically, colloidal gold nanoparticles with different sizes are loaded onto NPGD substrates to form NPG hybrid nanocomposites with tunable plasmonic resonance peaks in the near-infrared spectral range. Newly formed plasmonic hot-spots due to the coupling between individual nanoparticles and NPG disk have been identified in the nanocomposites, which have been experimentally studied using extinction and surface-enhanced Raman scattering. Numerical modeling and simulations have been employed to further unravel various coupling scenarios between AuNP and NPGDs. PMID:28657586

Inner Disk Structure and Transport Mechanisms in the Transitional Disk around T Cha

NASA Astrophysics Data System (ADS)

Brown, Alexander

2017-08-01

To better understand how Earth-like planets form around low-mass stars, we propose to study the UV (HST), X-ray (XMM), and optical (LCOGT) variability of the young star T Cha. This variability is caused by obscuration of the star by clumpy material in the rim of its inner disk. Changing sight lines through the disk allow measurement of the temperature and column density of both molecular and atomic gas and the physical properties of the dust grains in the well-mixed inner disk, as well as determining the gas-to-dust ratio. The gas-to-dust ratio affects planetesimal growth and disk stability but is difficult to measure in local regions of disks. Three 5 orbit visits, separated by 3-7 days, are required for use of analysis techniques comprising both differential pair-method comparison of spectra with differing A_v (particularly important for determining the dust extinction curve, A_lambda, where removal of the foreground extinction requires multiple epochs) and detailed spectral fitting of gas absorption features at each epoch. The inner disk of T Cha is particularly interesting, because T Cha has a transitional disk with a large gap at 0.2-15 AU in the dust disk and allows study of the gas and dust structure in the terrestrial planet formation zone during this important rapid phase of protoplanetary disk evolution. Characterizing the high energy (UV/X-ray) radiation field is also essential for in-depth studies of the disk in other spectral regions. Results from these observations will have wide relevance to the modeling and understanding of protoplanetary disk structure and evolution, and the complex gas and dust physics and chemistry in disk surface layers.

Constrained Evolution of a Radially Magnetized Protoplanetary Disk: Implications for Planetary Migration

NASA Astrophysics Data System (ADS)

Russo, Matthew; Thompson, Christopher

2015-12-01

We consider the inner ˜1 AU of a protoplanetary disk (PPD) at a stage where angular momentum transport is driven by the mixing of a radial magnetic field into the disk from a T Tauri wind. Because the radial profile of the imposed magnetic field is well constrained, a constrained calculation of the disk mass flow becomes possible. The vertical disk profiles obtained in Paper I imply a stronger magnetization in the inner disk, faster accretion, and a secular depletion of the disk material. Inward transport of solids allows the disk to maintain a broad optical absorption layer even when the grain abundance becomes too small to suppress its ionization. Thus, a PPD may show a strong mid- to near-infrared spectral excess even while its mass profile departs radically from the minimum-mass solar nebula. The disk surface density is buffered at ˜30 g cm-2 below this, X-rays trigger magnetorotational turbulence at the midplane strong enough to loft millimeter- to centimeter-sized particles high in the disk, followed by catastrophic fragmentation. A sharp density gradient bounds the inner depleted disk and propagates outward to ˜1-2 AU over a few megayears. Earth-mass planets migrate through the inner disk over a similar timescale, whereas the migration of Jupiters is limited by the supply of gas. Gas-mediated migration must stall outside 0.04 AU, where silicates are sublimated and the disk shifts to a much lower column. A transition disk emerges when the dust/gas ratio in the MRI-active layer falls below Xd ˜ 10-6 (ad/μm), where ad is the grain size.

Tracing Water Vapor and Ice During Dust Growth

NASA Astrophysics Data System (ADS)

Krijt, Sebastiaan; Ciesla, Fred J.; Bergin, Edwin A.

2016-12-01

The processes that govern the evolution of dust and water (in the form of vapor or ice) in protoplanetary disks are intimately connected. We have developed a model that simulates dust coagulation, dust dynamics (settling, turbulent mixing), vapor diffusion, and condensation/sublimation of volatiles onto grains in a vertical column of a protoplanetary disk. We employ the model to study how dust growth and dynamics influence the vertical distribution of water vapor and water ice in the region just outside the radial snowline. Our main finding is that coagulation (boosted by the enhanced stickiness of icy grains) and the ensuing vertical settling of solids results in water vapor being depleted, but not totally removed, from the region above the snowline on a timescale commensurate with the vertical turbulent mixing timescale. Depending on the strength of the turbulence and the temperature, the depletion can reach factors of up to ˜50 in the disk atmosphere. In our isothermal column, this vapor depletion results in the vertical snowline moving closer to the midplane (by up to 2 gas scale heights) and the gas-phase {{C}}/{{O}} ratio above the vertical snowline increasing. Our findings illustrate the importance of dynamical effects and the need for understanding coevolutionary dynamics of gas and solids in planet-forming environments.

A novel RP-HPLC method for simultaneous determination of potassium sorbate and sodium benzoate in soft drinks using C18-bonded monolithic silica column.

PubMed

Can, Nafiz O; Arli, Goksel; Lafci, Yigit

2011-08-01

Potassium sorbate and sodium benzoate are food additives that are generally employed for prevention of food spoilage originating from bacteria, molds or yeasts. Although these compounds were generally recognized as safe due to their low risk of acute and chronic toxicity, they have limitations of usage to protect human health. Development and validation of a novel RP-HPLC method, in which a C18-bonded monolithic silica column was used as stationary phase to assay these compounds, is described for the first time. Aliquots of 10 μL of samples were injected into chromatograph and eluted using phosphate buffer (0.025 M, pH 2.0)-water-acetonitrile (50:45:5, v/v/v) solution, which was pumped at the rate of 3.0 mL/min. To sharpen the peaks, 10 mM octylamine was added to the mobile phase. Potassium sorbate and sodium benzoate were detected at about 12(th) and 14(th) min, respectively, and quantified at 230 nm using photodiode array detector. A total of 41 samples were prepared by simply filtering through 0.45 μm filters after sonication, and injected into the system without any pre-treatment steps. Applicability of the method was demonstrated by performing total procedure on samples of different brands and types, and their compliance to official regulations was assessed. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Rapid chromatographic determination of caseins in milk with photometric and fluorimetric detection using a hydrophobic monolithic column.

PubMed

Ramírez-Palomino, P; Fernández-Romero, J M; Gómez-Hens, A

2014-01-01

Reverse-phase liquid chromatographic methods using a hydrophobic C18 monolithic column and on-line photometric and fluorimetric detection for the determination of the major casein (CN) proteins in milk are presented. The separation of αs1-CN, αs2-CN, β-CN and κ-CN was achieved in only five minutes. Fluorimetric detection enabled better analytical results than photometric detection. Thus, the dynamic ranges of the calibration graphs and detection limits obtained using fluorimetric detection were (mgmL(-)(1)): αs1-CN (0.74-10.0, 0.22), αs2-CN (0.15-10.0, 0.045), β-CN (0.68-10.0, 0.20) and κ-CN (0.21-10.0, 0.06). The analytical features of the photometric method, which does not allow the quantification of β-casein, were (mgmL(-)(1)): αs1-CN (1.5-9.0, 0.45), αs2-CN (1.4-10.0, 0.43) and κ-CN (0.4-9.0, 0.12). Precision data, expressed as relative standard deviation, ranged between 0.6% and 5.3% for the fluorimetric method and between 2.4% and 6.2% for the photometric method. Both methods were applied to the analysis of three different milk samples, obtaining recoveries in the ranges of 86.6-103.2% and 92.0-106.5% using fluorimetric and photometric detection, respectively. Copyright © 2013 Elsevier Ltd. All rights reserved.

Effect of bioparticle size on dispersion and retention in monolithic and perfusive beds

PubMed Central

Trilisky, Egor I.; Lenhoff, Abraham M.

2010-01-01

Single-component pulse response studies were used to compare the retention and transport behavior of small molecules, proteins, and a virus on commercially available monolithic and perfusive ion-exchangers. Temporal distortion and extra-column effects were corrected for using a simple algorithm based on the method of moments. It was found that temporal distortion is inversely related to the number of theoretical plates. With increasing bioparticle size, retention increased and the transition from a non-eluting to a non-adsorbing state with increasing ionic strength became more abrupt. Both of these observations are qualitatively explained by calculations of particle-surface electrostatic attractive energy. Calculations also show that, for sufficiently large bioparticles, such as viruses or cells, hydrodynamic drag can promote elution. Under non-adsorbing conditions, plate height increased only weakly with flow rate and the skew remained unchanged. With increasing retention, plate height increased dramatically for proteins. Plate height was scaled by permeability rather than bead diameter to enable comparison among different stationary phases. PMID:20951383

Surface figure control for coated optics

DOEpatents

Ray-Chaudhuri, Avijit K.; Spence, Paul A.; Kanouff, Michael P.

2001-01-01

A pedestal optical substrate that simultaneously provides high substrate dynamic stiffness, provides low surface figure sensitivity to mechanical mounting hardware inputs, and constrains surface figure changes caused by optical coatings to be primarily spherical in nature. The pedestal optical substrate includes a disk-like optic or substrate section having a top surface that is coated, a disk-like base section that provides location at which the substrate can be mounted, and a connecting cylindrical section between the base and optics or substrate sections. The optic section has an optical section thickness.sup.2 /optical section diameter ratio of between about 5 to 10 mm, and a thickness variation between front and back surfaces of less than about 10%. The connecting cylindrical section may be attached via three spaced legs or members. However, the pedestal optical substrate can be manufactured from a solid piece of material to form a monolith, thus avoiding joints between the sections, or the disk-like base can be formed separately and connected to the connecting section. By way of example, the pedestal optical substrate may be utilized in the fabrication of optics for an extreme ultraviolet (EUV) lithography imaging system, or in any optical system requiring coated optics and substrates with reduced sensitivity to mechanical mounts.

Ca II and Na I absorption in the QSO S4 0248 + 430 due to an intervening galaxy

NASA Technical Reports Server (NTRS)

Womble, Donna S.; Junkkarinen, Vesa T.; Cohen, Ross D.; Burbidge, E. Margaret

1990-01-01

Observations of the QSO S4 0248 + 430 and a nearby anonymous galaxy are presented. Two absorption components are found in both Ca II H and K and Na I D1 and D2 at z(a) = 0.0515, 0.0523. Column densities of log N(Ca II) = 13.29, 13.50, and log N(Na I) = 13.79, 14.18 are found for z(a) = 0.0515, 0.0523 absorption systems, respectively. The column density ratios imply considerable calcium depletion and disk-type absorbing gas. At least one and possibly both absorption components are produced by high-velocity gas. A broadband image of the field shows an asymmetrical armlike feature or possible tidal tail covering and extending past the position of the QSO. The presence of this extended feature and the apparent difference between the absorption velocities and galaxy rotation velocity suggest that the absorbing gas is not ordinary disk gas, but rather is a result of tidal disruption.

Analysis of protein phosphorylation by monolithic extraction columns based on poly(divinylbenzene) containing embedded titanium dioxide and zirconium dioxide nano-powders.

PubMed

Rainer, Matthias; Sonderegger, Harald; Bakry, Rania; Huck, Christian W; Morandell, Sandra; Huber, Lukas A; Gjerde, Douglas T; Bonn, Günther K

2008-11-01

The potential of an organic monolith with incorporated titanium dioxide (TiO(2)) and zirconium dioxide (ZrO(2)) nanoparticles was evaluated for the selective enrichment of phosphorylated peptides from tryptic digests. A pipette tip was fitted with a monolith based on divinylbenzene (DVB) of highly porous structure, which allows sample to pass through the monolithic bed. The enrichment of phosphopeptides was enhanced by increasing the pipetting cycles during the sample preparation and a higher recovery could be achieved with adequate buffer systems. A complete automated process was developed for enrichment of phosphopeptides leading to high reproducibility and resulting in a robust method designed to minimize analytical variance while providing high sensitivity at high sample throughput. The effect of particle size on the selectivity of phosphopeptides was investigated by comparative studies with nano- and microscale TiO(2) and ZrO(2) powders. Eleven phosphopeptides from alpha-casein digest could be recovered by an optimized mixture of microscale TiO(2)/ZrO(2) particles, whereas nine additional phosphopeptides could be retained by the same mixture of nano-structured material. When compared to conventional immobilized metal-ion affinity chromatography and commercial phosphorylation-enrichment kits, higher selectivity was observed in case of self fabricated tips. About 20 phosphopeptides could be retained from alpha-casein and five from beta-casein digests by using TiO(2) and ZrO(2) based extraction tips. Further selectivity for phosphopeptides was demonstrated by enriching a digest of in vitro phosphorylated extracellular signal regulated kinase 1 (ERK1). Two phosphorylated peptides of ERK1 could be identified by MALDI-MS/MS measurements and a following MASCOT database search.

Intervertebral disk width in dogs with and without clinical signs of disk associated cervical spondylomyelopathy

PubMed Central

2012-01-01

Background Disk-associated cervical spondylomyelopathy (DA-CSM) is a multifactorial neurological disorder in which progressive caudal cervical spinal cord compression is mainly caused by one or more intervertebral disk protrusions. The Doberman pinscher breed seems predisposed for this condition. The underlying cause and pathophysiology of DA-CSM are currently unknown. Recently, wider intervertebral disks have been put forward as a risk factor for development of clinically relevant DA-CSM. However, little is known about other factors affecting intervertebral disk width. Therefore the aim of this study was to assess the association between intervertebral disk width, measured on magnetic resonance imaging (MRI), and clinical status, age, gender and intervertebral disk location in dogs with and without clinical signs of DA-CSM. Methods Doberman pinschers with clinical signs of DA-CSM (N=17),clinically normal Doberman pinschers (N=20), and clinically normal English Foxhounds (N=17), underwent MRI of the cervical vertebral column. On sagittal T2-weighted images, intervertebral disk width was measured from C2-C3 to C6-C7. Intra –and interobserver agreement were assessed on a subset of 20 of the 54 imaging studies. Results Intervertebral disk width was not significantly different between Doberman pinschers with clinical signs of DA-CSM, clinically normal Doberman pinschers or clinically normal English Foxhounds (p=0.43). Intervertebral disk width was positively associated with increasing age (p=0.029). Each monthly increase in age resulted in an increase of disk width by 0.0057mm. Intervertebral disk width was not significantly affected by gender (p=0.056), but was significantly influenced by intervertebral disk location (p <0.0001). The assessed measurements were associated with a good intra –and interobserver agreement. Conclusions The present study does not provide evidence that wider intervertebral disks are associated with clinical status in dogs with and without DA-CSM. Instead, it seems that cervical intervertebral disk width in dogs is positively associated with increase in age. PMID:22839697

Signatures of Hot Molecular Hydrogen Absorption from Protoplanetary Disks. I. Non-thermal Populations

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

Hoadley, Keri; France, Kevin; Arulanantham, Nicole

2017-09-01

The environment around protoplanetary disks (PPDs) regulates processes that drive the chemical and structural evolution of circumstellar material. We perform a detailed empirical survey of warm molecular hydrogen (H{sub 2}) absorption observed against H i-Ly α (Ly α : λ 1215.67) emission profiles for 22 PPDs, using archival Hubble Space Telescope ultraviolet (UV) spectra to identify H{sub 2} absorption signatures and quantify the column densities of H{sub 2} ground states in each sightline. We compare thermal equilibrium models of H{sub 2} to the observed H{sub 2} rovibrational level distributions. We find that, for the majority of targets, there is amore » clear deviation in high-energy states ( T {sub exc} ≳ 20,000 K) away from thermal equilibrium populations ( T (H{sub 2}) ≳ 3500 K). We create a metric to estimate the total column density of non-thermal H{sub 2} ( N (H{sub 2}){sub nLTE}) and find that the total column densities of thermal ( N (H{sub 2})) and N (H{sub 2}){sub nLTE} correlate for transition disks and targets with detectable C iv-pumped H{sub 2} fluorescence. We compare N (H{sub 2}) and N (H{sub 2}){sub nLTE} to circumstellar observables and find that N (H{sub 2}){sub nLTE} correlates with X-ray and far-UV luminosities, but no correlations are observed with the luminosities of discrete emission features (e.g., Ly α , C iv). Additionally, N (H{sub 2}) and N (H{sub 2}){sub nLTE} are too low to account for the H{sub 2} fluorescence observed in PPDs, so we speculate that this H{sub 2} may instead be associated with a diffuse, hot, atomic halo surrounding the planet-forming disk. We create a simple photon-pumping model for each target to test this hypothesis and find that Ly α efficiently pumps H{sub 2} levels with T {sub exc} ≥ 10,000 K out of thermal equilibrium.« less

Long-Term Effects of Dredging Operations Program. Design of an Improved Column Leaching Apparatus for Sediments and Dredged Material

DTIC Science & Technology

1991-07-01

Wastes and Flue Gas Desulfurization Sludgas, Interim Report," EPA-600/2-76-182, Municipal Environ- mental Laboratory, US Environmental Protection Agency...Kinman, R. N. 1979. "Leachate and Gas Production Under Controlled Moisture Condition," "Municipal Solid Waste: Land Disposal" EPA- 600/9-79-029a, M. P...includes upflow mode with distribution disks at both the top and bottom of the column. Pore water velocity is controlled to be less than 1 E-05 cm/sec

Considerations on comprehensive and off-line supercritical fluid chromatography x reversed-phase liquid chromatography for the analysis of triacylglycerols in fish oil.

PubMed

François, Isabelle; Pereira, Alberto dos Santos; Sandra, Pat

2010-06-01

The separation of the triacylglycerols in fish oil was performed by comprehensive and off-line supercritical fluid chromatography combined with RP-LC. The first dimension consisted of two serially coupled silver-ion (SI)-loaded columns operated with a supercritical mobile phase (supercritical fluid chromatography, SFC) in both the cases, whereas the second dimension was performed in non-aqueous RP mode (NARP-LC) on a 10-cm monolithic octadecyl silica (ODS) or a 45-cm long ODS column packed with 1.8 microm particles for the comprehensive and off-line separations, respectively. Despite the outstanding performance of the SI-SFC x NARP-LC interface, the high complexity of the sample rendered the online separation far from complete. The off-line approach gave much better separation mainly because of the higher peak capacity of the second-dimension column, but even in this case, the use of MS was mandatory to elucidate the different triacylglycerols in fish oil. The disadvantage of the off-line procedure was the long analysis time.

Multiclonal plastic antibodies for selective aflatoxin extraction from food samples.

PubMed

Bayram, Engin; Yılmaz, Erkut; Uzun, Lokman; Say, Rıdvan; Denizli, Adil

2017-04-15

Herein, we focused on developing a new generation of monolithic columns for extracting aflatoxin from real food samples by combining the superior features of molecularly imprinted polymers and cryogels. To accomplish this, we designed multiclonal plastic antibodies through simultaneous imprinting of aflatoxin subtypes B1, B2, G1, and G2. We applied Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), and spectrofluorimetry to characterize the materials, and conducted selectivity studies using ochratoxin A and aflatoxin M1 (a metabolite of aflatoxin B1), as well as other aflatoxins, under competitive conditions. We determined optimal aflatoxin extraction conditions in terms of concentration, flow rate, temperature, and embedded particle amount as up to 25ng/mL for each species, 0.43mL/min, 7.0, 30°C, and 200mg, respectively. These multiclonal plastic antibodies showed imprinting efficiencies against ochratoxin A and aflatoxin M1 of 1.84 and 26.39, respectively, even under competitive conditions. Finally, we tested reusability, repeatability, reproducibility, and robustness of columns throughout inter- and intra-column variation studies. Copyright © 2016 Elsevier Ltd. All rights reserved.

Hepatotoxic microcystin removal using pumice embedded monolithic composite cryogel as an alternative water treatment method.

PubMed

Gurbuz, Fatma; Ceylan, Şeyda; Odabaşı, Mehmet; Codd, Geoffrey A

2016-03-01

Microcystins are the most commonly encountered water-borne cyanotoxins which present short- and long-term risks to human health. Guidelines at international and national level, and legislation in some countries, have been introduced for the effective health risk management of these potent hepatotoxic, tumour-promoters. The stable cyclic structure of microcystins and their common production by cyanobacteria in waterbodies at times of high total dissolved organic carbon content presents challenges to drinking water treatment facilities, with conventional, advanced and novel strategies under evaluation. Here, we have studied the removal of microcystins using three different forms of pumice particles (PPs), which are embedded into macroporous cryogel columns. Macroporous composite cryogel columns (MCCs) are a new generation of separation media designed to face this challenging task. Three different MCCs were prepared by adding plain PPs, Cu(2+)-attached PPs and Fe(3+)-attached PPs to reaction media before the cryogelation step. Column studies showed that MCCs could be successfully used as an alternative water treatment method for successful microcystin removal. Copyright © 2016 Elsevier Ltd. All rights reserved.

Inventoring Gas in Debris Disks: UV Spectroscopy of Eta Tel

NASA Astrophysics Data System (ADS)

Roberge, Aki

2015-10-01

Debris disks stand between gas-rich protoplanetary disks and mature planetary systems, shedding light on the late stages of planet formation. Their dust component has been extensively studied, yet has provided little information about disk chemical composition. More information can be provided by their gas content, but astonishingly little is known about it. Only two debris disks have measurements of their gas composition, which is shockingly carbon-rich (Beta Pictoris and 49 Ceti). Basic questions remain unanswered. What are the typical gas-to-dust ratios in debris disks? What is the chemical composition of debris gas and its parent material? The answers to these questions have profound implications for terrestrial planet assembly and the origins of planetary atmospheres.Most detections of debris gas to date were achieved with line of sight UV/optical absorption spectroscopy of edge-on disks, using the central star as the background source. This technique is far more sensitive to small amounts of gas than emission line studies. The UV bandpass is particularly important, since strong transitions of numerous atomic and molecular species lie there. We propose extending our intriguing studies of debris gas with STIS UV spectroscopy of a highly promising debris disk system, Eta Tel. This disk is edge-on and contains circumstellar atomic gas (CII). We will measure column densities of the most important gas species, find the relative elemental gas abundances, and determine the gas mass using a powerful gas disk modeling code. We will also divide our observations into two visits, to search for signs of star-grazing exocomets, which are seen in both Beta Pic and 49 Cet.

A Novel Method for gamma - text{photons} Depth-of-Interaction Detection in Monolithic Scintillation Crystals

NASA Astrophysics Data System (ADS)

Pani, Roberto; Bettiol, Marco; Preziosi, Enrico; Borrazzo, Cristian; Pellegrini, Rosanna; González, Antonio J.; Conde, Pablo; Cinti, Maria Nerina; Fabbri, Andrea; Di Castro, Elisabetta; Majewski, Stan

2016-10-01

Achieved spatial resolution of the PET systems is often limited by the parallax error due to the lack of information about the Depth of Interaction (DoI) inside the crystal of the incoming 511 keV annihilation photons. The smaller the diameter of the PET ring and the thicker the scintillator are, the more this error affects imaging performance. In this work, a DoI calculator suitable for monolithic scintillation crystals and based on the shape of the scintillation light distribution at the photodetector surface has been proposed. To test the estimator performance, a test PET module with a 50 × 50 × 20 mm monolithic LYSO crystal coupled to a 12 × 12 SiPM array has been employed. In addition, for calibration and validation of the method, Geant4 simulations have been also used. The key result of the application of the proposed DoI estimator is obtaining a continuous DoI estimation with an average DoI resolution of about 5 mm in the 20 mm-thick crystal. Benefiting from the DoI estimation capabilities of the method, it has been also possible to achieve additional important goals, first of all reducing the parallax error. First, because the scintillation light collection varies as a function of the 3D position of the interaction of the annihilation photon inside the crystal, a method to correct this response variation via a proper 3D look-up-table is proposed. This has led to an improvement of about 35% in energy resolution. Moreover, a DoI-dependent position algorithm has been proposed, allowing an improvement of both planar (X-Y) position linearity and planar spatial resolution. This algorithm is specifically developed for the rows/columns multi-channel readout logic, that reduces the number of independent channels from N × N to N + N, where N is the number of SiPM photodetection elements (12 in our case) in each row and column. This development was performed in the framework of the MindView PET/MilI brain imaging project.

Erratum: ``The Effects of Metallicity and Grain Size on Gravitational Instabilities in Protoplanetary Disks'' (ApJ 636, L149 [2006])

NASA Astrophysics Data System (ADS)

Cai, Kai; Durisen, Richard H.; Michael, Scott; Boley, Aaron C.; Mejía, Annie C.; Pickett, Megan K.; D'Alessio, Paola

2006-05-01

We have found that the total cumulative radiative energy losses shown in Figure 2 of the above-mentioned Letter were computed for only half the disk. This caused the final global cooling times tcool in the eighth column of the original Table 1 to be too large by a factor of 2. Proper values of tcool are given in the revised Table 1 below. To be more consistent with what the Letter states, we now use instantaneous values for both the total internal energy and the final total net cooling rates to compute final tcool's, instead of averaging the loss rates over an interval of time at the end of the calculations before dividing, as was done in the Letter. We also take this opportunity to make a few other inconsequential corrections to the fourth column of the table. In addition to the changes to Table 1, the approximate initial tcool relation in the fourth paragraph of § 3.2 becomes tcool~Z/Zsolar to within tens of percent. Despite the corrections, our conclusions in the Letter remain unchanged. Most importantly, the final tcool's vary with metallicity and are still too long for disk fragmentation to occur with our equation of state over the range of Z examined. We regret any inconvenience our errors may have caused.

Two Key Parameters Controlling Particle Clumping Caused by Streaming Instability in the Dead-zone Dust Layer of a Protoplanetary Disk

NASA Astrophysics Data System (ADS)

Sekiya, Minoru; Onishi, Isamu K.

2018-06-01

The streaming instability and Kelvin–Helmholtz instability are considered the two major sources causing clumping of dust particles and turbulence in the dust layer of a protoplanetary disk as long as we consider the dead zone where the magnetorotational instability does not grow. Extensive numerical simulations have been carried out in order to elucidate the condition for the development of particle clumping caused by the streaming instability. In this paper, a set of two parameters suitable for classifying the numerical results is proposed. One is the Stokes number that has been employed in previous works and the other is the dust particle column density that is nondimensionalized using the gas density in the midplane, Keplerian angular velocity, and difference between the Keplerian and gaseous orbital velocities. The magnitude of dust clumping is a measure of the behavior of the dust layer. Using three-dimensional numerical simulations of dust particles and gas based on Athena code v. 4.2, it is confirmed that the magnitude of dust clumping for two disk models are similar if the corresponding sets of values of the two parameters are identical to each other, even if the values of the metallicity (i.e., the ratio of the columns density of the dust particles to that of the gas) are different.

A rapid and sensitive method for the quantitation of montelukast in sheep plasma using liquid chromatography/tandem mass spectrometry.

PubMed

Papp, Robert; Luk, Pauline; Mullett, Wayne M; Kwong, Elizabeth

2007-10-15

A rapid LC-MS/MS method was developed and partially validated for the quantitation of montelukast in spiked sheep plasma. A total run time of 1.5 min was achieved using a short monolithic column and employing a rapid gradient. Sample preparation involved protein precipitation with twofold acetonitrile by volume during which a deuterated internal standard (montelukast D-6) was incorporated. The MRM transitions for montelukast and the deuterated internal standard were 586/422 and 592/427, respectively. A linear dynamic range of 0.25-500 ng/mL with a correlation coefficient of 0.9999 was achieved. Precision was below 5% at all levels except at the LOQ (0.36 ng/mL) which demonstrated an overall of R.S.D. of 8%. Post-column infusion experiments were performed with precipitated plasma matrix and showed minimal interference with the peaks of interest.

A Numerical Model of Exchange Chromatography Through 3D Lattice Structures

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

Salloum, Maher; Robinson, David B.

Rapid progress in the development of additive manufacturing technologies is opening new opportunities to fabricate structures that control mass transport in three dimensions across a broad range of length scales. We describe a structure that can be fabricated by newly available commercial 3D printers. It contains an array of regular three-dimensional flow paths that are in intimate contact with a solid phase, and thoroughly shuffle material among the paths. We implement a chemically reacting flow model to study its behavior as an exchange chromatography column, and compare it to an array of one-dimensional flow paths that resemble more traditional honeycombmore » monoliths. A reaction front moves through the columns and then elutes. Here, the front is sharper at all flow rates for the structure with three-dimensional flow paths, and this structure is more robust to channel width defects than the one-dimensional array.« less

Active pixel sensor pixel having a photodetector whose output is coupled to an output transistor gate

NASA Technical Reports Server (NTRS)

Fossum, Eric R. (Inventor); Nakamura, Junichi (Inventor); Kemeny, Sabrina E. (Inventor)

2005-01-01

An imaging device formed as a monolithic complementary metal oxide semiconductor integrated circuit in an industry standard complementary metal oxide semiconductor process, the integrated circuit including a focal plane array of pixel cells, each one of the cells including a photogate overlying the substrate for accumulating photo-generated charge in an underlying portion of the substrate and a charge coupled device section formed on the substrate adjacent the photogate having a sensing node and at least one charge coupled device stage for transferring charge from the underlying portion of the substrate to the sensing node. There is also a readout circuit, part of which can be disposed at the bottom of each column of cells and be common to all the cells in the column. A Simple Floating Gate (SFG) pixel structure could also be employed in the imager to provide a non-destructive readout and smaller pixel sizes.

A Numerical Model of Exchange Chromatography Through 3D Lattice Structures

DOE PAGES

Salloum, Maher; Robinson, David B.

2018-01-30

Rapid progress in the development of additive manufacturing technologies is opening new opportunities to fabricate structures that control mass transport in three dimensions across a broad range of length scales. We describe a structure that can be fabricated by newly available commercial 3D printers. It contains an array of regular three-dimensional flow paths that are in intimate contact with a solid phase, and thoroughly shuffle material among the paths. We implement a chemically reacting flow model to study its behavior as an exchange chromatography column, and compare it to an array of one-dimensional flow paths that resemble more traditional honeycombmore » monoliths. A reaction front moves through the columns and then elutes. Here, the front is sharper at all flow rates for the structure with three-dimensional flow paths, and this structure is more robust to channel width defects than the one-dimensional array.« less

Direct-injection screening for acidic drugs in plasma and neutral drugs in equine urine by differential-gradient LC-LC coupled MS/MS.

PubMed

Stanley, Shawn M R; Wee, Wei Khee; Lim, Boon Huat; Foo, Hsiao Ching

2007-04-01

Direct-injection LC-LC hybrid tandem MS methods have been developed for undertaking broad-based screening for acidic drugs in protein-precipitated plasma and neutral doping agents in equine urine. In both analyses, analytes present in the matrix were trapped using a HLB extraction column before being refocused and separated on a Chromolith RP-18e monolithic analytical column using a controlled differential gradient generated by proportional dilution of the first column's eluent with water. Each method has been optimised by the adoption of a mobile phase and gradient that was tailored to enhance ionisation in the MS source while maintaining good chromatographic behaviour for the majority of the target drugs. The analytical column eluent was fed into the heated nebulizer (HN) part of the Duospray interface attached to a 4000 QTRAP mass spectrometer. Information dependent acquisition (IDA) with dynamic background subtraction (DBS) was configured to trigger a sensitive enhanced product ion (EPI) scan when a multiple reaction monitoring (MRM) survey scan signal exceeded the defined criteria. Ninety-one percent of acidic drugs in protein-precipitated plasma and 80% of the neutral compounds in equine urine were detected when spiked at 10 ng/ml.

Preliminary evaluation of monolithic column high-performance liquid chromatography with tris(2,2'-bipyridyl)ruthenium(II) chemiluminescence detection for the determination of quetiapine in human body fluids.

PubMed

Bellomarino, Sara A; Brown, Allyson J; Conlan, Xavier A; Barnett, Neil W

2009-03-15

High-performance liquid chromatography (HPLC) with tris(2,2'-bipyridyl)ruthenium(II) chemiluminescence detection methodology is reported for the determination of the atypical antipsychotic drug quetiapine and the observation of its major active and inactive metabolites in human urine and serum. The method uses a monolithic chromatographic column allowing high flow rates of 3 mLmin(-1) enabling rapid quantification. Flow injection analysis (FIA) with tris(2,2'-bipyridyl)ruthenium(II) chemiluminescence detection and HPLC time of flight mass spectrometry (TOF-MS) were used for the determination of quetiapine in a pharmaceutical preparation to establish its suitability as a calibration standard. The limit of detection achieved with FIA was 2 x 10(-11) molL(-1) in simple aqueous solution. The limits of detection achieved with HPLC were 7 x 10(-8) and 2 x 10(-10) molL(-1) in urine and serum, respectively. The calibration range for FIA was between 5 x 10(-9) and 1 x 10(-6) molL(-1). The calibration ranges for HPLC were between 1 x 10(-7)-1 x 10(-4) and 1 x 10(-8)-1 x 10(-4) molL(-1) in urine and serum, respectively. The quetiapine concentrations in patient samples were found to be 3 x 10(-6) molL(-1) in urine and 7 x 10(-7) molL(-1) in serum. Without the need for preconcentration, the HPLC detection limits compared favourably with those in previously published methodologies. The metabolites were identified using HPLC-TOF-MS.

Concept designs of nonrotating-type centrifugal blood pump and basic study on output characteristics of the oscillating disk-type centrifugal pump.

PubMed

Kabei, N; Tuichiya, K; Sakurai, Y

1994-09-01

When designing a turbo-type blood pump as an artificial heart, the gap between a rotating shaft and a pump housing should be perfectly sealed to prevent any leakage or contamination through a seal. In addition, blood coagulation in a blood chamber must be avoided. To overcome these problems, we proposed five different nonrotating-type turbo pumps: a caudal-fin-type axial-flow pump, a caudal-fin-type centrifugal pump, a nutating-column-type centrifugal pump, a nutating-collapsible-tube-type centrifugal pump, and an oscillating-disk-type centrifugal pump. We selected and developed the oscillating-disk-type centrifugal pump that consists of a disk, a driving rod, a seal, an oscillation mechanism, and a pump housing. The disk is mounted on the end of the rod, which is connected to a high-speed DC motor through an oscillation mechanism. The rod and the disk do not rotate, but they oscillate in the pump housing. This movement of the disk generates forward fluid flow around the axis (i.e., the rotational fluid flow). Centrifugal force due to fluid rotation supports the pressure difference between the outlet and the inlet. The diameter of the disk is 39 mm, the maximum inner diameter of the pump housing is 40 mm, and the volume of the blood chamber for 25 degrees' oscillation is 16.9 ml. The performance of the pump was tested in a mock circulatory system.(ABSTRACT TRUNCATED AT 250 WORDS)

X-ray Reflected Spectra from Accretion Disk Models. I. Constant Density Atmospheres

NASA Technical Reports Server (NTRS)

Garcia, Javier; Kallman, Timothy R.

2009-01-01

We present new models for illuminated accretion disks, their structure and reprocessed emission. We consider the effects of incident X-rays on the surface of an accretion disk by solving simultaneously the equations of radiative transfer, energy balance and ionization equilibrium over a large range of column densities. We assume plane-parallel geometry and azimuthal symmetry, such that each calculation corresponds to a ring at a given distance from the central object. Our models include recent and complete atomic data for K-shell of the iron and oxygen isonuclear sequences. We examine the effect on the spectrum of fluorescent Ka line emission and absorption in the emitted spectrum. We also explore the dependence of the spectrum on the strength of the incident X-rays and other input parameters, and discuss the importance of Comptonization on the emitted spectrum.

DOUBLE DCO{sup +} RINGS REVEAL CO ICE DESORPTION IN THE OUTER DISK AROUND IM LUP

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

Öberg, Karin I.; Loomis, Ryan; Andrews, Sean M.

2015-09-10

In a protoplanetary disk, a combination of thermal and non-thermal desorption processes regulate where volatiles are liberated from icy grain mantles into the gas phase. Non-thermal desorption should result in volatile-enriched gas in disk-regions where complete freeze-out is otherwise expected. We present Atacama Large Millimeter/Submillimeter Array observations of the disk around the young star IM Lup in 1.4 mm continuum, C{sup 18}O 2–1, H{sup 13}CO{sup +} 3–2 and DCO{sup +} 3–2 emission at ∼0.″5 resolution. The images of these dust and gas tracers are clearly resolved. The DCO{sup +} line exhibits a striking pair of concentric rings of emission thatmore » peak at radii of ∼0.″6 and 2″ (∼90 and 300 AU, respectively). Based on disk chemistry model comparison, the inner DCO{sup +} ring is associated with the balance of CO freeze-out and thermal desorption due to a radial decrease in disk temperature. The outer DCO{sup +} ring is explained by non-thermal desorption of CO ice in the low-column-density outer disk, repopulating the disk midplane with cold CO gas. The CO gas then reacts with abundant H{sub 2}D{sup +} to form the observed DCO{sup +} outer ring. These observations demonstrate that spatially resolved DCO{sup +} emission can be used to trace otherwise hidden cold gas reservoirs in the outmost disk regions, opening a new window onto their chemistry and kinematics.« less

Multi-epoch monitoring of the AA Tauri-like star V 354 Mon. Indications for a low gas-to-dust ratio in the inner disk warp

NASA Astrophysics Data System (ADS)

Schneider, P. C.; Manara, C. F.; Facchini, S.; Günther, H. M.; Herczeg, G. J.; Fedele, D.; Teixeira, P. S.

2018-06-01

Disk warps around classical T Tauri stars (CTTSs) can periodically obscure the central star for some viewing geometries. For these so- called AA Tau-like variables, the obscuring material is located in the inner disk and absorption spectroscopy allows one to characterize its dust and gas content. Since the observed emission from CTTSs consists of several components (photospheric, accretion, jet, and disk emission), which can all vary with time, it is generally challenging to disentangling disk features from emission variability. Multi- epoch, flux-calibrated, broadband spectra provide us with the necessary information to cleanly separate absorption from emission variability. We applied this method to three epochs of VLT/X-shooter spectra of the CTTS V 354 Mon (CSI Mon-660) located in NGC 2264 and find that: (a) the accretion emission remains virtually unchanged between the three epochs; (b) the broadband flux evolution is best described by disk material obscuring part of the star, and (c) the Na and K gas absorption lines show only a minor increase in equivalent width during phases of high dust extinction. The limits on the absorbing gas column densities indicate a low gas-to-dust ratio in the inner disk, less than a tenth of the ISM value. We speculate that the evolutionary state of V 354 Mon, rather old with a low accretion rate, is responsible for the dust excess through an evolution toward a dust dominated disk or through the fragmentation of larger bodies that drifted inward from larger radii in a still gas dominated disk.

Multiple Paths of Deuterium Fractionation in Protoplanetary Disks

NASA Astrophysics Data System (ADS)

Aikawa, Yuri; Furuya, Kenji; Hincelin, Ugo; Herbst, Eric

2018-03-01

We investigate deuterium chemistry coupled with the nuclear spin-state chemistry of H2 and {{{H}}}3+ in protoplanetary disks. Multiple paths of deuterium fractionation are found; exchange reactions with D atoms, such as HCO+ + D, are effective in addition to those with HD. In a disk model with grain sizes appropriate for dark clouds, the freeze-out of molecules is severe in the outer midplane, while the disk surface is shielded from UV radiation. Gaseous molecules, including DCO+, thus become abundant at the disk surface, which tends to make their column density distribution relatively flat. If the dust grains have grown to millimeter size, the freeze-out rate of neutral species is reduced and the abundances of gaseous molecules, including DCO+ and N2D+, are enhanced in the cold midplane. Turbulent diffusion transports D atoms and radicals at the disk surface to the midplane, and stable ice species in the midplane to the disk surface. The effects of turbulence on chemistry are thus multifold; while DCO+ and N2D+ abundances increase or decrease depending on the regions, HCN and DCN in the gas and ice are greatly reduced at the innermost radii, compared to the model without turbulence. When cosmic rays penetrate the disk, the ortho-to-para ratio (OPR) of H2 is found to be thermal in the disk, except in the cold (≲10 K) midplane. We also analyze the OPR of {{{H}}}3+ and H2D+, as well as the main reactions of H2D+, DCO+, and N2D+, in order to analytically derive their abundances in the cold midplane.

High-Precision Displacement Sensing of Monolithic Piezoelectric Disk Resonators Using a Single-Electron Transistor

NASA Astrophysics Data System (ADS)

Li, J.; Santos, J. T.; Sillanpää, M. A.

2018-02-01

A single-electron transistor (SET) can be used as an extremely sensitive charge detector. Mechanical displacements can be converted into charge, and hence, SETs can become sensitive detectors of mechanical oscillations. For studying small-energy oscillations, an important approach to realize the mechanical resonators is to use piezoelectric materials. Besides coupling to traditional electric circuitry, the strain-generated piezoelectric charge allows for measuring ultrasmall oscillations via SET detection. Here, we explore the usage of SETs to detect the shear-mode oscillations of a 6-mm-diameter quartz disk resonator with a resonance frequency around 9 MHz. We measure the mechanical oscillations using either a conventional DC SET, or use the SET as a homodyne or heterodyne mixer, or finally, as a radio-frequency single-electron transistor (RF-SET). The RF-SET readout is shown to be the most sensitive method, allowing us to measure mechanical displacement amplitudes below 10^{-13} m. We conclude that a detection based on a SET offers a potential to reach the sensitivity at the quantum limit of the mechanical vibrations.

High-Precision Displacement Sensing of Monolithic Piezoelectric Disk Resonators Using a Single-Electron Transistor

NASA Astrophysics Data System (ADS)

Li, J.; Santos, J. T.; Sillanpää, M. A.

2018-06-01

A single-electron transistor (SET) can be used as an extremely sensitive charge detector. Mechanical displacements can be converted into charge, and hence, SETs can become sensitive detectors of mechanical oscillations. For studying small-energy oscillations, an important approach to realize the mechanical resonators is to use piezoelectric materials. Besides coupling to traditional electric circuitry, the strain-generated piezoelectric charge allows for measuring ultrasmall oscillations via SET detection. Here, we explore the usage of SETs to detect the shear-mode oscillations of a 6-mm-diameter quartz disk resonator with a resonance frequency around 9 MHz. We measure the mechanical oscillations using either a conventional DC SET, or use the SET as a homodyne or heterodyne mixer, or finally, as a radio-frequency single-electron transistor (RF-SET). The RF-SET readout is shown to be the most sensitive method, allowing us to measure mechanical displacement amplitudes below 10^{-13} m. We conclude that a detection based on a SET offers a potential to reach the sensitivity at the quantum limit of the mechanical vibrations.

Supermacroporous cryogel matrix for integrated protein isolation. Immobilized metal affinity chromatographic purification of urokinase from cell culture broth of a human kidney cell line.

PubMed

Kumar, Ashok; Bansal, Vibha; Andersson, Jonatan; Roychoudhury, Pradip K; Mattiasson, Bo

2006-01-20

A new type of supermacroporous, monolithic, cryogel affinity adsorbent was developed, allowing the specific capture of urokinase from conditioned media of human fibrosarcoma cell line HT1080. The affinity adsorbent was designed with the objective of using it as a capture column in an integrated perfusion/protein separation bioreactor setup. A comparative study between the utility of this novel cryogel based matrix and the conventional Sepharose based affinity matrix for the continuous capture of urokinase in an integrated bioreactor system was performed. Cu(II)-ion was coupled to epoxy activated polyacrylamide cryogel and Sepharose using iminodiacetic acid (IDA) as the chelating ligand. About 27-fold purification of urokinase from the conditioned culture media was achieved with Cu(II)-IDA-polyacrylamide cryogel column giving specific activity of about 814 Plough units (PU)/mg protein and enzyme yields of about 80%. High yields (95%) were obtained with Cu(II)-IDA-Sepharose column by virtue of its high binding capacity. However, the adsorbent showed lower selectivity as compared to cryogel matrix giving specific activity of 161 PU/mg protein and purification factor of 5.3. The high porosity, selectivity and reasonably good binding capacity of Cu(II)-IDA-polyacrylamide cryogel column make it a promising option for use as a protein capture column in integrated perfusion/separation processes. The urokinase peak pool from Cu(II)-IDA-polyacrylamide cryogel column could be further resolved into separate fractions for high and low molecular weight forms of urokinase by gel filtration chromatography on Sephacryl S-200. The selectivity of the cryogel based IMAC matrix for urokinase was found to be higher as compared to that of Cu(II)-IDA-Sepharose column.

SPAX - PAX with Super-Pages

NASA Astrophysics Data System (ADS)

Bößwetter, Daniel

Much has been written about the pros and cons of column-orientation as a means to speed up read-mostly analytic workloads in relational databases. In this paper we try to dissect the primitive mechanisms of a database that help express the coherence of tuples and present a novel way of organizing relational data in order to exploit the advantages of both, the row-oriented and the column-oriented world. As we go, we break with yet another bad habit of databases, namely the equal granularity of reads and writes which leads us to the introduction of consecutive clusters of disk pages called super-pages.

Multiperiod-grating surface-emitting lasers

NASA Technical Reports Server (NTRS)

Lang, Robert J. (Inventor)

1992-01-01

Surface-emitting distributed feedback (DFB) lasers are disclosed with hybrid gratings. A first-order grating is provided at one or both ends of the active region of the laser for retroreflection of light back into the active region, and a second-order or nonresonant grating is provided at the opposite end for coupling light out perpendicular to the surfaces of the laser or in some other selected direction. The gratings may be curved to focus light retroreflected into the active region and to focus light coupled out to a point. When so focused to a point, the DFB laser may be part of a monolithic read head for a laser recorded disk, or an optical coupler into an optical fiber.

Coping with Low Back Pain.

ERIC Educational Resources Information Center

Kindig, L. E.; Mrvos, S. R.

Guidelines are offered for the prevention and relief of lower back pain. The structure of the spine is described, and the functions and composition of spinal disks are explained. A list is included of common causes of abnormalities of the spinal column, and injuries which may cause the fracture of the vertebrae are described. Factors causing low…

Surface modification of SU8 photoresist for shrinkage improvement in a monolithic MEMS microstructure

NASA Astrophysics Data System (ADS)

Chung, C. K.; Hong, Y. Z.

2007-02-01

The effect of O2 plasma treatment on the surface property of exposed and unexposed SU8 photoresist has been investigated for the fabrication of a monolithic MEMS microstructure. It can solve the non-uniformity problem of second resist coating on the SU8 with high intrinsic shrinkage after exposure and post-exposure baking (PEB) in the fabrication of the stacked polymer-metal or polymer-polymer structure, which was used in the application of microfluid, bio and chemistry. The thickness difference of untreated SU8 before PEB between the exposed and unexposed SU8 was about 0.3% while that after PEB increased to about 6%. It could result in large non-uniformity of about 18 µm thickness difference for the following second resist coating on the hydrophobic surface without plasma treatment. The surface property of SU8 in terms of the contact angle and surface energy can be adjusted by O2 plasma treatment for enhancing the coating uniformity of the following resist. The measured contact angles of the exposed and unexposed SU8 decrease with O2 plasma time, corresponding to the increased surface energy determined by the Lifshitz-van der Waals/Lewis acid-base approach. It displayed that the similar hydrophilic surface property can minimize the thickness difference of second resist coating on the first shrunken SU8. A monolithic nozzle plate with a physical resolution of 600 dpi in a single column was demonstrated for an inkjet application based on the improved uniformity.

Open tubular lab-on-column/mass spectrometry for targeted proteomics of nanogram sample amounts.

PubMed

Hustoft, Hanne Kolsrud; Vehus, Tore; Brandtzaeg, Ole Kristian; Krauss, Stefan; Greibrokk, Tyge; Wilson, Steven Ray; Lundanes, Elsa

2014-01-01

A novel open tubular nanoproteomic platform featuring accelerated on-line protein digestion and high-resolution nano liquid chromatography mass spectrometry (LC-MS) has been developed. The platform features very narrow open tubular columns, and is hence particularly suited for limited sample amounts. For enzymatic digestion of proteins, samples are passed through a 20 µm inner diameter (ID) trypsin + endoproteinase Lys-C immobilized open tubular enzyme reactor (OTER). Resulting peptides are subsequently trapped on a monolithic pre-column and transferred on-line to a 10 µm ID porous layer open tubular (PLOT) liquid chromatography LC separation column. Wnt/ß-catenein signaling pathway (Wnt-pathway) proteins of potentially diagnostic value were digested+detected in targeted-MS/MS mode in small cell samples and tumor tissues within 120 minutes. For example, a potential biomarker Axin1 was identifiable in just 10 ng of sample (protein extract of ∼1,000 HCT15 colon cancer cells). In comprehensive mode, the current OTER-PLOT set-up could be used to identify approximately 1500 proteins in HCT15 cells using a relatively short digestion+detection cycle (240 minutes), outperforming previously reported on-line digestion/separation systems. The platform is fully automated utilizing common commercial instrumentation and parts, while the reactor and columns are simple to produce and have low carry-over. These initial results point to automated solutions for fast and very sensitive MS based proteomics, especially for samples of limited size.

Missing matter in the vicinity of the sun

NASA Technical Reports Server (NTRS)

Bahcall, John N.

1986-01-01

The Poisson and Vlasov equations are solved numerically for realistic Galaxy models which include multiple disk components, a Population II spheroid, and an unseen massive halo. The total amount of matter in the vicinity of the sun is determined by comparing the observed distributions of tracer stars, samples of F dwarfs, and K giants with the predictions of the Galaxy models. Results are obtained for a number of different assumed distributions of the unseen disk mass. For all the observed samples, typical models imply that about half of the mass in the solar vicinity must be in the form of unobserved matter. The volume density of unobserved material near the sun is about 0.1 solar mass/cu pc; the corresponding column density is about 30 solar mass/sq pc. This so far unseen material must be in a disk with an exponential scale height of less than 0.7 kpc.

Features of the accretion in the EX Hydrae system: Results of numerical simulation

NASA Astrophysics Data System (ADS)

Isakova, P. B.; Zhilkin, A. G.; Bisikalo, D. V.; Semena, A. N.; Revnivtsev, M. G.

2017-07-01

A two-dimensional numerical model in the axisymmetric approximation that describes the flow structure in the magnetosphere of the white dwarf in the EX Hya system has been developed. Results of simulations show that the accretion in EX Hya proceeds via accretion columns, which are not closed and have curtain-like shapes. The thickness of the accretion curtains depends only weakly on the thickness of the accretion disk. This thickness developed in the simulations does not agree with observations. It is concluded that the main reason for the formation of thick accretion curtains in the model is the assumption that the magnetic field penetrates fully into the plasma of the disk. An analysis based on simple estimates shows that a diamagnetic disk that fully or partially shields the magnetic field of the star may be a more attractive explanation for the observed features of the accretion in EX Hya.

X-ray Luminosity and Absorption Column Fluctuations in the H2O Maser Galaxy NGC 4258 from Weeks to Years

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

Argon, A.

2004-07-30

The authors report monitoring of the 0.3-10 keV spectrum of NGC 4258 with the XMM-Newton observatory at five epochs over 1.5 years. They also report reprocessing of an overlapping four epoch series of archival Chandra observations (0.5-10 keV). By including earlier ASCA and Beppo-SAX observations, they present a new, nine year time-series of models fit to the X-ray spectrum of NGC 4258. They model the Chandra and XMM-Newton data self-consistently with partially absorbed, hard power-law, soft thermal plasma, and soft power-law components. Over the nine years, the photo-electric absorbing column ({approx} 10{sup 23} cm{sup -2}) did not vary detectably, exceptmore » for a {approx} 40% drop between two ASCA epochs separated by 3 years (in 1993 and 1996) and a {approx} 60% rise between two XMM-Newton epochs separated by just 5 months (in 2001 and 2002). In contrast, factor of 2-3 changes are seen in absorbed flux on the timescale of years. These are uncorrelated with changes in absorbing column and indicative of central engine variability. The most rapid change in luminosity (5-10 keV) that the authors detect (with XMM-Newton and Chandra) is on the order of 30% over 19 days. The warped disk that is a known source of H{sub 2}O maser emission in NGC 4258 is believed to cross the line of sight to the central engine. They propose that the variations in absorbing column arise from inhomogeneities in the rotating disk, as they sweep across the line of sight. They estimate that the inhomogeneities are {approx} 10{sup 15} cm in size.« less

Characterizing the thermal distributions of warm molecular hydrogen in protoplanetary disks

NASA Astrophysics Data System (ADS)

Hoadley, Keri; France, Kevin

2016-01-01

Probing the surviving molecular gas within the inner regions of protoplanetary disks (PPDs) around T Tauri stars (1 - 10 Myr) provides insight into the conditions in which planet formation and migration occurs while the gas disk is still present. Recent studies done by Hoadley et al. 2015 and Banzatti & Pontipoddan 2015 suggest that gas in the inner disks of PPDs appear to "respond" to the loss of small dust grains with evolving PPD stage, and IR-CO emission may either be thermally or photo-excited by stellar UV radiation, depending on PPD evolutionary stage. Because far-UV H2 emission lines are dominantly photo-excited by stellar HI-Lyman alpha photons, we observe H2 absorption features against the stellar Lyman alpha wings in a large sample of PPDs at various evolutionary stages. We aim to characterize whether the inner disk H2 environment is in thermal equilibrium at various stages of PPD evolution. We use a sophisticated first-principles approach to fitting multiple absorption features along the red- and blue-wings of the observed stellar Lyman alpha profiles to extract column density estimates of H2 along the line of sight to the target. We find that the high kinetic energy H2 observed in absorption against the LyA wing may be described as a part of the thermal distribution with high kinetic temperature - a potential indication of an inner disk molecular hazy "envelope" around the cooler bulk disk. Ongoing research may help determine the state of the gas and whether it evolves with disk evolutionary stage.

The Gas-rich Circumbinary Disk of HR 4049. II. A Detailed Study of the Near-infrared Spectrum

NASA Astrophysics Data System (ADS)

Malek, S. E.; Cami, J.

2014-10-01

HR 4049 is a peculiar evolved binary surrounded by a circumbinary disk. Mid-infrared observations show that the disk is rich in molecular gas and radially extended. To study the properties of this disk, we re-analyzed a set of near-infrared observations at high spectral resolution obtained with Gemini-Phoenix. These data cover absorption lines originating from the first overtone of CO and from H2O in the 2.3 μm region as well as more complex emission-absorption profiles from H2O and the fundamental mode of CO near 4.6 μm. By using an excitation diagram and from modeling the spectrum, we find that most of the CO overtone and H2O absorption originates from hot gas (T ex ≈ 1000 K) with high column densities, consistent with the mid-infrared data. The strong emission in the wavelength range of the CO fundamental furthermore suggests that there is a significant quantity of gas in the inner cavity of the disk. In addition, there is a much colder component in the line of sight to the disk. A detailed analysis of the overtone line profiles reveals variations in the line widths that are consistent with a radially extended disk in Keplerian rotation with hotter gas closer to the central star. We estimate the mass of the primary to be ~0.34 M ⊙ and discuss the implications for its evolutionary status.

MAVEN/IUVS Apoapse Observations of the Martian FUV Dayglow

NASA Astrophysics Data System (ADS)

Correira, J.; Evans, J. S.; Stevens, M. H.; Schneider, N. M.; Stewart, I. F.; Deighan, J.; Jain, S.; Chaffin, M.; Crismani, M. M. J.; McClintock, B.; Holsclaw, G.; Lefèvre, F.; Lo, D.; Stiepen, A.; Clarke, J. T.; Mahaffy, P. R.; Bougher, S. W.; Bell, J. M.; Jakosky, B. M.

2015-12-01

We present FUV data (115 - 190 nm) from MAVEN/IUVS apoapse mode observations for the Oct 2014 through Feb 2015 time period. During apoapse mode the highly elliptical orbit of MAVEN allows for up to four apoapse disk images by IUVS per day. Maps of FUV feature intensities and intensity ratios as well as derived CO/CO2 and O/CO2 column density ratios will be shown. Column density ratios are derived from lookup tables created using the Atmospheric Ultraviolet Radiance Integrated Code [Strickland et al., 1999] in conjunction with observed intensity ratios. Column density ratios provide a measure of composition changes in the Martian atmosphere. Due to MAVEN's orbital geometry the observations from this time period focus on the southern hemisphere. The broad view provided by apoapse observations allows for the investigation of spatial and temporal variations (both long term and local time) of the atmospheric composition (via the column density ratios). IUVS FUV intensities and derived column density ratios will also be compared with model results from Mars Global Ionosphere/Thermosphere Model (MGITM) and the Mars Climate Database (MCD).

The Star Schema Benchmark and Augmented Fact Table Indexing

NASA Astrophysics Data System (ADS)

O'Neil, Patrick; O'Neil, Elizabeth; Chen, Xuedong; Revilak, Stephen

We provide a benchmark measuring star schema queries retrieving data from a fact table with Where clause column restrictions on dimension tables. Clustering is crucial to performance with modern disk technology, since retrievals with filter factors down to 0.0005 are now performed most efficiently by sequential table search rather than by indexed access. DB2’s Multi-Dimensional Clustering (MDC) provides methods to "dice" the fact table along a number of orthogonal "dimensions", but only when these dimensions are columns in the fact table. The diced cells cluster fact rows on several of these "dimensions" at once so queries restricting several such columns can access crucially localized data, with much faster query response. Unfortunately, columns of dimension tables of a star schema are not usually represented in the fact table. In this paper, we show a simple way to adjoin physical copies of dimension columns to the fact table, dicing data to effectively cluster query retrieval, and explain how such dicing can be achieved on database products other than DB2. We provide benchmark measurements to show successful use of this methodology on three commercial database products.

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

Higuchi, Aya E.; Sakai, Nami; Sato, Aki

We have detected [C i] {sup 3} P {sub 1}–{sup 3} P {sub 0} emissions in the gaseous debris disks of 49 Ceti and β Pictoris with the 10 m telescope of the Atacama Submillimeter Telescope Experiment, which is the first detection of such emissions. The line profiles of [C i] are found to resemble those of CO( J = 3–2) observed with the same telescope and the Atacama Large Millimeter/submillimeter Array. This result suggests that atomic carbon (C) coexists with CO in the debris disks and is likely formed by the photodissociation of CO. Assuming an optically thin [Cmore » i] emission with the excitation temperature ranging from 30 to 100 K, the column density of C is evaluated to be (2.2 ± 0.2) × 10{sup 17} and (2.5 ± 0.7) × 10{sup 16} cm{sup −2} for 49 Ceti and β Pictoris, respectively. The C/CO column density ratio is thus derived to be 54 ± 19 and 69 ± 42 for 49 Ceti and β Pictoris, respectively. These ratios are higher than those of molecular clouds and diffuse clouds by an order of magnitude. The unusually high ratios of C to CO are likely attributed to a lack of H{sub 2} molecules needed to reproduce CO molecules efficiently from C. This result implies a small number of H{sub 2} molecules in the gas disk, i.e., there is an appreciable contribution of secondary gas from dust grains.« less

Droop-Free, Reliable, and High-Power InGaN/GaN Nanowire Light-Emitting Diodes for Monolithic Metal-Optoelectronics.

PubMed

Zhao, Chao; Ng, Tien Khee; ElAfandy, Rami T; Prabaswara, Aditya; Consiglio, Giuseppe Bernardo; Ajia, Idris A; Roqan, Iman S; Janjua, Bilal; Shen, Chao; Eid, Jessica; Alyamani, Ahmed Y; El-Desouki, Munir M; Ooi, Boon S

2016-07-13

A droop-free nitride light-emitting diode (LED) with the capacity to operate beyond the "green gap" has been a subject of intense scientific and engineering interest. While several properties of nanowires on silicon make them promising for use in LED development, the high aspect ratio of individual nanowires and their laterally discontinuous features limit phonon transport and device performance. Here, we report on the monolithic integration of metal heat-sink and droop-free InGaN/GaN quantum-disks-in-nanowire LEDs emitting at ∼710 nm. The reliable operation of our uncooled nanowire-LEDs (NW-LEDs) epitaxially grown on molybdenum was evident in the constant-current soft burn-in performed on a 380 μm × 380 μm LED. The square LED sustained 600 mA electrical stress over an 8 h period, providing stable light output at maturity without catastrophic failure. The absence of carrier and phonon transport barriers in NW-LEDs was further inferred from current-dependent Raman measurements (up to 700 mA), which revealed the low self-heating. The radiative recombination rates of NW-LEDs between room temperature and 40 °C was not limited by Shockley-Read-Hall recombination, Auger recombination, or carrier leakage mechanisms, thus realizing droop-free operation. The discovery of reliable, droop-free devices constitutes significant progress toward the development of nanowires for practical applications. Our monolithic approach realized a high-performance device that will revolutionize the way high power, low-junction-temperature LED lamps are manufactured for solid-state lighting and for applications in high-temperature harsh environment.

OT1_mputman_1: ASCII: All Sky observations of Galactic CII

NASA Astrophysics Data System (ADS)

Putman, M.

2010-07-01

The Milky Way and other galaxies require a significant source of ongoing star formation fuel to explain their star formation histories. A new ubiquitous population of discrete, cold clouds have recently been discovered at the disk-halo interface of our Galaxy that could potentially provide this source of fuel. We propose to observe a small sample of these disk-halo clouds with HIFI to determine if the level of [CII] emission detected suggests they represent the cooling of warm clouds at the interface between the star forming disk and halo. These cooling clouds are predicted by simulations of warm clouds moving into the disk-halo interface region. We target 5 clouds in this proposal for which we have high resolution HI maps and can observe the densest core of the cloud. The results of our observations will also be used to interpret the surprisingly high detections of [CII] for low HI column density clouds in the Galactic Plane by the GOT C+ Key Program by extending the clouds probed to high latitude environments.

Photophoretic Levitation and Trapping of Dust in the Inner Regions of Protoplanetary Disks

NASA Astrophysics Data System (ADS)

McNally, Colin P.; McClure, Melissa K.

2017-01-01

In protoplanetary disks, the differential gravity-driven settling of dust grains with respect to gas and with respect to grains of varying sizes determines the observability of grains, and sets the conditions for grain growth and eventually planet formation. In this work, we explore the effect of photophoresis on the settling of large dust grains in the inner regions of actively accreting protoplanetary disks. Photophoretic forces on dust grains result from the collision of gas molecules with differentially heated grains. We undertake one-dimensional dust settling calculations to determine the equilibrium vertical distribution of dust grains in each column of the disk. In the process we introduce a new treatment of the photophoresis force which is consistent at all optical depths with the representation of the radiative intensity field in a two-stream radiative transfer approximation. The levitation of large dust grains creates a photophoretic dust trap several scale heights above the mid-plane in the inner regions of the disk where the dissipation of accretion energy is significant. We find that differential settling of dust grains is radically altered in these regions of the disk, with large dust grains trapped in a layer below the stellar irradiation surface, where the dust to gas mass ratio can be enhanced by a factor of a hundred for the relevant particles. The photophoretic trapping effect has a strong dependence on particle size and porosity.

A Persistent Disk Wind in GRS 1915+105 with NICER

NASA Astrophysics Data System (ADS)

Neilsen, J.; Cackett, E.; Remillard, R. A.; Homan, J.; Steiner, J. F.; Gendreau, K.; Arzoumanian, Z.; Prigozhin, G.; LaMarr, B.; Doty, J.; Eikenberry, S.; Tombesi, F.; Ludlam, R.; Kara, E.; Altamirano, D.; Fabian, A. C.

2018-06-01

The bright, erratic black hole X-ray binary GRS 1915+105 has long been a target for studies of disk instabilities, radio/infrared jets, and accretion disk winds, with implications that often apply to sources that do not exhibit its exotic X-ray variability. With the launch of the Neutron star Interior Composition Explorer (NICER), we have a new opportunity to study the disk wind in GRS 1915+105 and its variability on short and long timescales. Here we present our analysis of 39 NICER observations of GRS 1915+105 collected during five months of the mission data validation and verification phase, focusing on Fe XXV and Fe XXVI absorption. We report the detection of strong Fe XXVI in 32 (>80%) of these observations, with another four marginal detections; Fe XXV is less common, but both likely arise in the well-known disk wind. We explore how the properties of this wind depend on broad characteristics of the X-ray lightcurve: mean count rate, hardness ratio, and fractional rms variability. The trends with count rate and rms are consistent with an average wind column density that is fairly steady between observations but varies rapidly with the source on timescales of seconds. The line dependence on spectral hardness echoes the known behavior of disk winds in outbursts of Galactic black holes; these results clearly indicate that NICER is a powerful tool for studying black hole winds.

Chromatographic analysis of salicylic compounds in different species of the genus Salix.

PubMed

Pobłocka-Olech, Loretta; van Nederkassel, Anne-Marie; Vander Heyden, Yvan; Krauze-Baranowska, Mirosława; Glód, Daniel; Baczek, Tomasz

2007-11-01

The separation of nine phenol glycosides--salicin, salicortin, 2'-acetylsalicortin, populin, tremulacin, salidroside, triandrin, picein and helicin--by normal phase (NP), reversed phase (RP) HPLC techniques and a coupling of NP and RP monolithic silica columns was studied. Among the above nine compounds only five--salicin, populin, tremulacin, salidroside and triandrin--were resolved in an NP system with a mobile phase comprising hexane/isopropanol/methanol (87:12:1, v/v/v). Optimized separation was performed with two coupled monolithic silica columns of different polarity (bare silica and RP-18). The method was applied to verify the presence of salicylic compounds and other phenolic derivatives in the bark of six species from the genus Salix, namely S. purpurea, S. daphnoides clone 1095, S. alba clone 1100, S. triandra, S. viminalis, and S. herbacea. Gradient elution with a mobile phase composed of acetonitrile and water containing 0.05% of trifluoroacetic acid, with increasing acetonitrile concentration from 3% to 48%, was chosen as optimal. For the selective detection of the salicylic compounds, an evaporative light scattering detector was employed along with a UV detector. The differences in the composition of phenols in the different plant materials were confirmed. Additionally, it must be emphasized that for the first time the presence of 2'-acetylsalicortin was revealed in S. alba clone 1100. Furthermore, an SPE-HPLC method was developed for the rapid analysis of the salicin content, analyzed as free and total fraction, in willow barks. The determined concentrations of total salicin varied from 25.4 mg/g in S. alba clone 1100 to 96.47 mg/g in S. daphnoides clone 1095.

On-line hyphenation of solid-phase extraction to chromatographic separation of sulfonamides with fused-core columns in sequential injection chromatography.

PubMed

Batista, Alex D; Chocholouš, Petr; Satínský, Dalibor; Solich, Petr; Rocha, Fábio R P

2015-02-01

On-line sample pretreatment (clean-up and analyte preconcentration) is for the first time coupled to sequential injection chromatography. The approach combines anion-exchange solid-phase extraction and the highly effective pentafluorophenylpropyl (F5) fused-core particle column for separation of eight sulfonamide antibiotics with similar structures (sulfathiazole, sulfanilamide, sulfacetamide, sulfadiazine, sulfamerazine, sulfadimidine, sulfamethoxazole and sulfadimethoxine). The stationary phase was selected after a critical comparison of the performance achieved by three fused-core reversed phase columns (Ascentis(®) Express RP-Amide, Phenyl-Hexyl, and F5) and two monolithic columns (Chromolith(®) High Resolution RP-18 and CN). Acetonitrile and acetate buffer pH 5.0 at 0.60 mL min(-1) were used as mobile phase to perform the separations before spectrophotometric detection. The first mobile phase was successfully used as eluent from SPE column ensuring transfer of a narrow zone to the chromatographic column. Enrichment factors up to 39.2 were achieved with a 500 µL sample volume. The developed procedure showed analysis time <10.5 min, resolutions >1.83 with peak symmetry ≤1.52, LODs between 4.9 and 27 µg L(-1), linear response ranges from 30.0 to 1000.0 µg L(-1) (r(2)>0.996) and RSDs of peak heights <2.9% (n=6) at a 100 µg L(-1) level and enabled the screening control of freshwater samples contaminated at the 100 µg L(-1) level. The proposed approach expanded the analytical potentiality of SIC and avoided the time-consuming batch sample pretreatment step, thus minimizing risks of sample contamination and analyte losses. Copyright © 2014 Elsevier B.V. All rights reserved.

CN rings in full protoplanetary disks around young stars as probes of disk structure

NASA Astrophysics Data System (ADS)

Cazzoletti, P.; van Dishoeck, E. F.; Visser, R.; Facchini, S.; Bruderer, S.

2018-01-01

Aims: Bright ring-like structure emission of the CN molecule has been observed in protoplanetary disks. We investigate whether such structures are due to the morphology of the disk itself or if they are instead an intrinsic feature of CN emission. With the intention of using CN as a diagnostic, we also address to which physical and chemical parameters CN is most sensitive. Methods: A set of disk models were run for different stellar spectra, masses, and physical structures via the 2D thermochemical code DALI. An updated chemical network that accounts for the most relevant CN reactions was adopted. Results: Ring-shaped emission is found to be a common feature of all adopted models; the highest abundance is found in the upper outer regions of the disk, and the column density peaks at 30-100 AU for T Tauri stars with standard accretion rates. Higher mass disks generally show brighter CN. Higher UV fields, such as those appropriate for T Tauri stars with high accretion rates or for Herbig Ae stars or for higher disk flaring, generally result in brighter and larger rings. These trends are due to the main formation paths of CN, which all start with vibrationally excited H_2^* molecules, that are produced through far ultraviolet (FUV) pumping of H2. The model results compare well with observed disk-integrated CN fluxes and the observed location of the CN ring for the TW Hya disk. Conclusions: CN rings are produced naturally in protoplanetary disks and do not require a specific underlying disk structure such as a dust cavity or gap. The strong link between FUV flux and CN emission can provide critical information regarding the vertical structure of the disk and the distribution of dust grains which affects the UV penetration, and could help to break some degeneracies in the SED fitting. In contrast with C2H or c-C3H2, the CN flux is not very sensitive to carbon and oxygen depletion.

Modeling of Spinal Column of Seated Human Body under Exposure to Whole-Body Vibration

NASA Astrophysics Data System (ADS)

Tamaoki, Gen; Yoshimura, Takuya; Kuriyama, Kaoru; Nakai, Kazuma

In vehicle systems occupational drivers might expose themselves to vibration for a long time. This may cause illness of the spinal column such as low back pain. Therefore, it is necessary to evaluate the influence of vibration to the spinal column. Thus the modeling of seated human body is conducted in order to evaluate the effect of whole-body vibration to the spinal column. This model has the spinal column and the support structures such as the muscles of the back and the abdomen. The spinal column is made by the vertebrae and the intervertebral disks that are considered the rigid body and the rotational spring and damper respectively. The parameter of this model is decided by the literature and the body type of the subject with respect to the mass and the model structure. And stiffness and damping parameters are searched by fitting the model simulation results to the experimental measured data with respect to the vibration transmissibilities from the seat surface to the spinal column and the head and with respect to the driving-point apparent mass. In addition, the natural modes of the model compare with the result of experimental modal analysis. The influence of the abdomen and the muscles of the back are investigated by comparing three models with respect to above vibration characteristics. Three model are the proposed model, the model that has the spinal column and the model that has the muscles of the back in addition to the spinal column.

Comprehensive overview of recent preparation and application trends of various open tubular capillary columns in separation science.

PubMed

Cheong, Won Jo; Ali, Faiz; Kim, Yune Sung; Lee, Jin Wook

2013-09-20

Open tubular (OT) capillary columns have been increasingly used in a variety of fields of separation science such as CEC, LC, and SPE. Especially their application in CEC has attracted a lot of attention for their outstanding separation performance. Various forms of OT stationary phase materials have been employed such as in-situ prepared polymers, molecular imprinted polymers (MIPs), brush ligands, host ligands, block copolymers, aptamers, carbon nanotubes, polysaccharides, proteins, tentacles, nanoparticles, monoliths, and polyelectrolyte multi-layers. They have been prepared either in the chemically bound format or physically adsorbed format. Sol-gel technologies and nanoparticles have been sometimes involved in their preparation. There have been also some unique miscellaneous studies, for example, adopting preferentially adsorbed mobile phase components as stationary phases. In this review, recent progresses since mostly 2007 will be critically discussed in detail with some summarized descriptions for the work before the date. Copyright © 2013 Elsevier B.V. All rights reserved.

Capillary liquid chromatographic analysis of fat-soluble vitamins and beta-carotene in combination with in-tube solid-phase microextraction.

PubMed

Xu, Hui; Jia, Li

2009-01-01

A capillary liquid chromatography (CLC) system with UV/vis detection was coupled with an in-tube solid-phase microextraction (SPME) device for the analysis of fat-soluble vitamins and beta-carotene. A monolithic silica-ODS column was used as the extraction medium. An optical-fiber flow cell with a long light path in the UV/vis detector was utilized to further enhance the detection sensitivity. In the in-tube SPME/CLC system, the pre-condition of the extraction column and the effect of the injection volume were investigated. The detection limits (LOD) for the fat-soluble vitamins and beta-carotene were in the range from 1.9 to 173 ng/mL based on the signal-to-noise ratio of 3 (S/N=3). The relative standard deviations of migration time and peak area for each analyte were less than 5.0%. The method was applied to the analysis of fat-soluble vitamins and beta-carotene contents in corns.

Low pressure ion chromatography with a low cost paired emitter-detector diode based detector for the determination of alkaline earth metals in water samples.

PubMed

Barron, Leon; Nesterenko, Pavel N; Diamond, Dermot; O'Toole, Martina; Lau, King Tong; Paull, Brett

2006-09-01

The use of a low pressure ion chromatograph based upon short (25 mm x 4.6 mm) surfactant coated monolithic columns and a low cost paired emitter-detector diode (PEDD) based detector, for the determination of alkaline earth metals in aqueous matrices is presented. The system was applied to the separation of magnesium, calcium, strontium and barium in less than 7min using a 0.15M KCl mobile phase at pH 3, with post-column reaction detection at 570 nm using o-cresolphthalein complexone. A comparison of the performance of the PEDD detector with a standard laboratory absorbance detector is shown, with limits of detection for magnesium and calcium using the low cost PEDD detector equal to 0.16 and 0.23 mg L(-1), respectively. Finally, the developed system was used for the determination of calcium and magnesium in a commercial spring water sample.

Simultaneous determination of D-aspartic acid and D-glutamic acid in rat tissues and physiological fluids using a multi-loop two-dimensional HPLC procedure.

PubMed

Han, Hai; Miyoshi, Yurika; Ueno, Kyoko; Okamura, Chieko; Tojo, Yosuke; Mita, Masashi; Lindner, Wolfgang; Zaitsu, Kiyoshi; Hamase, Kenji

2011-11-01

For a metabolomics study focusing on the analysis of aspartic and glutamic acid enantiomers, a fully automated two-dimensional HPLC system employing a microbore-ODS column and a narrowbore-enantioselective column was developed. By using this system, a detailed distribution of D-Asp and D-Glu besides L-Asp and L-Glu in mammals was elucidated. For the total analysis concept, the amino acids were first pre-column derivatized with 4-fluoro-7-nitro-2,1,3-benzoxadiazole (NBD-F) to be sensitively and fluorometrically detected. For the non-stereoselective separation of the analytes in the first dimension a monolithic ODS column (750 mm × 0.53 mm i.d.) was adopted, and a self-packed narrowbore-Pirkle type enantioselective column (Sumichiral OA-2500S, 250 mm × 1.5 mm i.d.) was selected for the second dimension. In the rat plasma, RSD values for intra-day and inter-day precision were less than 6.8%, and the accuracy ranged between 96.1% and 105.8%. The values of LOQ of D-Asp and D-Glu were 5 fmol/injection (0.625 nmol/g tissue). The present method was successfully applied to the simultaneous determination of free aspartic acid and glutamic acid enantiomers in 7 brain areas, 11 peripheral tissues, plasma and urine of Wistar rats. Biologically significant D-Asp values were found in various tissue samples whereas for D-Glu the values were very low possibly indicating less significance. Copyright © 2011 Elsevier B.V. All rights reserved.

Disk-Wind Connection During the Heartbeats of GRS 1915+105

NASA Technical Reports Server (NTRS)

Zoghbi, Abderahmen; Miller, J. M.; King, A. L.; Miller, M. C.; Proga, D.; Kallman, T.; Fabian, A. C.; Harrison, F. A.; Kaastra, J.; Raymond, J.;

Water vapor distribution in protoplanetary disks

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

Du, Fujun; Bergin, Edwin A., E-mail: fdu@umich.edu

Water vapor has been detected in protoplanetary disks. In this work, we model the distribution of water vapor in protoplanetary disks with a thermo-chemical code. For a set of parameterized disk models, we calculate the distribution of dust temperature and radiation field of the disk with a Monte Carlo method, and then solve the gas temperature distribution and chemical composition. The radiative transfer includes detailed treatment of scattering by atomic hydrogen and absorption by water of Lyα photons, since the Lyα line dominates the UV spectrum of accreting young stars. In a fiducial model, we find that warm water vapormore » with temperature around 300 K is mainly distributed in a small and well-confined region in the inner disk. The inner boundary of the warm water region is where the shielding of UV field due to dust and water itself become significant. The outer boundary is where the dust temperature drops below the water condensation temperature. A more luminous central star leads to a more extended distribution of warm water vapor, while dust growth and settling tends to reduce the amount of warm water vapor. Based on typical assumptions regarding the elemental oxygen abundance and the water chemistry, the column density of warm water vapor can be as high as 10{sup 22} cm{sup –2}. A small amount of hot water vapor with temperature higher than ∼300 K exists in a more extended region in the upper atmosphere of the disk. Cold water vapor with temperature lower than 100 K is distributed over the entire disk, produced by photodesorption of the water ice.« less

A KEPLERIAN-LIKE DISK AROUND THE FORMING O-TYPE STAR AFGL 4176

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

Johnston, Katharine G.; Hoare, Melvin G.; Robitaille, Thomas P.

We present Atacama Large Millimeter/submillimeter Array line and continuum observations at 1.2 mm with ∼0.″3 resolution that uncover a Keplerian-like disk around the forming O-type star AFGL 4176. The continuum emission from the disk at 1.21 mm (source mm1) has a deconvolved size of 870 ± 110 AU × 330 ± 300 AU and arises from a structure ∼8 M{sub ⊙} in mass, calculated assuming a dust temperature of 190 K. The first-moment maps, pixel-to-pixel line modeling, assuming local thermodynamic equilibrium (LTE), and position–velocity diagrams of the CH{sub 3}CN J = 13–12 K-line emission all show a velocity gradient alongmore » the major axis of the source, coupled with an increase in velocity at small radii, consistent with Keplerian-like rotation. The LTE line modeling shows that where CH{sub 3}CN J = 13–12 is excited, the temperatures in the disk range from ∼70 to at least 300 K and that the H{sub 2} column density peaks at 2.8 × 10{sup 24} cm{sup −2}. In addition, we present Atacama Pathfinder Experiment {sup 12}CO observations that show a large-scale outflow from AFGL 4176 perpendicular to the major axis of mm1, supporting the disk interpretation. Finally, we present a radiative transfer model of a Keplerian disk surrounding an O7 star, with a disk mass and radius of 12 M{sub ⊙} and 2000 AU that reproduces the line and continuum data, further supporting our conclusion that our observations have uncovered a Keplerian-like disk around an O-type star.« less

On Shocks Driven by High-mass Planets in Radiatively Inefficient Disks. II. Three-dimensional Global Disk Simulations

NASA Astrophysics Data System (ADS)

Lyra, Wladimir; Richert, Alexander J. W.; Boley, Aaron; Turner, Neal; Mac Low, Mordecai-Mark; Okuzumi, Satoshi; Flock, Mario

2016-02-01

Recent high-resolution, near-infrared images of protoplanetary disks have shown that these disks often present spiral features. Spiral arms are among the structures predicted by models of disk-planet interaction and thus it is tempting to suspect that planetary perturbers are responsible for these signatures. However, such interpretation is not free of problems. The observed spirals have large pitch angles, and in at least one case (HD 100546) it appears effectively unpolarized, implying thermal emission of the order of 1000 K (465 ± 40 K at closer inspection). We have recently shown in two-dimensional models that shock dissipation in the supersonic wake of high-mass planets can lead to significant heating if the disk is sufficiently adiabatic. Here we extend this analysis to three dimensions in thermodynamically evolving disks. We use the Pencil Code in spherical coordinates for our models, with a prescription for thermal cooling based on the optical depth of the local vertical gas column. We use a 5MJ planet, and show that shocks in the region around the planet where the Lindblad resonances occur heat the gas to substantially higher temperatures than the ambient gas. The gas is accelerated vertically away from the midplane to form shock bores, and the gas falling back toward the midplane breaks up into a turbulent surf. This turbulence, although localized, has high α values, reaching 0.05 in the inner Lindblad resonance, and 0.1 in the outer one. We find evidence that the disk regions heated up by the shocks become superadiabatic, generating convection far from the planet’s orbit.

Disk-Wind Connection during the Heartbeats of GRS 1915+105

NASA Astrophysics Data System (ADS)

Zoghbi, Abderahmen; Miller, J. M.; King, A. L.; Miller, M. C.; Proga, D.; Kallman, T.; Fabian, A. C.; Harrison, F. A.; Kaastra, J.; Raymond, J.; Reynolds, C. S.; Boggs, S. E.; Christensen, F. E.; Craig, W.; Hailey, C. J.; Stern, D.; Zhang, W. W.

2016-12-01

Disk and wind signatures are seen in the soft state of Galactic black holes, while the jet is seen in the hard state. Here we study the disk-wind connection in the ρ class of variability in GRS 1915+105 using a joint NuSTAR-Chandra observation. The source shows 50 s limit cycle oscillations. By including new information provided by the reflection spectrum and using phase-resolved spectroscopy, we find that the change in the inner disk inferred from the blackbody emission is not matched by reflection measurements. The latter is almost constant, independent of the continuum model. The two radii are comparable only if the disk temperature color correction factor changes, an effect that could be due to the changing opacity of the disk caused by changes in metal abundances. The disk inclination is similar to that inferred from the jet axis, and oscillates by ˜10°. The simultaneous Chandra data show the presence of two wind components with velocities between 500 and 5000 km s-1, and possibly two more with velocities reaching 20,000 km s-1 (˜0.06 c). The column densities are ˜5 × 1022 cm-2. An upper limit to the wind response time of 2 s is measured, implying a launch radius of <6 × 1010 cm. The changes in wind velocity and absorbed flux require the geometry of the wind to change during the oscillations, constraining the wind to be launched from a distance of 290-1300 r g from the black hole. Both data sets support fundamental model predictions in which a bulge originates in the inner disk and moves outward as the instability progresses.

[The possibilities for diagnostics of prescription of death coming based on the changes in the lumbar intervertebral disks (the comparison of the morphological, immunohistochemical and topographical findings)].

PubMed

Byval'tsev, V A; Stepanov, I A; Semenov, A V; Perfil'ev, D V; Belykh, E G; Bardonova, L A; Nikiforov, S B; Sudakov, N P; Bespyatykh, I V; Antipina, S L

The objective of the present study was the comprehensive analysis of the postmortem changes in the lumbar intervertebral disks within different periods after death. A total of seven vertebromotor segments were distinguished in the lumbosacral region of the vertebral column based on the examination of 7 corpses. All these segments were divided into three groups in accordance with the prescription of death coming as follows: up to 12 hours (group 1), between 12 and 24 hours (group 2), and between 24 and 36 hours (group 3) after death. The models of the segments thus obtained were subjected to the study by means of diffusion weighted MRI. The removed intervertebral disks were used for morphological and immunohistochemical investigations. The comparison of the diffusion coefficients (DI) revealed the significant difference between the intervertebral disks assigned to groups 1 and 2 (p<0.01). The number of the cells in the pulpal core, the vertebral end plate, and the fibrous ring in all the above groups of the intervertebral disks was significantly reduced (p<0.01). The analysis of the correlation dependence between cell density and diffusion coefficients has demonstrated the well apparent relationship between these characteristics of the intervertebral disks comprising groups 1 and 2. It is concluded that diffusion weighted MRI in the combination with the calculation of diffusion coefficients for the intervertebral disks provides a tool for diagnostics of prescription of death coming as confirmed by the results of the morphometric studies and immunohistochemical analysis.

Determination of intracellular glutathione and cysteine using HPLC with a monolithic column after derivatization with monobromobimane.

PubMed

Conlan, Xavier A; Stupka, Nicole; McDermott, Geoffrey P; Francis, Paul S; Barnett, Neil W

2010-05-01

An optimized high-performance liquid chromatography (HPLC) method is used to show that, as myoblasts differentiate into multinucleated muscle fibers, there is a shift to a more oxidized cell redox state. The HPLC method incorporated derivatization with monobromobimane for the determination of the reduced (GSH) and oxidized (GSSG) forms of glutathione and the reduced (Cys) and oxidized (CysSS) forms of cysteine. The derivatization was optimized to improve the sensitivity of the approach; the limits of detection for glutathione and cysteine were 3 x 10(-8) and 5 x 10(-8) M, respectively. 2009 John Wiley & Sons, Ltd.

Modelling of microalgal growth and lipid production in Dunaliella tertiolecta using nitrogen-phosphorus-potassium fertilizer medium in sintered disk chromatographic glass bubble column.

PubMed

Kumar, Anup; Guria, Chandan; Chitres, G; Chakraborty, Arunangshu; Pathak, A K

2016-10-01

A comprehensive mathematical model involving NPK-10:26:26 fertilizer, NaCl, NaHCO3, light and temperature operating variables for Dunaliella tertiolecta cultivation is formulated to predict microalgae-biomass and lipid productivity. Proposed model includes Monod/Andrews kinetics for the absorption of essential nutrients into algae-biomass and Droop model involving internal nutrient cell quota for microalgae growth, assuming algae-biomass is composed of sugar, functional-pool and neutral-lipid. Biokinetic model parameters are determined by minimizing the residual-sum-of-square-errors between experimental and computed microalgae-biomass and lipid productivity using genetic algorithm. Developed model is validated with the experiments of Dunaliella tertiolecta cultivation using air-agitated sintered-disk chromatographic glass-bubble column and the effects of operating variables on microalgae-biomass and lipid productivity is investigated. Finally, parametric sensitivity analysis is carried out to know the sensitivity of model parameters on the obtained results in the input parameter space. Proposed model may be helpful in scale-up studies and implementation of model-based control strategy in large-scale algal cultivation. Copyright © 2016 Elsevier Ltd. All rights reserved.

PHOTOPHORETIC LEVITATION AND TRAPPING OF DUST IN THE INNER REGIONS OF PROTOPLANETARY DISKS

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

McNally, Colin P.; McClure, Melissa K., E-mail: cmcnally@nbi.dk, E-mail: mmcclure@eso.org

In protoplanetary disks, the differential gravity-driven settling of dust grains with respect to gas and with respect to grains of varying sizes determines the observability of grains, and sets the conditions for grain growth and eventually planet formation. In this work, we explore the effect of photophoresis on the settling of large dust grains in the inner regions of actively accreting protoplanetary disks. Photophoretic forces on dust grains result from the collision of gas molecules with differentially heated grains. We undertake one-dimensional dust settling calculations to determine the equilibrium vertical distribution of dust grains in each column of the disk.more » In the process we introduce a new treatment of the photophoresis force which is consistent at all optical depths with the representation of the radiative intensity field in a two-stream radiative transfer approximation. The levitation of large dust grains creates a photophoretic dust trap several scale heights above the mid-plane in the inner regions of the disk where the dissipation of accretion energy is significant. We find that differential settling of dust grains is radically altered in these regions of the disk, with large dust grains trapped in a layer below the stellar irradiation surface, where the dust to gas mass ratio can be enhanced by a factor of a hundred for the relevant particles. The photophoretic trapping effect has a strong dependence on particle size and porosity.« less

Relevant signs of stable and unstable thoracolumbar vertebral column trauma

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

Gehweiler, J.A.; Daffner, R.H.; Osborne, R.L.

1981-12-01

One-hundred and seventeen patients with acute thoracolumbar vertebral column fracture or fracture-dislocations were analyzed and classified into stable (36%) and unstable (64%). Eight helpful roentgen signs were observed that may serve to direct attention to serious underlying, often occult, fractures and dislocations. The changes fall into four principal groups: abnormal soft tissues, abnormal vertebral alignment, abnormal joints, and widened vertebral canal. All stable and unstable lesions showed abnormal soft tissues, while 70% demonstrated kyphosis and/or scoliosis, and an abnormal adjacent intervertebral disk space. All unstable lesions showed one or more of the following signs: displaced vertebra, widened interspinous space, abnormalmore » apophyseal joint(s), and widened vertebral canal.« less

Experimental Investigation of Rotating Menisci

NASA Astrophysics Data System (ADS)

Reichel, Yvonne; Dreyer, Michael E.

2014-07-01

In upper stages of spacecrafts, Propellant Management Devices (PMD's) can be used to position liquid propellant over the outlet in the absence of gravity. Centrifugal forces due to spin of the upper stage can drive the liquid away from the desired location resulting in malfunction of the stage. In this study, a simplified model consisting of two parallel, segmented and unsegmented disks and a central tube assembled at the center of the upper disk is analyzed experimentally during rotation in microgravity. For each drop tower experiment, the angular speed caused by a centrifugal stage in the drop capsule is kept constant. Steady-states for the menisci between the disks are observed for moderate rotation. For larger angular speeds, a stable shape of the free surfaces fail to sustain and the liquid is driven away. Additionally, tests were performed without rotation to quantify two effects: the removal of a metallic cylinder around the model to establish the liquid column and the determination of the the settling time from terrestrial to microgravity conditions.

Resolving the Nuclear Obscuring Disk in the Compton-thick Seyfert Galaxy NGC 5643 with ALMA

NASA Astrophysics Data System (ADS)

Alonso-Herrero, A.; Pereira-Santaella, M.; García-Burillo, S.; Davies, R. I.; Combes, F.; Asmus, D.; Bunker, A.; Díaz-Santos, T.; Gandhi, P.; González-Martín, O.; Hernán-Caballero, A.; Hicks, E.; Hönig, S.; Labiano, A.; Levenson, N. A.; Packham, C.; Ramos Almeida, C.; Ricci, C.; Rigopoulou, D.; Rosario, D.; Sani, E.; Ward, M. J.

2018-06-01

We present ALMA Band 6 12CO(2–1) line and rest-frame 232 GHz continuum observations of the nearby Compton-thick Seyfert galaxy NGC 5643 with angular resolutions 0.″11–0.″26 (9–21 pc). The CO(2–1) integrated line map reveals emission from the nuclear and circumnuclear region with a two-arm nuclear spiral extending ∼10″ on each side. The circumnuclear CO(2–1) kinematics can be fitted with a rotating disk, although there are regions with large residual velocities and/or velocity dispersions. The CO(2–1) line profiles of these regions show two different velocity components. One is ascribed to the circular component and the other to the interaction of the AGN outflow, as traced by the [O III]λ5007 Å emission, with molecular gas in the disk a few hundred parsecs from the AGN. On nuclear scales, we detected an inclined CO(2–1) disk (diameter 26 pc, FWHM) oriented almost in a north–south direction. The CO(2–1) nuclear kinematics can be fitted with a rotating disk that appears to be tilted with respect to the large-scale disk. There are strong non-circular motions in the central 0.″2–0.″3 with velocities of up to 110 km s‑1. In the absence of a nuclear bar, these motions could be explained as radial outflows in the nuclear disk. We estimate a total molecular gas mass for the nuclear disk of M(H2) = 1.1 × 107 M ⊙ and an H2 column density toward the location of the AGN of N(H2) ∼ 5 × 1023 cm‑2, for a standard CO-to-H2 conversion factor. We interpret this nuclear molecular gas disk as the obscuring torus of NGC 5643 as well as the collimating structure of the ionization cone.

Herschel survey and modelling of externally-illuminated photoevaporating protoplanetary disks.

PubMed

Champion, J; Berné, O; Vicente, S; Kamp, I; Le Petit, F; Gusdorf, A; Joblin, C; Goicoechea, J R

2017-08-01

Protoplanetary disks undergo substantial mass-loss by photoevaporation, a mechanism which is crucial to their dynamical evolution. However, the processes regulating the gas energetics have not been well constrained by observations so far. We aim at studying the processes involved in disk photoevaporation when it is driven by far-UV photons (i.e. 6 < E < 13.6 eV). We present a unique Herschel survey and new ALMA observations of four externally-illuminated photoevaporating disks (a.k.a. proplyds). For the analysis of these data, we developed a 1D model of the photodissociation region (PDR) of a proplyd, based on the Meudon PDR code and we computed the far infrared line emission. With this model, we successfully reproduce most of the observations and derive key physical parameters, i.e. densities at the disk surface of about 10 6 cm -3 and local gas temperatures of about 1000 K. Our modelling suggests that all studied disks are found in a transitional regime resulting from the interplay between several heating and cooling processes that we identify. These differ from those dominating in classical PDRs i.e. grain photo-electric effect and cooling by [OI] and [CII] FIR lines. This specific energetic regime is associated to an equilibrium dynamical point of the photoevaporation flow: the mass-loss rate is self-regulated to keep the envelope column density at a value that maintains the temperature at the disk surface around 1000 K. From the physical parameters derived from our best-fit models, we estimate mass-loss rates - of the order of 10 -7 M ⊙ /yr - that are in agreement with earlier spectroscopic observation of ionised gas tracers. This holds only if we assume photoevaporation in the supercritical regime where the evaporation flow is launched from the disk surface at sound speed. We have identified the energetic regime regulating FUV-photoevaporation in proplyds. This regime could be implemented into models of the dynamical evolution of protoplanetary disks.

The Mass and Absorption Columns of Galactic Gaseous Halos

NASA Astrophysics Data System (ADS)

Qu, Zhijie; Bregman, Joel N.

2018-01-01

The gaseous halo surrounding the galaxy is a reservoir for the gas on the galaxy disk, supplying materials for the star formation. We developed a gaseous halo model connecting the galactic disk and the gaseous halo by assuming the star formation rate is equal to the radiative cooling rate. Besides the single-phase collisional gaseous halo, we also consider the photoionization effect and a time-independent cooling model that assumes the mass cooling rate is constant over all temperatures. The photoionization dominates the low mass galaxy and the outskirts of the massive galaxy due to the low-temperature or low-density nature. The multi-phase cooling model dominates the denser region within the cooling radius, where the efficient radiative cooling must be included. Applying these two improvements, our model can reproduce the most of observed high ionization state ions (i.e., O VI, O VII, Ne VIII and Mg X). Our models show that the O VI column density is almost a constant of around 10^14 cm^-2 over a wide stellar mass from M_\\star ~10^8 M_Sun to 10^11 M_Sun, which is constant with current observations. This model also implies the O VI is photoionized for the galaxy with a halo mass <~ 3 * 10^11 M_Sun, while for more massive galaxies, the O VI is from the cooling-down medium from higher temperature materials (collisional ionized). As higher ionization states, Mg X and Ne VIII are also consistent with observations with the column density of 10^13.5 - 10^14.0 cm^-2, however, the absorber-galaxy pair sample is few to constrain the connection with the galaxy. Based on our calculation, such a gaseous halo cannot close the census of baryonic materials in the galaxy, which shows the same tendency as the baryonic fraction function of the EAGLE simulation. Finally, our model predicts plateaus of the Ne VIII and the Mg X column densities above the sub-L^* galaxy, and the possibly detectable O VII and O VIII column densities for low-mass galaxies, which help to determine the required detection limit for the future observations and missions.

Developing Inventory Records Using the AppleWorks Data Base Subprogram and Apple IIe or GS Computers.

ERIC Educational Resources Information Center

Schlenker, Richard M.

This manual is a "how to" training device for developing inventory records in the AppleWorks program using an Apple IIe or Apple IIGS Computer with Duodisk or two disk drives and an 80-column card. The manual provides step-by-step directions, and includes 17 figures depicting the computer screen at the various stages of the inventory…

UV Spectroscopy of Star-Grazing Comets Within the 49 Ceti Debris Disk

NASA Technical Reports Server (NTRS)

Miles, Brittany E.; Roberge, Aki; Welsh, Barry

2016-01-01

We present the analysis of time-variable Doppler-shifted absorption features in far-UV spectra of the unusual 49 Ceti debris disk. This nearly edge-on disk is one of the brightest known and is one of the very few containing detectable amounts of circumstellar (CS) gas as well as dust. In our two visits of Hubble Space Telescope STIS spectra, variable absorption features are seen on the wings of lines arising from CII and CIV but not for any of the other CS absorption lines. Similar variable features have long been seen in spectra of the well-studied Beta Pictoris debris disk and attributed to the transits of star-grazing comets. We calculated the velocity ranges and apparent column densities of the 49 Cet variable gas, which appears to have been moving at velocities of tens to hundreds of kms(-1) relative to the central star. The velocities in the redshifted variable event seen in the second visit show that the maximum distances of the in falling gas at the time of transit were about 0.050.2 au from the central star. A preliminary attempt at a composition analysis of the redshifted event suggests that the C/O ratio in the in falling gas is super-solar, as it is in the bulk of the stable disk gas.

A gas density drop in the inner 6 AU of the transition disk around the Herbig Ae star HD 139614 . Further evidence for a giant planet inside the disk?

NASA Astrophysics Data System (ADS)

Carmona, A.; Thi, W. F.; Kamp, I.; Baruteau, C.; Matter, A.; van den Ancker, M.; Pinte, C.; Kóspál, A.; Audard, M.; Liebhart, A.; Sicilia-Aguilar, A.; Pinilla, P.; Regály, Zs.; Güdel, M.; Henning, Th.; Cieza, L. A.; Baldovin-Saavedra, C.; Meeus, G.; Eiroa, C.

2017-02-01

Context. Quantifying the gas surface density inside the dust cavities and gaps of transition disks is important to establish their origin. Aims: We seek to constrain the surface density of warm gas in the inner disk of HD 139614, an accreting 9 Myr Herbig Ae star with a (pre-)transition disk exhibiting a dust gap from 2.3 ± 0.1 to 5.3 ± 0.3 AU. Methods: We observed HD 139614 with ESO/VLT CRIRES and obtained high-resolution (R 90 000) spectra of CO ro-vibrational emission at 4.7 μm. We derived constraints on the disk's structure by modeling the CO isotopolog line-profiles, the spectroastrometric signal, and the rotational diagrams using grids of flat Keplerian disk models. Results: We detected υ = 1 → 0 12CO, 2→1 12CO, 1→0 13CO, 1→0 C18O, and 1→0 C17O ro-vibrational lines. Lines are consistent with disk emission and thermal excitation. 12CO υ = 1 → 0 lines have an average width of 14 km s-1, Tgas of 450 K and an emitting region from 1 to 15 AU. 13CO and C18O lines are on average 70 and 100 K colder, 1 and 4 km s-1 narrower than 12CO υ = 1 → 0, and are dominated by emission at R ≥ 6 AU. The 12CO υ = 1 → 0 composite line-profile indicates that if there is a gap devoid of gas it must have a width narrower than 2 AU. We find that a drop in the gas surface density (δgas) at R < 5-6 AU is required to be able to simultaneously reproduce the line-profiles and rotational diagrams of the three CO isotopologs. Models without a gas density drop generate 13CO and C18O emission lines that are too broad and warm. The value of δgas can range from 10-2 to 10-4 depending on the gas-to-dust ratio of the outer disk. We find that the gas surface density profile at 1 < R < 6 AU is flat or increases with radius. We derive a gas column density at 1 < R < 6 AU of NH = 3 × 1019-1021 cm-2 (7 × 10-5-2.4 × 10-3 g cm-2) assuming NCO = 10-4NH. We find a 5σ upper limit on the CO column density NCO at R ≤ 1 AU of 5 × 1015 cm-2 (NH ≤ 5 × 1019 cm-2). Conclusions: The dust gap in the disk of HD 139614 has molecular gas. The distribution and amount of gas at R ≤ 6 AU in HD 139614 is very different from that of a primordial disk. The gas surface density in the disk at R ≤ 1 AU and at 1 < R < 6 AU is significantly lower than the surface density that would be expected from the accretion rate of HD 139614 (10-8 M⊙ yr-1) assuming a standard viscous α-disk model. The gas density drop, the non-negative density gradient in the gas inside 6 AU, and the absence of a wide (>2 AU) gas gap, suggest the presence of an embedded <2 MJ planet at around 4 AU. Based on CRIRES observations collected at the VLTI and VLT (European Southern Observatory, Paranal, Chile) with program 091.C-0671(B).

CHEMICAL IMAGING OF THE CO SNOW LINE IN THE HD 163296 DISK

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

Qi, Chunhua; Öberg, Karin I.; Andrews, Sean M.

2015-11-10

The condensation fronts (snow lines) of H{sub 2}O, CO, and other abundant volatiles in the midplane of a protoplanetary disk affect several aspects of planet formation. Locating the CO snow line, where the CO gas column density is expected to drop substantially, based solely on CO emission profiles, is challenging. This has prompted an exploration of chemical signatures of CO freeze-out. We present ALMA Cycle 1 observations of the N{sub 2}H{sup +} J = 3−2 and DCO{sup +} J = 4−3 emission lines toward the disk around the Herbig Ae star HD 163296 at ∼0.″5 (60 AU) resolution, and evaluatemore » their utility as tracers of the CO snow line location. The N{sub 2}H{sup +} emission is distributed in a ring with an inner radius at 90 AU, corresponding to a midplane temperature of 25 K. This result is consistent with a new analysis of optically thin C{sup 18}O data, which implies a sharp drop in CO abundance at 90 AU. Thus N{sub 2}H{sup +} appears to be a robust tracer of the midplane CO snow line. The DCO{sup +} emission also has a ring morphology, but neither the inner nor the outer radius coincide with the CO snow line location of 90 AU, indicative of a complex relationship between DCO{sup +} emission and CO freeze-out in the disk midplane. Compared to TW Hya, CO freezes out at a higher temperature in the disk around HD 163296 (25 versus 17 K in the TW Hya disk), perhaps due to different ice compositions. This highlights the importance of actually measuring the CO snow line location, rather than assuming a constant CO freeze-out temperature for all disks.« less

X-ray radiative transfer in protoplanetary disks. The role of dust and X-ray background fields

NASA Astrophysics Data System (ADS)

Rab, Ch.; Güdel, M.; Woitke, P.; Kamp, I.; Thi, W.-F.; Min, M.; Aresu, G.; Meijerink, R.

2018-01-01

Context. The X-ray luminosities of T Tauri stars are about two to four orders of magnitude higher than the luminosity of the contemporary Sun. As these stars are born in clusters, their disks are not only irradiated by their parent star but also by an X-ray background field produced by the cluster members. Aims: We aim to quantify the impact of X-ray background fields produced by young embedded clusters on the chemical structure of disks. Further, we want to investigate the importance of the dust for X-ray radiative transfer in disks. Methods: We present a new X-ray radiative transfer module for the radiation thermo-chemical disk code PRODIMO (PROtoplanetary DIsk MOdel), which includes X-ray scattering and absorption by both the gas and dust component. The X-ray dust opacities can be calculated for various dust compositions and dust-size distributions. For the X-ray radiative transfer we consider irradiation by the star and by X-ray background fields. To study the impact of X-rays on the chemical structure of disks we use the well established disk ionization tracers N2H+ and HCO+. Results: For evolved dust populations (e.g. grain growth), X-ray opacities are mostly dominated by the gas; only for photon energies E ≳ 5-10 keV do dust opacities become relevant. Consequently the local disk X-ray radiation field is only affected in dense regions close to the disk midplane. X-ray background fields can dominate the local X-ray disk ionization rate for disk radii r ≳ 20 au. However, the N2H+ and HCO+ column densities are only significantly affected in cases of low cosmic-ray ionization rates (≲10-19 s-1), or if the background flux is at least a factor of ten higher than the flux level of ≈10-5 erg cm-2 s-1 expected for clusters typical for the solar vicinity. Conclusions: Observable signatures of X-ray background fields in low-mass star-formation regions, like Taurus, are only expected for cluster members experiencing a strong X-ray background field (e.g. due to their location within the cluster). For the majority of the cluster members, the X-ray background field has relatively little impact on the disk chemical structure.

Affinity binding of inclusion bodies on supermacroporous monolithic cryogels using labeling with specific antibodies.

PubMed

Ahlqvist, Josefin; Kumar, Ashok; Sundström, Heléne; Ledung, Erika; Hörnsten, E Gunnar; Enfors, Sven-Olof; Mattiasson, Bo

2006-03-23

A new chromatographic method based on affinity supermacroporous monolithic cryogels is developed for binding and analyzing inclusion bodies during fermentation. The work demonstrated that it is possible to bind specific IgG and IgY antibodies to the 15 and 17 amino acids at the terminus ends of a 33 kDa target protein aggregated as inclusion bodies. The antibody treated inclusion bodies from lysed fermentation broth can be specifically retained in protein A and pseudo-biospecific ligand sulfamethazine modified supermacroporous cryogels. The degree of binding of IgG and IgY treated inclusion bodies to the Protein A and sulfamethazine gels are investigated, as well as the influence of pH on the sulfamethazine ligand. Optimum binding of 78 and 72% was observed on both protein A and sulfamethazine modified cryogel columns, respectively, using IgG labeling of the inclusion bodies. The antibody treated inclusion bodies pass through unretained in the sulfamethazine supermacroporous gel at pH that does not favour the binding between the ligand on the gel and the antibodies on the surface of inclusion bodies. Also the unlabeled inclusion bodies went through the gel unretained, showing no non-specific binding or trapping within the gel. These findings may very well be the foundation for the building of a powerful analytical tool during fermentation of inclusion bodies as well as a convenient way to purify them from fermentation broth. These results also support our earlier findings [Kumar, A., Plieva, F.M., Galaev, I.Yu., Mattiasson, B., 2003. Affinity fractionation of lymphocytes using a monolithic cyogel. J. Immunol. Methods 283, 185-194] with mammalian cells that were surface labeled with specific antibodies and recognized on protein A supermacroporous gels. A general binding and separation system can be established on antibody binding cryogel affinity matrices.

Online analysis of five organic ultraviolet filters in environmental water samples using magnetism-enhanced monolith-based in-tube solid phase microextraction coupled with high-performance liquid chromatography.

PubMed

Mei, Meng; Huang, Xiaojia

2017-11-24

Due to the endocrine disrupting properties, organic UV filters have been a great risk for humans and other organisms. Therefore, development of accurate and effective analytical methods is needed for the determination of UV filters in environmental waters. In this work, a fast, sensitive and environmentally friendly method combining magnetism-enhanced monolith-based in-tube solid phase microextraction with high-performance liquid chromatography with diode array detection (DAD) (ME-MB-IT/SPME-HPLC-DAD) for the online analysis of five organic UV filters in environmental water samples was developed. To extract UV filters effectively, an ionic liquid-based monolithic capillary column doped with magnetic nanoparticles was prepared by in-situ polymerization and used as extraction medium of online ME-MB-IT/SPME-HPLC-DAD system. Several extraction conditions including the intensity of magnetic field, sampling and desorption flow rate, volume of sample and desorption solvent, pH value and ionic strength of sample matrix were optimized thoroughly. Under the optimized conditions, the extraction efficiencies for five organic UV filters were in the range of 44.0-100%. The limits of detection (S/N=3) and limits of quantification (S/N=10) were 0.04-0.26μg/L and 0.12-0.87μg/L, respectively. The precisions indicated by relative standard deviations (RSDs) were less than 10% for both intra- and inter-day variabilities. Finally, the developed method was successfully applied to the determination of UV filters in three environmental water samples and satisfactory results were obtained. Copyright © 2017 Elsevier B.V. All rights reserved.

Phosphorus runoff losses from subsurface-applied poultry litter on coastal plain soils.

PubMed

Kibet, Leonard C; Allen, Arthur L; Kleinman, Peter J A; Feyereisen, Gary W; Church, Clinton; Saporito, Lou S; Way, Thomas R

2011-01-01

The application of poultry litter to soils is a water quality concern on the Delmarva Peninsula, as runoff contributes P to the eutrophic Chesapeake Bay. This study compared a new subsurface applicator for poultry litter with conventional surface application and tillage incorporation of litter on a Coastal Plain soil under no-till management. Monolith lysimeters (61 cm by 61 cm by 61 cm) were collected immediately after litter application and subjected to rainfall simulation (61 mm h(-1) 1 h) 15 and 42 d later. In the first rainfall event, subsurface application of litter significantly lowered total P losses in runoff (1.90 kg ha(-1)) compared with surface application (4.78 kg ha(-1)). Losses of P with subsurface application were not significantly different from disked litter or an unamended control. By the second event, total P losses did not differ significantly between surface and subsurface litter treatments but were at least twofold greater than losses from the disked and control treatments. A rising water table in the second event likely mobilized dissolved forms of P in subsurface-applied litter to the soil surface, enriching runoff water with P. Across both events, subsurface application of litter did not significantly decrease cumulative losses of P relative to surface-applied litter, whereas disking the litter into the soil did. Results confirm the short-term reduction of runoff P losses with subsurface litter application observed elsewhere but highlight the modifying effect of soil hydrology on this technology's ability to minimize P loss in runoff.

MOLECULAR GAS DISK STRUCTURES AROUND ACTIVE GALACTIC NUCLEI

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

Wada, Keiichi; Papadopoulos, Padeli P.; Spaans, Marco

We present new high-resolution numerical simulations of the interstellar medium (ISM) in a central R {<=} 32 parsecs region around a supermassive black hole (1.3 x 10{sup 7} M{sub sun}) at a galactic center. Three-dimensional hydrodynamic modeling of the ISM (Wada and Norman 2002) with the nuclear starburst now includes tracking of the formation of molecular hydrogen (H{sub 2}) out of the neutral hydrogen phase as a function of the evolving ambient ISM conditions with a finer spatial resolution (0.125 pc). In a quasi-equilibrium state, mass fraction of H{sub 2} is about 0.4 (total H{sub 2} mass is {approx_equal}1.5 xmore » 10{sup 6} M{sub sun}) of the total gas mass for the uniform far ultra-violet (FUV) with G {sub 0} = 10 in Habing unit. As shown in the previous model, the gas forms an inhomogeneous disk, whose scale height becomes larger in the outer region. H{sub 2} forms a thin nuclear disk in the inner {approx_equal}5 pc, which is surrounded by molecular clouds swelled up toward h {approx}< 10 pc. The velocity field of the disk is highly turbulent in the torus region, whose velocity dispersion is {approx_equal}20 km s{sup -1} on average. Average supernova (SN) rate of {approx_equal}5 x 10{sup -5} yr{sup -1} is large enough to energize these structures. Gas column densities toward the nucleus larger than 10{sup 22} cm{sup -2} are observed if the viewing angle is smaller than {theta} {sub v} {approx_equal} 50 deg. from the edge-on. However, the column densities are distributed over almost two orders of magnitude around the average for any given viewing angle due to the clumpy nature of the torus. For a stronger FUV (G {sub 0} = 100), the total H{sub 2} mass in an equilibrium is only slightly smaller ({approx_equal}0.35), a testimony to the strong self-shielding nature of H{sub 2}, and the molecular gas is somewhat more concentrated in a midplane. Other properties of the ISM are not very sensitive either to the FUV intensity or the SN rate. Finally, the morphology and kinematics of the circum nuclear molecular gas disks emerging from our models are similar to that revealed by recent near infrared observations using VLTI/Keck.« less

THE ROLES OF RADIATION AND RAM PRESSURE IN DRIVING GALACTIC WINDS

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

Sharma, Mahavir; Nath, Biman B., E-mail: mahavir@rri.res.in, E-mail: biman@rri.res.in

We study gaseous outflows from disk galaxies driven by the combined effects of ram pressure on cold gas clouds and radiation pressure on dust grains. Taking into account the gravity due to disk, bulge, and dark matter halo, and assuming continuous star formation in the disk, we show that radiation or ram pressure alone is not sufficient to drive escaping winds from disk galaxies and that both processes contribute. We show that in the parameter space of star formation rate (SFR) and rotation speed of galaxies the wind speed in galaxies with rotation speeds v{sub c} {<=} 200 km s{supmore » -1} and SFR {<=} 100 M{sub Sun} yr{sup -1} has a larger contribution from ram pressure, and that in high-mass galaxies with large SFR radiation from the disk has a greater role in driving galactic winds. The ratio of wind speed to circular speed can be approximated as v{sub w} / v{sub c} {approx} 10{sup 0.7}, [SFR/50{sub Sun }yr{sup -1}]{sup 0.4} [v{sub c}/120 km s{sup -1}]{sup -1.25}. We show that this conclusion is borne out by observations of galactic winds at low and high redshift and also of circumgalactic gas. We also estimate the mass loading factors under the combined effect of ram and radiation pressure, and show that the ratio of mass-loss rate to SFR scales roughly as v{sup -1}{sub c}{Sigma}{sub g}{sup -1}, where {Sigma}{sub g} is the gas column density in the disk.« less

Effects of the type and thickness of ceramic, substrate, and cement on the optical color of a lithium disilicate ceramic.

PubMed

Pires, Laís A; Novais, Pollyanna M R; Araújo, Vinícius D; Pegoraro, Luiz F

2017-01-01

Reproducing the characteristics of natural teeth in ceramic crowns remains a complex and difficult process. The purpose of this in vitro study was to evaluate the effect of the substrate, cement, type, and thickness of the ceramic on the resulting color of a lithium disilicate ceramic. Forty ceramic disks were prepared from IPS e.max Press LT (low translucency) and HO (high opacity) in 2 different thicknesses (1.5 and 2 mm). The LT groups were composed of monolithic ceramic disks, and the HO groups were composed of disks fabricated with a 0.5-mm thickness combined with a 1- or 1.5-mm veneering ceramic thickness. Disks made of composite resin (R) and alloy (A) were used as substrate structures. The resin cement used was Variolink II. Color was measured with a spectrophotometer and expressed in CIELAB coordinates. Color differences (ΔE) were calculated. The data were analyzed with ANOVA and the Tukey HSD test (α=.05). When the ΔE of ceramic disks with both substrates, with and without cement, were compared, the lowest value (3) was obtained for ceramic HO with a 2-mm thickness/alloy substrate/without cement; the highest value (10) was obtained for ceramic LT with a1.5-mm thickness/alloy substrate/with cement. This difference was statistically significant. When the effect of cement on the ΔE of ceramics in both substrates was compared, the lowest value (1.1) occurred with ceramic HO with a 1.5-mm thickness/resin substrate, and the highest was observed for ceramic LT with a 1.5-mm thickness/alloy substrate (6.4). This difference was statistically significant. The substrate color, type and thickness of ceramic, and presence of the cement significantly influenced the resulting optical color. The ΔE values of cemented HO ceramics were lower than that of the LT ceramic. Copyright © 2016 Editorial Council for the Journal of Prosthetic Dentistry. Published by Elsevier Inc. All rights reserved.

Absorption features in the quasar HS 1603 + 3820 II. Distance to the absorber obtained from photoionisation modelling

NASA Astrophysics Data System (ADS)

Różańska, A.; Nikołajuk, M.; Czerny, B.; Dobrzycki, A.; Hryniewicz, K.; Bechtold, J.; Ebeling, H.

2014-04-01

We present the photoionisation modelling of the intrinsic absorber in the bright quasar HS 1603 + 3820. We constructed the broad-band spectral energy distribution using the optical/UV/X-ray observations from different instruments as inputs for the photoionisation calculations. The spectra from the Keck telescope show extremely high CIV to HI ratios, for the first absorber in system A, named A1. This value, together with high column density of CIV ion, place strong constraints on the photoionisation model. We used two photoionisation codes to derive the hydrogen number density at the cloud illuminated surface. By estimating bolometric luminosity of HS 1603 + 3820 using the typical formula for quasars, we calculated the distance to A1. We could find one photoionization solution, by assuming either a constant density cloud (which was modelled using CLOUDY), or a stratified cloud (which was modelled using TITAN), as well as the solar abundances. This model explained both the ionic column density of CIV and the high CIV to HI ratio. The location of A1 is 0.1 pc, and it is situated even closer to the nucleus than the possible location of the Broad Line Region in this object. The upper limit of the distance is sensitive to the adopted covering factor and the carbon abundance. Photoionisation modelling always prefers dense clouds with the number density n0 = 1010 - 1012 cm-3, which explains intrinsic absorption in HS 1603 + 3820. This number density is of the same order as that in the disk atmosphere at the implied distance of A1. Therefore, our results show that the disk wind that escapes from the outermost accretion disk atmosphere can build up dense absorber in quasars.

The Mass and Absorption Columns of Galactic Gaseous Halos

NASA Astrophysics Data System (ADS)

Qu, Zhijie; Bregman, Joel N.

2018-03-01

The galactic gaseous halo is a gas reservoir for the interstellar medium in the galaxy disk, supplying materials for star formation. We developed a gaseous halo model connecting the galaxy disk and the gaseous halo by assuming that the star formation rate on the disk is balanced by the radiative cooling rate of the gaseous halo, including stellar feedback. In addition to a single-temperature gaseous halo in collisional ionization equilibrium, we also consider the photoionization effect and a steady-state cooling model. Photoionization is important for modifying the ion distribution in low-mass galaxies and in the outskirts of massive galaxies due to the low densities. The multiphase cooling model dominates the region within the cooling radius, where t cooling = t Hubble. Our model reproduces most of the observed high ionization state ions for a wide range of galaxy masses (i.e., O VI, O VII, Ne VIII, Mg X, and O VIII). We find that the O VI column density has a narrow range around ≈1014 cm‑2 for halo masses from M ⋆ ≈ 3 × 1010 M ⊙ to 6 × 1012 M ⊙, which is consistent with some but not all observational studies. For galaxies with halo masses ≲3 × 1011 M ⊙, photoionization produces most of the O VI, while for more massive galaxies, the O VI is from the medium that is cooling from higher temperatures. Fitting the Galactic (Milky-Way) O VII and O VIII suggests a gaseous halo model where the metallicity is ≈0.55 Z ⊙ and the gaseous halo has a maximum temperature of ≈1.9 × 106 K. This gaseous halo model does not close the census of baryonic material within R 200.

An Extreme, Blueshifted Iron Line in the Narrow Line Seyfert 1 PG 1402+261

NASA Technical Reports Server (NTRS)

Reeves, J. N.; Porquet, D.; Turner, T. J.

2004-01-01

We report on a short, XMM-Newton observation of the radio-quiet Narrow Line Seyfert 1 PG 1402+261. The EPIC X-ray spectrum of PG 1402+261 shows a strong excess of counts between 6 - 9 keV in the rest frame. This feature can be modeled by an unusually strong (equivalent width 2 keV) and very broad energy at 7.3 keV appears blue-shifted with respect to the iron Kalpha emission band between 6.4 - 6.97 keV, whilst the blue-wing of the line extends to 9 keV in the quasar rest frame. The line profile can be fitted by reflection from the inner accretion disk, but an inclination angle of greater than 60 degrees is required to model the extreme blue-wing of the line. Furthermore the extreme strength of the line requires a geometry whereby the hard X-ray emission from PG1402+261 above 2 keV is dominated by the pure-reflection component from the disk, whilst little or none of the direct hard power-law is observed. Alternatively the spectrum above 2 keV may instead be explained by an ionized absorber, if the column density is sufficiently high (NH greater than 3 x 10(exp 23) per square centimeter) and if the matter is ionized enough to produce a deep (tau approximately equal to 1) iron K-shell absorption edge at 9 keV. This absorber could originate in a large column density, high velocity outflow, perhaps similar to those which appear to be observed in several other high accretion rate AGN. Further observations, especially at higher spectral resolution, are required to distinguish between the accretion disk reflection or outflow scenarios.

Photoionization of disk galaxies: An explanation of the sharp edges in the H I distribution

NASA Technical Reports Server (NTRS)

Dove, James B.; Shull, J. Michael

1994-01-01

We have reproduced the observed radial truncation of the H I distribution in isolated spiral galaxies with a model in which extragalactic radiation photoionizes the gaseous disk. For a galactic mass distribution model that reproduces the observed rotation curves, including dark matter in the disk and halo, the vertical structure of the gas is determined self-consistently. The ionization structure and column densities of H and He ions are computed by solving the radiation transfer equation for both continuum and lines. Our model is similar to that of Maloney, and the H I structure differs by less than 10%. The radial structure of the column density of H I is found to be more sensitive to the extragalactic radiation field than to the distribution of mass. For this reason, considerable progress can be made in determining the extragalactic flux of ionizing photons, phi(sub ex), with more 21 cm observations of isolated galaxies. However, owing to the uncertainty of the radial distribution of total hydrogen at large radii, inferring the extragalactic flux by comparing the observed edges to photoionization models is somewhat subjective. We find 1 x 10(exp 4)/sq cm/s is less than or approximately phi(sub ex) is less than or approximately 5 x 10(exp 4)/sq cm/s, corresponding to 2.1 is less than or approximately iota(sub 0) is less than or approximately 10.5 x 10(exp -23) ergs/sq cm/s/Hz/sr for a 1/nu spectrum. Although somewhat higher, our inferred range of iota(sub 0) is consistent with the large range of values obtained by Kulkarni & Fall from the 'proximity effect' toward Quasi-Stellar Objects (QSOs) at approximately 0.5.

Building Parts Inventory Files Using the AppleWorks Data Base Subprogram and Apple IIe or GS Computers.

ERIC Educational Resources Information Center

Schlenker, Richard M.

This manual is a "how to" training device for building database files using the AppleWorks program with an Apple IIe or Apple IIGS Computer with Duodisk or two disk drives and an 80-column card. The manual provides step-by-step directions, and includes 25 figures depicting the computer screen at the various stages of the database file…

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

Chemerisov, S.; Bailey, J.; Heltemes, T.

A series of four one-day irradiations was conducted with 100Mo-enriched disk targets. After irradiation, the enriched disks were removed from the target and dissolved. The resulting solution was processed using a NorthStar RadioGenix™ 99mTc generator either at Argonne National Laboratory or at the NorthStar Medical Radioisotopes facility. Runs on the RadioGenix system produced inconsistent analytical results for 99mTc in the Tc/Mo solution. These inconsistencies were attributed to the impurities in the solution or improper column packing. During the irradiations, the performance of the optic transitional radiation (OTR) and infrared cameras was tested in high radiation field. The OTR cameras survivedmore » all irradiations, while the IR cameras failed every time. The addition of X-ray and neutron shielding improved camera survivability and decreased the number of upsets.« less

Affinity binding of antibodies to supermacroporous cryogel adsorbents with immobilized protein A for removal of anthrax toxin protective antigen.

PubMed

Ingavle, Ganesh C; Baillie, Les W J; Zheng, Yishan; Lis, Elzbieta K; Savina, Irina N; Howell, Carol A; Mikhalovsky, Sergey V; Sandeman, Susan R

2015-05-01

Polymeric cryogels are efficient carriers for the immobilization of biomolecules because of their unique macroporous structure, permeability, mechanical stability and different surface chemical functionalities. The aim of the study was to demonstrate the potential use of macroporous monolithic cryogels for biotoxin removal using anthrax toxin protective antigen (PA), the central cell-binding component of the anthrax exotoxins, and covalent immobilization of monoclonal antibodies. The affinity ligand (protein A) was chemically coupled to the reactive hydroxyl and epoxy-derivatized monolithic cryogels and the binding efficiencies of protein A, monoclonal antibodies to the cryogel column were determined. Our results show differences in the binding capacity of protein A as well as monoclonal antibodies to the cryogel adsorbents caused by ligand concentrations, physical properties and morphology of surface matrices. The cytotoxicity potential of the cryogels was determined by an in vitro viability assay using V79 lung fibroblast as a model cell and the results reveal that the cryogels are non-cytotoxic. Finally, the adsorptive capacities of PA from phosphate buffered saline (PBS) were evaluated towards a non-glycosylated, plant-derived human monoclonal antibody (PANG) and a glycosylated human monoclonal antibody (Valortim(®)), both of which were covalently attached via protein A immobilization. Optimal binding capacities of 108 and 117 mg/g of antibody to the adsorbent were observed for PANG attached poly(acrylamide-allyl glycidyl ether) [poly(AAm-AGE)] and Valortim(®) attached poly(AAm-AGE) cryogels, respectively, This indicated that glycosylation status of Valortim(®) antibody could significantly increase (8%) its binding capacity relative to the PANG antibody on poly(AAm-AGE)-protien-A column (p < 0.05). The amounts of PA which remained in the solution after passing PA spiked PBS through PANG or Valortim bound poly(AAm-AGE) cryogel were significantly (p < 0.05) decreased relative to the amount of PA remained in the solution after passing through unmodified as well as protein A modified poly(AAm-AGE) cryogel columns, indicates efficient PA removal from spiked PBS over 60 min of circulation. The high adsorption capacity towards anthrax toxin PA of the cryogel adsorbents indicated potential application of these materials for treatment of Bacillus anthracis infection. Copyright © 2015 The Authors. Published by Elsevier Ltd.. All rights reserved.

A CMOS ASIC Design for SiPM Arrays

PubMed Central

Dey, Samrat; Banks, Lushon; Chen, Shaw-Pin; Xu, Wenbin; Lewellen, Thomas K.; Miyaoka, Robert S.; Rudell, Jacques C.

2012-01-01

Our lab has previously reported on novel board-level readout electronics for an 8×8 silicon photomultiplier (SiPM) array featuring row/column summation technique to reduce the hardware requirements for signal processing. We are taking the next step by implementing a monolithic CMOS chip which is based on the row-column architecture. In addition, this paper explores the option of using diagonal summation as well as calibration to compensate for temperature and process variations. Further description of a timing pickoff signal which aligns all of the positioning (spatial channels) pulses in the array is described. The ASIC design is targeted to be scalable with the detector size and flexible to accommodate detectors from different vendors. This paper focuses on circuit implementation issues associated with the design of the ASIC to interface our Phase II MiCES FPGA board with a SiPM array. Moreover, a discussion is provided for strategies to eventually integrate all the analog and mixed-signal electronics with the SiPM, on either a single-silicon substrate or multi-chip module (MCM). PMID:24825923

Pressurized capillary electrochromatographic analysis of water-soluble vitamins by combining with on-line concentration technique.

PubMed

Jia, Li; Liu, Yaling; Du, Yanyan; Xing, Da

2007-06-22

A pressurized capillary electrochromatography (pCEC) system was developed for the separation of water-soluble vitamins, in which UV absorbance was used as the detection method and a monolithic silica-ODS column as the separation column. The parameters (type and content of organic solvent in the mobile phase, type and concentration of electrolyte, pH of the electrolyte buffer, applied voltage and flow rate) affecting the separation resolution were evaluated. The combination of two on-line concentration techniques, namely, solvent gradient zone sharpening effect and field-enhanced sample stacking, was utilized to improve detection sensitivity, which proved to be beneficial to enhance the detection sensitivity by enabling the injection of large volumes of samples. Coupling electrokinetic injection with the on-line concentration techniques was much more beneficial for the concentration of positively charged vitamins. Comparing with the conventional injection mode, the enhancement in the detection sensitivities of water-soluble vitamins using the on-line concentration technique is in the range of 3 to 35-fold. The developed pCEC method was applied to evaluate water-soluble vitamins in corns.

Macromolecular crowding-assisted fabrication of liquid-crystalline imprinted polymers.

PubMed

Zhang, Chen; Zhang, Jing; Huang, Yan-Ping; Liu, Zhao-Sheng

2015-04-01

A macromolecular crowding-assisted liquid-crystalline molecularly imprinted monolith (LC-MIM) was prepared successfully for the first time. The imprinted stationary phase was synthesized with polymethyl methacrylate (PMMA) or polystyrene (PS) as the crowding agent, 4-cyanophenyl dicyclohexyl propylene (CPCE) as the liquid-crystal monomer, and hydroquinidine as the pseudo-template for the chiral separation of cinchona alkaloids in HPLC. A low level of cross-linker (26%) has been found to be sufficient to achieve molecular recognition on the crowding-assisted LC-MIM due to the physical cross-linking of mesogenic groups in place of chemical cross-linking, and baseline separation of quinidine and quinine could be achieved with good resolution (R(s) = 2.96), selectivity factor (α = 2.16), and column efficiency (N = 2650 plates/m). In contrast, the LC-MIM prepared without crowding agents displayed the smallest diastereoselectivity (α = 1.90), while the crowding-assisted MIM with high level of cross-linker (80%) obtained the greatest selectivity factor (α = 7.65), but the lowest column efficiency (N = 177 plates/m).

Validated RP-HPLC/DAD Method for the Quantification of Insect Repellent Ethyl 2-Aminobenzoate in Membrane-Moderated Matrix Type Monolithic Polymeric Device.

PubMed

Islam, Johirul; Zaman, Kamaruz; Chakrabarti, Srijita; Sharma Bora, Nilutpal; Mandal, Santa; Pratim Pathak, Manash; Srinivas Raju, Pakalapati; Chattopadhyay, Pronobesh

2017-07-01

A simple, accurate and sensitive reversed-phase high-performance liquid chromatographic (RP-HPLC) method has been developed for the estimation of ethyl 2-aminobenzoate (EAB) in a matrix type monolithic polymeric device and validated as per the International Conference on Harmonization guidelines. The analysis was performed isocratically on a ZORBAX Eclipse plus C18 analytical column (250 × 4.4 mm, 5 μm) and a diode array detector (DAD) using acetonitrile and water (75:25 v/v) as the mobile phase by keeping the flow-rate constant at 1.0 mL/min. Determination of EAB was not interfered in the presence of excipients. Inter- and intra-day relative standard deviations were not higher than 2%. Mean recovery was between 98.7 and 101.3%. Calibration curve was linear in the concentration range of 0.5-10 µg/mL. Limits of detection and quantification were 0.19 and 0.60 µg/mL, respectively. Thus, the present report put forward a novel method for the estimation of EAB, an emerging insect repellent, by using RP-HPLC technique. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

The gaseous component of the disk around Beta Pictoris

NASA Technical Reports Server (NTRS)

Hobbs, L. M.; Vidal-Madjar, A.; Ferlet, R.; Albert, C. E.; Gry, C.

1985-01-01

Optical spectra of alpha Lyr, alpha PsA, and beta Pic have been obtained at a velocity resolution of 3 km/s. No circumstellar absorption lines of Ca II or Na I are detected toward alpha Lyr or alpha PsA at sensitive limits. In the favorable case of beta Pic, where the circumstellar disk imaged by Smith and Terrile (1984) is seen nearly edge-on, a strong, narrow, circumstellar Ca II K absorption line previously reported by Slettebak (1982) and weaker, still narrower circumstellar Na I D lines are detected. Negative results of high sensitivity also are obtained for the Ca I 4226 A and CH(+) 4232 A lines, along with upper limits on the Zn II 2026, 2062 A doublet from archival IUE spectra. Under assumptions which agree with other well-established observations of the gaseous abundances of calcium and zinc, the total gaseous column density of hydrogen along a radius of the circumstellar disk is between 10 to the 18th and 4 x 10 to the 20th/sq cm. Within the boundaries of the dust disk detected by Smith and Terrile (1984) the total gaseous mass then is less than about 2, or less than 1 percent of the mass of the planetary system. A simplified model of the density distribution in the gaseous disk yields a characteristic total density n(H) of about 100,000/cu cm, which exceeds that of all interplanetary gas at earth's position by a factor of about 10,000.

Radiation hydrodynamic simulations of line-driven disk winds for ultra-fast outflows

NASA Astrophysics Data System (ADS)

Nomura, Mariko; Ohsuga, Ken; Takahashi, Hiroyuki R.; Wada, Keiichi; Yoshida, Tessei

2016-02-01

Using two-dimensional radiation hydrodynamic simulations, we investigate the origin of the ultra-fast outflows (UFOs) that are often observed in luminous active galactic nuclei (AGNs). We found that the radiation force due to the spectral lines generates strong winds (line-driven disk winds) that are launched from the inner region of accretion disks (˜30 Schwarzschild radii). A wide range of black hole masses (MBH) and Eddington ratios (ε) was investigated to study the conditions causing the line-driven winds. For MBH = 106-109 M⊙ and ε = 0.1-0.7, funnel-shaped disk winds appear, in which dense matter is accelerated outward with an opening angle of 70°-80° and with 10% of the speed of light. If we observe the wind along its direction, the velocity, the column density, and the ionization state are consistent with those of the observed UFOs. As long as obscuration by the torus does not affect the observation of X-ray bands, the UFOs could be statistically observed in about 13%-28% of the luminous AGNs, which is not inconsistent with the observed ratio (˜40%). We also found that the results are insensitive to the X-ray luminosity and the density of the disk surface. Thus, we can conclude that UFOs could exist in any luminous AGNs, such as narrow-line Seyfert 1s and quasars with ε > 0.1, with which fast line-driven winds are associated.

Two-column sequential injection chromatography--new approach for fast and effective analysis and its comparison with gradient elution chromatography.

PubMed

Chocholous, Petr; Satínský, Dalibor; Sklenárová, Hana; Solich, Petr

2010-05-23

This work presents novel approach in low-pressure chromatography flow systems--two-column Sequential Injection Chromatography (2-C SIC) and its comparison with gradient elution chromatography on the same instrument. The system was equipped with two different chromatographic columns (connected to selection valve in parallel design) for isocratic separation and determination of all components in composed anti-inflammatory pharmaceutical preparation (tablets). The sample was first injected on the first column of length 30 mm where less retained analytes were separated and then the sample was injected on the second column of length 10 mm where more retained analytes were separated. The SIC system was based on a commercial SIChrom manifold (8-port high-pressure selection valve and medium-pressure syringe pump with 4 mL reservoir) (FIAlab, USA) with two commercially available monolithic columns the "first column" Chromolith Flash RP-18e (25 mm x 4.6 mm i.d. with guard column 5 mm x 4.6 mm i.d.) and the "second column" Chromolith RP-18e (10 mm x 4.6 mm i.d.) and CCD UV-vis detector USB 4000 with micro-volume 1.0 cm Z flow cell. Two mobile phases were used for analysis (one for each column). The mobile phase 1 used for elution of paracetamol, caffeine and salicylic acid (internal standard) was acetonitrile/water (10:90, v/v, the water part of pH 3.5 adjusted with acetic acid), flow rate was 0.9 mL min(-1) (volume 3.0 mL of mobile phase per analysis). The mobile phase 2 used for elution of propyphenazone was acetonitrile/water (30:70, v/v); flow rate was 1.2 mL min(-1) (volume 1.5 mL of mobile phase per analysis). Absorbance was monitored at 210 nm. Samples were prepared by dissolving of one tablet in 30% acetonitrile and 10 microL of filtered supernatant was injected on each column (2 x 10 microL). The chromatographic resolution between all compounds was >1.45 and analysis time was 5.5 min under the optimal conditions. Limits of detection were determined at 0.4 microg mL(-1) for paracetamol, at 0.5 microg mL(-1) for caffeine and at 0.7 microg mL(-1) for propyphenazone. The new two-column chromatographic set-up developed as an alternative approach to gradient elution chromatography shows evident advantages (time and solvent reduction more than one-third) as compared with single-column gradient SIC method with Chromolith Flash RP-18 (25 mm x 4.6 mm i.d. with guard column 5 mm x 4.6 mm i.d.). Copyright 2010 Elsevier B.V. All rights reserved.

Determination of Zn-citrate in human milk by CIM monolithic chromatography with atomic and mass spectrometry detection.

PubMed

Milačič, Radmila; Ajlec, Dejan; Zuliani, Tea; Žigon, Dušan; Ščančar, Janez

2012-11-15

In human milk zinc (Zn) is bound to proteins and low molecular mass (LMM) ligands. Numerous investigations demonstrated that Zn bioavailability in human milk is for infant much higher than in cow's milk. It was presumed that in the LMM human milk fraction highly bioavailable Zn-citrate prevails. However, literature data are controversial regarding the amount of Zn-citrate in human milk since analytical procedures reported were not quantitative. So, complex investigation was carried out to develop analytical method for quantitative determination of this biologically important molecule. Studies were performed within the pH range 5-7 by the use of synthetic solutions of Zn-citrate prepared in HEPES, MOPS and MES buffers. Zn-citrate was separated on weak anion-exchange convective interaction media (CIM) diethylaminoethyl (DEAE) monolithic chromatographic column using NH(4)NO(3) as an eluent. Separated Zn species were determined by flame atomic absorption spectrometry (FAAS) or inductively coupled plasma mass spectrometry (ICP-MS). Quantitative separation of Zn-citrate complexes ([Zn(Cit)](-) and [Zn(Cit)(2)](4-); column recoveries 94-102%) and good repeatability and reproducibility of results with relative standard deviation (RSD±3.0%) were obtained. In fractions under the chromatographic peaks Zn-binding ligand was identified by electrospray ionization tandem mass spectrometry (ESI-MS-MS). Limits of detection (LOD) for determination of Zn-citrate species by CIM DEAE-FAAS and CIM DEAE-ICP-MS were 0.01 μg Zn mL(-1) and 0.0005 μg Zn mL(-1), respectively. Both techniques were sensitive enough for quantification of Zn-citrate in human milk. Results demonstrated that about 23% of total Zn was present in the LMM milk fraction and that LMM-Zn corresponded to Zn-citrate. The developed speciation method represents a reliable analytical tool for investigation of the percentage and the amount of Zn-citrate in human milk. Copyright © 2012 Elsevier B.V. All rights reserved.

Automated Online Solid-Phase Derivatization for Sensitive Quantification of Endogenous S-Nitrosoglutathione and Rapid Capture of Other Low-Molecular-Mass S-Nitrosothiols.

PubMed

Wang, Xin; Garcia, Carlos T; Gong, Guanyu; Wishnok, John S; Tannenbaum, Steven R

2018-02-06

S-Nitrosothiols (RSNOs) constitute a circulating endogenous reservoir of nitric oxide and have important biological activities. In this study, an online coupling of solid-phase derivatization (SPD) with liquid chromatography-mass spectrometry (LC-MS) was developed and applied in the analysis of low-molecular-mass RSNOs. A derivatizing-reagent-modified polymer monolithic column was prepared and adapted for online SPD-LC-MS. Analytes from the LC autosampler flowed through the monolithic column for derivatization and then directly into the LC-MS for analysis. This integration of the online derivatization, LC separation, and MS detection facilitated system automation, allowing rapid, laborsaving, and sensitive detection of RSNOs. S-Nitrosoglutathione (GSNO) was quantified using this automated online method with good linearity (R 2 = 0.9994); the limit of detection was 0.015 nM. The online SPD-LC-MS method has been used to determine GSNO levels in mouse samples, 138 ± 13.2 nM of endogenous GSNO was detected in mouse plasma. Besides, the GSNO concentrations in liver (64.8 ± 11.3 pmol/mg protein), kidney (47.2 ± 6.1 pmol/mg protein), heart (8.9 ± 1.8 pmol/mg protein), muscle (1.9 ± 0.3 pmol/mg protein), hippocampus (5.3 ± 0.9 pmol/mg protein), striatum (6.7 ± 0.6 pmol/mg protein), cerebellum (31.4 ± 6.5 pmol/mg protein), and cortex (47.9 ± 4.6 pmol/mg protein) were also successfully quantified. When the derivatization was performed within 8 min, followed by LC-MS detection, samples could be rapidly analyzed compared with the offline manual method. Other low-molecular-mass RSNOs, such as S-nitrosocysteine and S-nitrosocysteinylglycine, were captured by rapid precursor-ion scanning, showing that the proposed method is a potentially powerful tool for capture, identification, and quantification of RSNOs in biological samples.

Velocity Data in a Fully Developed Wind Turbine Array Boundary Layer

NASA Astrophysics Data System (ADS)

Turner, John; Wosnik, Martin

2016-11-01

Results are reported from an experimental study of an array of porous disks simulating offshore wind turbines. The disks mimic power extraction of similarly scaled wind turbines via drag matching, and the array consists of 19x5 disks of 0.25 m diameter. The study was conducted in the UNH Flow Physics Facility (FPF), which has test section dimensions of 6.0 m wide, 2.7 m high and 72.0 m long. The FPF can achieve a boundary layer height on the order of 1 m at the entrance of the wind turbine array which puts the model turbines in the bottom third of the boundary layer, which is typical of field application. Careful consideration was given to an expanded uncertainty analysis, to determine possible measurements in this type of flow. For a given configuration (spacing, initial conditions, etc.), the velocity levels out and the wind farm approaches fully developed behavior, even within the maintained growth of the simulated atmospheric boundary layer. Benchmark pitot tube data was acquired in vertical profiles progressing streamwise behind the centered column at every row in the array.

Turbulent AGN tori .

NASA Astrophysics Data System (ADS)

Schartmann, M.; Meisenheimer, K.; Klahr, H.; Camenzind, M.; Wolf, S.; Henning, Th.

Recently, the MID-infrared Interferometric instrument (MIDI) at the VLTI has shown that dust tori in the two nearby Seyfert galaxies NGC 1068 and the Circinus galaxy are geometrically thick and can be well described by a thin, warm central disk, surrounded by a colder and fluffy torus component. By carrying out hydrodynamical simulations with the help of the TRAMP code \\citep{schartmann_Klahr_99}, we follow the evolution of a young nuclear star cluster in terms of discrete mass-loss and energy injection from stellar processes. This naturally leads to a filamentary large scale torus component, where cold gas is able to flow radially inwards. The filaments open out into a dense and very turbulent disk structure. In a post-processing step, we calculate observable quantities like spectral energy distributions or images with the help of the 3D radiative transfer code MC3D \\citep{schartmann_Wolf_03}. Good agreement is found in comparisons with data due to the existence of almost dust-free lines of sight through the large scale component and the large column densities caused by the dense disk.

Hand-Portable Gradient Capillary Liquid Chromatography Pumping System.

PubMed

Sharma, Sonika; Plistil, Alex; Barnett, Hal E; Tolley, H Dennis; Farnsworth, Paul B; Stearns, Stanley D; Lee, Milton L

2015-10-20

In this work, a novel splitless nanoflow gradient generator integrated with a stop-flow injector was developed and evaluated using an on-column UV-absorption detector. The gradient pumping system consisted of two nanoflow pumps controlled by micro stepper motors, a mixer connected to a serpentine tube, and a high-pressure valve. The gradient system weighed only 4 kg (9 lbs) and could generate up to 55 MPa (8000 psi) pressure. The system could operate using a 24 V DC battery and required 1.2 A for operation. The total volume capacity of the pump was 74 μL, and a sample volume of 60 nL could be injected. The system provided accurate nanoflow rates as low as 10 nL/min without employing a splitter, making it ideal for capillary column use. The gradient dwell volume was calculated to be 1.3 μL, which created a delay of approximately 4 min with a typical flow rate of 350 nL/min. Gradient performance was evaluated for gradient step accuracy, and excellent reproducibility was obtained in day-to-day experiments (RSD < 1.2%, n = 4). Linear gradient reproducibility was tested by separating a three-component pesticide mixture on a poly(ethylene glycol) diacrylate (PEGDA) monolithic column. The retention time reproducibility was very good in run-to-run experiments (RSD < 1.42%, n = 4). Finally, excellent separation of five phenols was demonstrated using the nanoflow gradient system.

Chemistry of a newly detected circumbinary disk in Ophiuchus

NASA Astrophysics Data System (ADS)

Artur de la Villarmois, Elizabeth; Kristensen, Lars E.; Jørgensen, Jes K.; Bergin, Edwin A.; Brinch, Christian; Frimann, Søren; Harsono, Daniel; Sakai, Nami; Yamamoto, Satoshi

2018-06-01

Context. Astronomers recently started discovering exoplanets around binary systems. Therefore, understanding the formation and evolution of circumbinary disks and their environment is crucial for a complete scenario of planet formation. Aims: The purpose of this paper is to present the detection of a circumbinary disk around the system Oph-IRS67 and analyse its chemical and physical structure. Methods: We present high-angular-resolution (0.''4, 60 AU) observations of C17O, H13CO+, C34S, SO2, C2H and c-C3H2 molecular transitions with the Atacama Large Millimeter/submillimeter Array (ALMA) at wavelengths of 0.8 mm. The spectrally and spatially resolved maps reveal the kinematics of the circumbinary disk as well as its chemistry. Molecular abundances are estimated using the non-local thermodynamic equilibrium (LTE) radiative-transfer tool RADEX. Results: The continuum emission agrees with the position of Oph-IRS67 A and B, and reveals the presence of a circumbinary disk around the two sources. The circumbinary disk has a diameter of 620 AU and is well traced by C17O and H13CO+ emission. Two further molecular species, C2H and c-C3H2, trace a higher-density region which is spatially offset from the sources ( 430 AU). Finally, SO2 shows compact and broad emission around only one of the sources, Oph-IRS67 B. The molecular transitions which trace the circumbinary disk are consistent with a Keplerian profile on smaller disk scales (≲200 AU) and an infalling profile for larger envelope scales (≳200 AU). The Keplerian fit leads to an enclosed mass of 2.2 M⊙. Inferred CO abundances with respect to H2 are comparable to the canonical ISM value of 2.7 × 10-4, reflecting that freeze-out of CO in the disk midplane is not significant. Conclusions: Molecular emission and kinematic studies prove the existence and first detection of the circumbinary disk associated with the system Oph-IRS67. The high-density region shows a different chemistry than the disk, being enriched in carbon chain molecules. The lack of methanol emission agrees with the scenario where the extended disk dominates the mass budget in the innermost regions of the protostellar envelope, generating a flat density profile where less material is exposed to high temperatures, and thus, complex organic molecules would be associated with lower column densities. Finally, Oph-IRS67 is a promising candidate for proper motion studies and the detection of both circumstellar disks with higher-angular-resolution observations.

Unsteady Plasma Ejections from Hollow Accretion Columns of Galactic Neutron Stars as a Trigger for Gamma-Ray Bursts

NASA Astrophysics Data System (ADS)

Gvaramadze, V. V.

1995-09-01

We propose a model of gamma-ray bursts (GRBs) based on close Galactic neutron stars with accretion disks. We outline a simple mechanism of unsteady plasma ejections during episodic accretion events. The relative kinetic energy of ejected blobs can be converted into gamma-rays by internal shocks. The beaming of gamma-ray emission can be responsible for the observed isotropic angular distribution of GRBs.

Silica particles encapsulated poly(styrene-divinylbenzene) monolithic stationary phases for micro-high performance liquid chromatography.

PubMed

Bakry, R; Stöggl, W M; Hochleitner, E O; Stecher, G; Huck, C W; Bonn, G K

2006-11-03

In the paper we demonstrate a new approach for the preparation and application of continuous silica bed columns that involve encapsulation (entrapment) of functionalized silica microparticles, which can be used as packing material in micro high performance liquid chromatography (micro-HPLC) and capillary electrochromatography (CEC). Like traditional packed columns, these capillaries possess characterized silica particles that offer high phase ratio and narrow pore size distribution leading to high retention and separation efficiency, respectively. More importantly, immobilization of the microparticles stabilizes the separation bed and eliminates the need for retaining frits. The developed capillary columns were fabricated in exactly the same way as a packed capillary column (slurry packing) but with an additional entrapment step. This immobilization of the packed bed was achieved by in situ polymerization of styrene and divinylbenzene in presence of decanol as a porogen and azobisisobutyronitrile as thermal initiator. Silica particles with different particle sizes and pore sizes ranging from 60 to 4000 A were studied. In addition different modified silica was used, including C-18 reversed phase, anion exchange and chiral stationary phases. Efficient separation of polyphenolic compounds, peptides, proteins and even DNA mutation were achieved using the developed technique depending on the properties of the silica particles used (particles pore size). For example, using 3 microm ProntoSIL C-18 particles with 300 A pore size, separation efficiencies in the range of 120,000-200,000 plates/m were obtained for protein separation, in a 6 cm x 200 microm i.d. capillary column. Using encapsulated silica C-18 with 1000 A pore size, separation of DNA homo and hetero duplexes were achieved under denaturing HPLC conditions for mutation detection. In addition, nucleotides were separated using anion exchange material encapsulated with poly(styrene-divinylbenzene) (PS/DVB), which indicated that the chromatographic properties of the silica packing material were still active after polymerization. The prepared capillary columns were found to be stable and could easily be operated continuously up to a pressure of 350 bar without column damage and capillary can be cut to any desired length.

CSI 2264: Characterizing Young Stars in NGC 2264 With Short-Duration Periodic Flux Dips in Their Light Curves

NASA Technical Reports Server (NTRS)

Stauffer, John; Cody, Ann Marie; McGinnis, Pauline; Rebull, Luisa; Hillenbrand, Lynne A.; Turner, Neal J.; Carpenter, John; Plavchan, Peter; Carey, Sean; Terebey, Susan;

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

Zoghbi, Abderahmen; Miller, J. M.; King, A. L.

Disk and wind signatures are seen in the soft state of Galactic black holes, while the jet is seen in the hard state. Here we study the disk–wind connection in the ρ class of variability in GRS 1915+105 using a joint NuSTAR – Chandra observation. The source shows 50 s limit cycle oscillations. By including new information provided by the reflection spectrum and using phase-resolved spectroscopy, we find that the change in the inner disk inferred from the blackbody emission is not matched by reflection measurements. The latter is almost constant, independent of the continuum model. The two radii are comparablemore » only if the disk temperature color correction factor changes, an effect that could be due to the changing opacity of the disk caused by changes in metal abundances. The disk inclination is similar to that inferred from the jet axis, and oscillates by ∼10°. The simultaneous Chandra data show the presence of two wind components with velocities between 500 and 5000 km s{sup −1}, and possibly two more with velocities reaching 20,000 km s{sup −1} (∼0.06 c ). The column densities are ∼5 × 10{sup 22} cm{sup −2}. An upper limit to the wind response time of 2 s is measured, implying a launch radius of <6 × 10{sup 10} cm. The changes in wind velocity and absorbed flux require the geometry of the wind to change during the oscillations, constraining the wind to be launched from a distance of 290–1300 r{sub g} from the black hole. Both data sets support fundamental model predictions in which a bulge originates in the inner disk and moves outward as the instability progresses.« less

Thermal, chemical, and optical properties of Crater Lake, Oregon

USGS Publications Warehouse

Larson, G.L.; Hoffman, R.L.; McIntire, D.C.; Buktenica, M.W.; Girdner, S.F.

2007-01-01

Crater Lake covers the floor of the Mount Mazama caldera that formed 7700 years ago. The lake has a surface area of 53 km2 and a maximum depth of 594 m. There is no outlet stream and surface inflow is limited to small streams and springs. Owing to its great volume and heat, the lake is not covered by snow and ice in winter unlike other lakes in the Cascade Range. The lake is isothermal in winter except for a slight increase in temperature in the deep lake from hyperadiabatic processes and inflow of hydrothermal fluids. During winter and spring the water column mixes to a depth of about 200-250 m from wind energy and convection. Circulation of the deep lake occurs periodically in winter and spring when cold, near-surface waters sink to the lake bottom; a process that results in the upwelling of nutrients, especially nitrate-N, into the upper strata of the lake. Thermal stratification occurs in late summer and fall. The maximum thickness of the epilimnion is about 20 m and the metalimnion extends to a depth of about 100 m. Thus, most of the lake volume is a cold hypolimnion. The year-round near-bottom temperature is about 3.5??C. Overall, hydrothermal fluids define and temporally maintain the basic water quality characteristics of the lake (e.g., pH, alkalinity and conductivity). Total phosphorus and orthophosphate-P concentrations are fairly uniform throughout the water column, where as total Kjeldahl-N and ammonia-N are highest in concentration in the upper lake. Concentrations of nitrate-N increase with depth below 200 m. No long-term changes in water quality have been detected. Secchi disk (20-cm) clarity varied seasonally and annually, but was typically highest in June and lowest in August. During the current study, August Secchi disk clarity readings averaged about 30 m. The maximum individual clarity reading was 41.5 m in June 1997. The lowest reading was 18.1 m in July 1995. From 1896 (white-dinner plate) to 2003, the average August Secchi disk reading was about 30 m. No long-term changes in the Secchi disk clarity were observed. Average turbidity of the water column (2-550 m) between June and September from 1991 to 2000 as measured by a transmissometer ranged between 88.8% and 90.7%. The depth of 1% of the incident solar radiation during thermal stratification varied annually between 80 m and 100 m. Both of these measurements provided additional evidence about the exceptional clarity of Crater Lake. ?? 2007 Springer Science+Business Media B.V.

X-Ray Shadowing Experiments Toward Infrared Dark Clouds

NASA Technical Reports Server (NTRS)

Anderson, L. E.; Snowden, S.; Bania, T. M.

2009-01-01

We searched for X-ray shadowing toward two infrared dark clouds (IRDCs) using the MOS detectors on XMM-Newton to learn about the Galactic distribution of X-ray emitting plasma. IRDCs make ideal X-ray shadowing targets of 3/4 keY photons due to their high column densities, relatively large angular sizes, and known kinematic distances. Here we focus on two clouds near 30 deg Galactic longitude at distances of 2 and 5 kpc from the Sun. We derive the foreground and background column densities of molecular and atomic gas in the direction of the clouds. We find that the 3/4 ke V emission must be distributed throughout the Galactic disk. It is therefore linked to the structure of the cooler material of the ISM, and to the birth of stars.

The theory of QSO absorption line systems and their relationship to the galaxies

NASA Technical Reports Server (NTRS)

Charlton, Jane

1993-01-01

The fundamental goal of this effort is to paint a picture of what the Ly-alpha forest clouds are and how they are distributed in space. Progress during the first phase of this program involved development of the 'Cheshire Cat Model' of Ly-alpha clouds in which systems over a large range of column densities are produced by disks with somewhat smaller column densities than those of normal galaxies. A prediction of the slab model of Ly-alpha clouds was confirmed by a new observational result, and the comparison of models to the new data allowed an estimate of the pressure of the intergalactic medium. This result should be forthcoming in pre-print form within the next month. The various results will now be described in more detail.

Effects of supercritical fluid chromatography conditions on enantioselectivity and performance of polyproline-derived chiral stationary phases.

PubMed

Novell, Arnau; Méndez, Alberto; Minguillón, Cristina

2015-07-17

The chromatographic behaviour and performance of four polyproline-derived chiral stationary phases (CSPs) were tested using supercritical fluid chromatography (SFC). A series of structurally related racemic compounds, whose enantioseparation was proved to be sensitive to the type of mobile phase used in NP-HPLC, were chosen to be tested in the SFC conditions. Good enantioselection ability was shown by the CSPs for the analytes tested in the new conditions. Resolution, efficiency and analysis time, were considerably improved with respect to NP-HPLC when CO2/alcohol mobile phases were used. Monolithic columns clearly show enhanced chromatographic parameters and improved performance respect to their bead-based counterparts. Copyright © 2015 Elsevier B.V. All rights reserved.

Method development for thermal analyses testing on Reillex HPQ resin using the advanced reactive system screening tool (ARSST)

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

Best, D.

Reillex™ HPQ resin was developed by Los Alamos Laboratory and Reilly Industries Inc. in an effort to increase safety and process efficiency during the recovery and purification of plutonium. Ionac™ A-641, another strong base macroporous anion exchange resin used in the nuclear industry, was known to undergo a runaway reaction in hot nitric acid solutions. Because of this, an extensive amount of thermal analyses testing on the Reillex™ HPQ resin in SRNL was performed in 1999-2001 prior to use. A report on the thermal stability qualification of the Reillex™ HPQ resin in 8M (35%) and 12M (53%) HNO 3 wasmore » reported in 2000. In 2001, the reactivity of Reillex™ HPQ resin in 14.4M (64%) HNO 3 was evaluated. In January of 2001, thermal stability scoping tests were performed on irradiated Reillex™ HPQ resin in 14.4M (64%) HNO 3 (as a worst case scenario) and the results sent to Fauske and Associates to calculate a rupture disk size for the HB-Line resin column. A technical report by Fauske and Associates was issued in February 2001 recommending a 2.0” vent line with a rupture disk set pressure of 60 psig. This calculation was based on ARSST thermal analyses scoping tests at SRNL in which 4 grams of dried resin and 6.0 grams of 64% nitric acid in a 10 gram test cell, produced a maximum pressure rate (dP/dt) of 720 psi/min (12 psi/sec) and a maximum temperature of 250 °C. In 2015, a new batch of Reillex™ HPQ resin was manufactured by Vertellus Industries. A test sample of the resin was sent to SRNL to perform acceptance and qualification thermal stability testing using the ARSST. During these tests, method development was performed to ensure that a representative resin to acid ratios were used while running the tests in the ARSST. Fauske and Associates recommended to either use a full test cell representative of the HB-Line column or a 10 gram sample in the test cell that was representative of the ratios of resin to nitric acid in the actual HB-Line column. An observation was made during method development testing that the 4 grams of resin to 6 grams of 64% acid ratio used in 2001 to determine the rupture disk size did not entirely wet the resin and was not representative of the actual HB-Line column. The results of this study raised questions as to whether the ratio of 4 grams of resin to 6 grams of 64% nitric acid recommended by Fauske and Associates in 2001 was the correct ratio.« less

Workshop: The Technical Requirements for Image-Guided Therapy (Focus: Spinal Cord and Spinal Column)

DTIC Science & Technology

2000-02-01

degenerative disease, spondylosis , ligamental ossification, fractures, tumors, and other causes. Compression is a painful condition that may require...series of 7000 patients who underwent lumbar disk surgery, Long indicates three reasons for failed surgery: 1. Failure of the patient to meet the...validated outcomes measures in the lumbar area, is used for a 70-year-old patient with osteoarthritis of the knees and low back pain as well as problems

Time-dependent Models of Magnetospheric Accretion onto Young Stars

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

Robinson, C. E.; Espaillat, C. C.; Owen, J. E.

Accretion onto Classical T Tauri stars is thought to take place through the action of magnetospheric processes, with gas in the inner disk being channeled onto the star’s surface by the stellar magnetic field lines. Young stars are known to accrete material in a time-variable manner, and the source of this variability remains an open problem, particularly on the shortest (∼day) timescales. Using one-dimensional time-dependent numerical simulations that follow the field line geometry, we find that for plausibly realistic young stars, steady-state transonic accretion occurs naturally in the absence of any other source of variability. However, we show that ifmore » the density in the inner disk varies smoothly in time with ∼day-long timescales (e.g., due to turbulence), this complication can lead to the development of shocks in the accretion column. These shocks propagate along the accretion column and ultimately hit the star, leading to rapid, large amplitude changes in the accretion rate. We argue that when these shocks hit the star, the observed time dependence will be a rapid increase in accretion luminosity, followed by a slower decline, and could be an explanation for some of the short-period variability observed in accreting young stars. Our one-dimensional approach bridges previous analytic work to more complicated multi-dimensional simulations and observations.« less

Planetesimal formation by an axisymmetric radial bump of the column density of the gas in a protoplanetary disk

NASA Astrophysics Data System (ADS)

Onishi, Isamu K.; Sekiya, Minoru

2017-04-01

We investigate the effect of a radial pressure bump in a protoplanetary disk on planetesimal formation. We performed the two-dimensional numerical simulation of the dynamical interaction of solid particles and gas with an initially defined pressure bump under the assumption of axisymmetry. The aim of this work is to elucidate the effects of the stellar vertical gravity that were omitted in a previous study. Our results are very different from the previous study, which omitted the vertical gravity. Because dust particles settle toward the midplane because of the vertical gravity to form a thin dust layer, the regions outside of the dust layer are scarcely affected by the back-reaction of the dust. Hence, the gas column density keeps its initial profile with a bump, and dust particles migrate toward the bump. In addition, the turbulence due to the Kelvin-Helmholtz instability caused by the difference of the azimuthal velocities between the inside and outside of the dust layer is suppressed where the radial pressure gradient is reduced by the pressure bump. The dust settling proceeds further where the turbulence is weak, and a number of dust clumps are formed. The dust density in some clumps exceeds the Roche density. Planetesimals are considered to be formed from these clumps owing to the self-gravity.[Figure not available: see fulltext.

The Gaia-ESO Survey and CSI 2264: Substructures, disks, and sequential star formation in the young open cluster NGC 2264

NASA Astrophysics Data System (ADS)

Venuti, L.; Prisinzano, L.; Sacco, G. G.; Flaccomio, E.; Bonito, R.; Damiani, F.; Micela, G.; Guarcello, M. G.; Randich, S.; Stauffer, J. R.; Cody, A. M.; Jeffries, R. D.; Alencar, S. H. P.; Alfaro, E. J.; Lanzafame, A. C.; Pancino, E.; Bayo, A.; Carraro, G.; Costado, M. T.; Frasca, A.; Jofré, P.; Morbidelli, L.; Sousa, S. G.; Zaggia, S.

2018-01-01

Context. Reconstructing the structure and history of young clusters is pivotal to understanding the mechanisms and timescales of early stellar evolution and planet formation. Recent studies suggest that star clusters often exhibit a hierarchical structure, possibly resulting from several star formation episodes occurring sequentially rather than a monolithic cloud collapse. Aims: We aim to explore the structure of the open cluster and star-forming region NGC 2264 ( 3 Myr), which is one of the youngest, richest and most accessible star clusters in the local spiral arm of our Galaxy; we link the spatial distribution of cluster members to other stellar properties such as age and evolutionary stage to probe the star formation history within the region. Methods: We combined spectroscopic data obtained as part of the Gaia-ESO Survey (GES) with multi-wavelength photometric data from the Coordinated Synoptic Investigation of NGC 2264 (CSI 2264) campaign. We examined a sample of 655 cluster members, with masses between 0.2 and 1.8 M⊙ and including both disk-bearing and disk-free young stars. We used Teff estimates from GES and g,r,i photometry from CSI 2264 to derive individual extinction and stellar parameters. Results: We find a significant age spread of 4-5 Myr among cluster members. Disk-bearing objects are statistically associated with younger isochronal ages than disk-free sources. The cluster has a hierarchical structure, with two main blocks along its latitudinal extension. The northern half develops around the O-type binary star S Mon; the southern half, close to the tip of the Cone Nebula, contains the most embedded regions of NGC 2264, populated mainly by objects with disks and ongoing accretion. The median ages of objects at different locations within the cluster, and the spatial distribution of disked and non-disked sources, suggest that star formation began in the north of the cluster, over 5 Myr ago, and was ignited in its southern region a few Myr later. Star formation is likely still ongoing in the most embedded regions of the cluster, while the outer regions host a widespread population of more evolved objects; these may be the result of an earlier star formation episode followed by outward migration on timescales of a few Myr. We find a detectable lag between the typical age of disk-bearing objects and that of accreting objects in the inner regions of NGC 2264: the first tend to be older than the second, but younger than disk-free sources at similar locations within the cluster. This supports earlier findings that the characteristic timescales of disk accretion are shorter than those of disk dispersal, and smaller than the average age of NGC 2264 (i.e., ≲3 Myr). At the same time, we note that disks in the north of the cluster tend to be shorter-lived ( 2.5 Myr) than elsewhere; this may reflect the impact of massive stars within the region (notably S Mon), that trigger rapid disk dispersal. Conclusions: Our results, consistent with earlier studies on NGC 2264 and other young clusters, support the idea of a star formation process that takes place sequentially over a prolonged span in a given region. A complete understanding of the dynamics of formation and evolution of star clusters requires accurate astrometric and kinematic characterization of its population; significant advance in this field is foreseen in the upcoming years thanks to the ongoing Gaia mission, coupled with extensive ground-based surveys like GES. Full Table B.1 is only available at the CDS via anonymous ftp to http://cdsarc.u-strasbg.fr (http://130.79.128.5) or via http://cdsarc.u-strasbg.fr/viz-bin/qcat?J/A+A/609/A10

Fast ionized X-ray absorbers in AGNs

NASA Astrophysics Data System (ADS)

Fukumura, K.; Tombesi, F.; Kazanas, D.; Shrader, C.; Behar, E.; Contopoulos, I.

2016-05-01

We investigate the physics of the X-ray ionized absorbers often identified as warm absorbers (WAs) and ultra-fast outflows (UFOs) in Seyfert AGNs from spectroscopic studies in the context of magnetically-driven accretion-disk wind scenario. Launched and accelerated by the action of a global magnetic field anchored to an underlying accretion disk around a black hole, outflowing plasma is irradiated and ionized by an AGN radiation field characterized by its spectral energy density (SED). By numerically solving the Grad-Shafranov equation in the magnetohydrodynamic (MHD) framework, the physical property of the magnetized disk-wind is determined by a wind parameter set, which is then incorporated into radiative transfer calculations with xstar photoionization code under heating-cooling equilibrium state to compute the absorber's properties such as column density N_H, line-of-sight (LoS) velocity v, ionization parameter ξ, among others. Assuming that the wind density scales as n ∝ r-1, we calculate theoretical absorption measure distribution (AMD) for various ions seen in AGNs as well as line spectra especially for the Fe Kα absorption feature by focusing on a bright quasar PG 1211+143 as a case study and show the model's plausibility. In this note we demonstrate that the proposed MHD-driven disk-wind scenario is not only consistent with the observed X-ray data, but also help better constrain the underlying nature of the AGN environment in a close proximity to a central engine.

Comparative Normal/Failing Rat Myocardium Cell Membrane Chromatographic Analysis System for Screening Specific Components That Counteract Doxorubicin-Induced Heart Failure from Acontium carmichaeli

PubMed Central

2015-01-01

Cell membrane chromatography (CMC) derived from pathological tissues is ideal for screening specific components acting on specific diseases from complex medicines owing to the maximum simulation of in vivo drug-receptor interactions. However, there are no pathological tissue-derived CMC models that have ever been developed, as well as no visualized affinity comparison of potential active components between normal and pathological CMC columns. In this study, a novel comparative normal/failing rat myocardium CMC analysis system based on online column selection and comprehensive two-dimensional (2D) chromatography/monolithic column/time-of-flight mass spectrometry was developed for parallel comparison of the chromatographic behaviors on both normal and pathological CMC columns, as well as rapid screening of the specific therapeutic agents that counteract doxorubicin (DOX)-induced heart failure from Acontium carmichaeli (Fuzi). In total, 16 potential active alkaloid components with similar structures in Fuzi were retained on both normal and failing myocardium CMC models. Most of them had obvious decreases of affinities on failing myocardium CMC compared with normal CMC model except for four components, talatizamine (TALA), 14-acetyl-TALA, hetisine, and 14-benzoylneoline. One compound TALA with the highest affinity was isolated for further in vitro pharmacodynamic validation and target identification to validate the screen results. Voltage-dependent K+ channel was confirmed as a binding target of TALA and 14-acetyl-TALA with high affinities. The online high throughput comparative CMC analysis method is suitable for screening specific active components from herbal medicines by increasing the specificity of screened results and can also be applied to other biological chromatography models. PMID:24731167

CO/H2 Abundance Ratio ≈ 10-4 in a Protoplanetary Disk

NASA Astrophysics Data System (ADS)

France, Kevin; Herczeg, Gregory J.; McJunkin, Matthew; Penton, Steven V.

2014-10-01

The relative abundances of atomic and molecular species in planet-forming disks around young stars provide important constraints on photochemical disk models and provide a baseline for calculating disk masses from measurements of trace species. A knowledge of absolute abundances, those relative to molecular hydrogen (H2), are challenging because of the weak rovibrational transition ladder of H2 and the inability to spatially resolve different emission components within the circumstellar environment. To address both of these issues, we present new contemporaneous measurements of CO and H2 absorption through the "warm molecular layer" of the protoplanetary disk around the Classical T Tauri Star RW Aurigae A. We use a newly commissioned observing mode of the Hubble Space Telescope Cosmic Origins Spectrograph to detect warm H2 absorption in this region for the first time. An analysis of the emission and absorption spectrum of RW Aur shows components from the accretion region near the stellar photosphere, the molecular disk, and several outflow components. The warm H2 and CO absorption lines are consistent with a disk origin. We model the 1092-1117 Å spectrum of RW Aur to derive log10 N(H2) = 19.90+0.33-0.22 cm-2 at T rot(H2) = 440 ± 39 K. The CO A - X bands observed from 1410 to 1520 Å are best fit by log10 N(CO) = 16.1 +0.3-0.5 cm-2 at T rot(CO) = 200+650-125 K. Combining direct measurements of the H I, H2, and CO column densities, we find a molecular fraction in the warm disk surface of f H2 >= 0.47 and derive a molecular abundance ratio of CO/H2 = 1.6+4.7-1.3 × 10-4, both consistent with canonical interstellar dense cloud values. Based on observations made with the NASA/ESA Hubble Space Telescope, obtained from the data archive at the Space Telescope Science Institute. STScI is operated by the Association of Universities for Research in Astronomy, Inc. under NASA contract NAS 5-26555.

Disk Accretion and the Stellar Birthline

NASA Astrophysics Data System (ADS)

Hartmann, Lee; Cassen, Patrick; Kenyon, Scott J.

1997-02-01

We present a simplified analysis of some effects of disk accretion on the early evolution of fully convective, low-mass pre-main-sequence stars. Our analysis builds on the previous seminal work of Stahler, but it differs in that the accretion of material occurs over a small area of the stellar surface, such as through a disk or magnetospheric accretion column, so that most of the stellar photosphere is free to radiate to space. This boundary condition is similar to the limiting case considered by Palla & Stahler for intermediate-mass stars. We argue that for a wide variety of disk mass accretion rates, material will be added to the star with relatively small amounts of thermal energy. Protostellar evolution calculated assuming this ``low-temperature'' limit of accretion generally follows the results of Stahler because of the thermostatic nature of deuterium fusion, which prevents protostars from contracting below a ``birthline'' in the H-R diagram. Our calculated protostellar radii tend to fall below Stahler's at higher masses; the additional energy loss from the stellar photosphere in the case of disk accretion tends to make the protostar contract. The low-temperature disk accretion evolutionary tracks never fall below the deuterium-fusion birthline until the internal deuterium is depleted, but protostellar tracks can lie above the birthline in the H-R diagram if the initial radius of the protostellar core is large enough or if rapid disk accretion (such as might occur during FU Ori outbursts) adds significant amounts of thermal energy to the star. These possibilities cannot be ruled out by either theoretical arguments or observational constraints at present, so that individual protostars might evolve along a multiplicity of birthlines with a modest range of luminosity at a given mass. Our results indicate that there are large uncertainties in assigning ages for the youngest stars from H-R diagram positions, given the uncertainty in birthline positions. Our calculations also suggest that the relatively low disk accretion rates characteristic of T Tauri stars below the birthline cause low-mass stars to contract only slightly faster than normal Hayashi track evolution, so that ages for older pre-main-sequence stars estimated from H-R diagram positions are relatively secure.

Experimental and Observational Studies of Molecular Hydrogen in Interstellar and Circumstellar Environments

NASA Astrophysics Data System (ADS)

Hoadley, Keri

2017-08-01

Understanding the evolution of gas over the lifetime of protoplanetary disks provides us with important clues about how planet formation mechanisms drive the diversity of exoplanetary systems observed to date. In the first part of my thesis, I discuss how I use fluorescent emission observations of molecular hydrogen (H2) in the far-ultraviolet (far-UV) with the Hubble Space Telescope to study the warm molecular regions (a < 10 AU) of planet-forming disks. I have created analytic disk models that produce synthetic H2 line profiles and statistically compare each disk realization with the data. I how the modeled radial distributions of H 2 help provide important constraints on the radiation properties of gas left in the inner disk of protoplanetary disks as they evolve. Additionally, I analyzed the absorption component of these fluorescence features, embedded within the hydrogen Lyman-alpha emission line produced by the accretion of material onto the host protostar. I present column density and temperature estimates for the H2 populations in each disk sightline, and discuss the behavior and possible spatial origins of these hot molecules. As part of my thesis, I address some observational requirements needed to gain further insights into the behavior of the warm, gaseous protoplanetary disk, focusing specifically on a spectrograph concept for the next-generation LUVOIR Surveyor. I discuss a testbed instrument, the Colorado High-resolution Echelle Stellar Spectrograph (CHESS), built as a demonstration of one component of the LUVOIR spectrograph and new technological improvements to UV optical components for the next generation of near- to far-UV astrophysical observatories. CHESS is a far-UV sounding rocket experiment designed to probe the warm and cool atoms and molecules near sites of recent star formation in the local interstellar medium. I present the science goals, design, research and development components, and calibration of the CHESS instrument. I provide results on observations taken during both launches of CHESS, with detailed analysis of the epsilon Per sightline, as inferred from the flight data. I conclude by providing future works and simple estimates of the performance of an instrument like CHESS on LUVOIR to study planet-forming environments.

Durability evaluation of ceramic components using CARES/LIFE

NASA Technical Reports Server (NTRS)

Nemeth, Noel N.; Powers, Lynn M.; Janosik, Lesley A.; Gyekenyesi, John P.

1994-01-01

The computer program CARES/LIFE calculates the time-dependent reliability of monolithic ceramic components subjected to thermomechanical and/or proof test loading. This program is an extension of the CARES (Ceramics Analysis and Reliability Evaluation of Structures) computer program. CARES/LIFE accounts for the phenomenon of subcritical crack growth (SCG) by utilizing the power law, Paris law, or Walker equation. The two-parameter Weibull cumulative distribution function is used to characterize the variation in component strength. The effects of multiaxial stresses are modeled using either the principle of independent action (PIA), the Weibull normal stress averaging method (NSA), or the Batdorf theory. Inert strength and fatigue parameters are estimated from rupture strength data of naturally flawed specimens loaded in static, dynamic, or cyclic fatigue. Application of this design methodology is demonstrated using experimental data from alumina bar and disk flexure specimens which exhibit SCG when exposed to water.

Durability evaluation of ceramic components using CARES/LIFE

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

Nemeth, N.N.; Janosik, L.A.; Gyekenyesi, J.P.

1996-01-01

The computer program CARES/LIFE calculates the time-dependent reliability of monolithic ceramic components subjected to thermomechanical and/or proof test loading. This program is an extension of the CARES (Ceramics Analysis and Reliability Evaluation of Structures) computer program. CARES/LIFE accounts for the phenomenon of subcritical crack growth (SCG) by utilizing the power law, Paris law, or Walker equation. The two-parameter Weibull cumulative distribution function is used to characterize the variation in component strength. The effects of multiaxial stresses are modeled using either the principle of independent action (PIA), the Weibull normal stress averaging method (NSA), or the Batdorf theory. Inert strength andmore » fatigue parameters are estimated from rupture strength data of naturally flawed specimens loaded in static, dynamic, or cyclic fatigue. Application of this design methodology is demonstrated using experimental data from alumina bar and disk flexure specimens, which exhibit SCG when exposed to water.« less

A poly(vinyl alcohol)/sodium alginate blend monolith with nanoscale porous structure

PubMed Central

2013-01-01

A stimuli-responsive poly(vinyl alcohol) (PVA)/sodium alginate (SA) blend monolith with nanoscale porous (mesoporous) structure is successfully fabricated by thermally impacted non-solvent induced phase separation (TINIPS) method. The PVA/SA blend monolith with different SA contents is conveniently fabricated in an aqueous methanol without any templates. The solvent suitable for the fabrication of the present blend monolith by TINIPS is different with that of the PVA monolith. The nanostructural control of the blend monolith is readily achieved by optimizing the fabrication conditions. Brunauer Emmett Teller measurement shows that the obtained blend monolith has a large surface area. Pore size distribution plot for the blend monolith obtained by the non-local density functional theory method reveals the existence of the nanoscale porous structure. Fourier transform infrared analysis reveals the strong interactions between PVA and SA. The pH-responsive property of the blend monolith is investigated on the basis of swelling ratio in different pH solutions. The present blend monolith of biocompatible and biodegradable PVA and SA with nanoscale porous structure has large potential for applications in biomedical and environmental fields. PMID:24093494

A poly(vinyl alcohol)/sodium alginate blend monolith with nanoscale porous structure.

PubMed

Sun, Xiaoxia; Uyama, Hiroshi

2013-10-04

A stimuli-responsive poly(vinyl alcohol) (PVA)/sodium alginate (SA) blend monolith with nanoscale porous (mesoporous) structure is successfully fabricated by thermally impacted non-solvent induced phase separation (TINIPS) method. The PVA/SA blend monolith with different SA contents is conveniently fabricated in an aqueous methanol without any templates. The solvent suitable for the fabrication of the present blend monolith by TINIPS is different with that of the PVA monolith. The nanostructural control of the blend monolith is readily achieved by optimizing the fabrication conditions. Brunauer Emmett Teller measurement shows that the obtained blend monolith has a large surface area. Pore size distribution plot for the blend monolith obtained by the non-local density functional theory method reveals the existence of the nanoscale porous structure. Fourier transform infrared analysis reveals the strong interactions between PVA and SA. The pH-responsive property of the blend monolith is investigated on the basis of swelling ratio in different pH solutions. The present blend monolith of biocompatible and biodegradable PVA and SA with nanoscale porous structure has large potential for applications in biomedical and environmental fields.

Facile fabrication of mesoporous poly(ethylene-co-vinyl alcohol)/chitosan blend monoliths.

PubMed

Wang, Guowei; Xin, Yuanrong; Uyama, Hiroshi

2015-11-05

Poly(ethylene-co-vinyl alcohol) (EVOH)/chitosan blend monoliths were fabricated by thermally-induced phase separation method. Chitosan was successfully incorporated into the polymeric monolith by selecting EVOH as the main component of the monolith. SEM images exhibit that the chitosan was located on the inner surface of the monolith. Fourier-transform infrared analysis and elemental analysis indicate the successful blend of EVOH and chitosan. BET results show that the blend monoliths had high specific surface area and uniform mesopore structure. Good adsorption ability toward various heavy metal ions was found in the blend monoliths due to the large chelation capacity of chitosan. The blend monoliths have potential application for waste water purification or bio-related applications. Copyright © 2015 Elsevier Ltd. All rights reserved.

Surface modified aerogel monoliths

NASA Technical Reports Server (NTRS)

Leventis, Nicholas (Inventor); Johnston, James C. (Inventor); Kuczmarski, Maria A. (Inventor); Meador, Mary Ann B. (Inventor)

2013-01-01

This invention comprises reinforced aerogel monoliths such as silica aerogels having a polymer coating on its outer geometric surface boundary, and to the method of preparing said aerogel monoliths. The polymer coatings on the aerogel monoliths are derived from polymer precursors selected from the group consisting of isocyanates as a precursor, precursors of epoxies, and precursors of polyimides. The coated aerogel monoliths can be modified further by encapsulating the aerogel with the polymer precursor reinforced with fibers such as carbon or glass fibers to obtain mechanically reinforced composite encapsulated aerogel monoliths.

Isolation and recovery of selected polybrominated diphenyl ethers from human serum and sheep serum: coupling reversed-phase solid-phase disk extraction and liquid-liquid extraction techniques with a capillary gas chromatographic electron capture negative ion mass spectrometric determinative technique.

PubMed

Loconto, Paul R; Isenga, David; O'Keefe, Michael; Knottnerus, Mark

2008-01-01

Polybrominated diphenyl ethers (PBDEs) are isolated and recovered with acceptable percent recoveries from human serum via liquid-liquid extraction and column chromatographic cleanup and fractionation with quantitation using capillary gas chromatography-mass spectrometry with electron capture negative ion and selected ion monitoring. PBDEs are found in unspiked serum. An alternative sample preparation approach is developed using sheep serum that utilizes a formic acid pre-treatment followed by reversed-phase solid-phase disk extraction and normal-phase solid-phase cleanup using acidified silica gel that yields>50% recoveries. When these percent recoveries are combined with a minimized phase ratio for human serum and very low instrument detection limits, method detection limits below 500 parts-per-trillion are realized.

Active pixel sensor array with multiresolution readout

NASA Technical Reports Server (NTRS)

Fossum, Eric R. (Inventor); Kemeny, Sabrina E. (Inventor); Pain, Bedabrata (Inventor)

1999-01-01

An imaging device formed as a monolithic complementary metal oxide semiconductor integrated circuit in an industry standard complementary metal oxide semiconductor process, the integrated circuit including a focal plane array of pixel cells, each one of the cells including a photogate overlying the substrate for accumulating photo-generated charge in an underlying portion of the substrate and a charge coupled device section formed on the substrate adjacent the photogate having a sensing node and at least one charge coupled device stage for transferring charge from the underlying portion of the substrate to the sensing node. There is also a readout circuit, part of which can be disposed at the bottom of each column of cells and be common to all the cells in the column. The imaging device can also include an electronic shutter formed on the substrate adjacent the photogate, and/or a storage section to allow for simultaneous integration. In addition, the imaging device can include a multiresolution imaging circuit to provide images of varying resolution. The multiresolution circuit could also be employed in an array where the photosensitive portion of each pixel cell is a photodiode. This latter embodiment could further be modified to facilitate low light imaging.

Determination of volatile compounds in cider apple juices using a covalently bonded ionic liquid coating as the stationary phase in gas chromatography.

PubMed

Pello-Palma, Jairo; González-Álvarez, Jaime; Gutiérrez-Álvarez, María Dolores; Dapena de la Fuente, Enrique; Mangas-Alonso, Juan José; Méndez-Sánchez, Daniel; Gotor-Fernández, Vicente; Arias-Abrodo, Pilar

2017-04-01

A chromatographic method for the separation of volatile compounds in Asturian cider apple juices has been developed. For this separation purpose, a monocationic imidazolium-based ionic liquid bearing a reactive terminal iodine atom was synthesized by a quaternization-anion exchange chemical sequence. Next, the gas chromatography (GC) stationary phase was prepared by covalently linking the imidazolium monolith to the reactive silanol groups of the inner capillary wall at 70 °C. This coated GC column exhibited good thermal stability (290 °C), as well as good efficiency (2000 plates/m) in the separation of volatile compounds from Asturian apple cider juices, and was characterized using the Abraham solvation parameter model. The intra-day and inter-day precision of the chromatographic method was evaluated, obtaining relative standard deviations from 3.7 to 12.9% and from 7.4 to 18.0%, respectively. Furthermore, recoveries from 82.5 to 122% were achieved. Graphical Abstract Covalent bonding of an ionic liquid to inner column wall led to a great improvement of the separation efficiencies of stationary phases in gas chromatography.

Development of molecularly imprinted column-on line-two dimensional liquid chromatography for rapidly and selectively monitoring estradiol in cosmetics.

PubMed

Guo, Pengqi; Xu, Xinya; Xian, Liang; Ge, Yanhui; Luo, Zhimin; Du, Wei; Jing, Wanghui; Zeng, Aiguo; Chang, Chun; Fu, Qiang

2016-12-01

Nowadays, the illegal use of estradiol in cosmetics has caused a series of events which endangering public health seriously. Therefore, it is imperative to establish a simple, fast and specific method for monitoring the illegal use of estradiol in cosmetics. In current study, we developed a molecular imprinted monolithic column two dimensional liquid chromatography method (MIMC-2D-LC) for rapid and selective determination of estradiol in various cosmetic samples. The best polymerization, morphology, structure property, surface groups, and the adsorption performance of the prepared material were investigated. The MIMC-2D-LC was validated and successfully used for detecting estradiol in cosmetic samples with good selectivity, sensitivity, efficiency and reproducibility. The linear range of the MIMC-2D-LC for estradiol was 0.5-50μgg -1 with the limit of detection of 0.08μgg -1 . Finally, six batches of cosmetic samples obtained from local markets were tested by the proposed method. The test results showed that the illegal use of estradiol still existed in the commercially available samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Extinction efficiencies from DDA calculations solved for finite circular cylinders and disks

NASA Technical Reports Server (NTRS)

Withrow, J. R.; Cox, S. K.

1993-01-01

One of the most commonly noted uncertainties with respect to the modeling of cirrus clouds and their effect upon the planetary radiation balance is the disputed validity of the use of Mie scattering results as an approximation to the scattering results of the hexagonal plates and columns found in cirrus clouds. This approximation has historically been a kind of default, a result of the lack of an appropriate analytical solution of Maxwell's equations to particles other than infinite cylinders and spheroids. Recently, however, the use of such approximate techniques as the Discrete Dipole Approximation has made scattering solutions on such particles a computationally intensive but feasible possibility. In this study, the Discrete Dipole Approximation (DDA) developed by Flatau (1992) is used to find such solutions for homogeneous, circular cylinders and disks. This can serve to not only assess the validity of the current radiative transfer schemes which are available for the study of cirrus but also to extend the current approximation of equivalent spheres to an approximation of second order, homogeneous finite circular cylinders and disks. The results will be presented in the form of a single variable, the extinction efficiency.

[Polycystic hydatidosis: casual finding of calcified hydatid cyst simulating mesenteric neoplasm].

PubMed

Moraes, Mário A P; Sobreira, Maria de Nazareth M; Medeiros Filho, Plínio; Tavares, Alexandre Cavalca; Gomes, Maria Iolanda

2003-01-01

A case of abdominal hydatidosis, without hepatic involvement, in a patient from the State of Acre is reported. The hydatid, already in degeneration and partially calcified, was discovered incidentally by a radiologic examination of the vertebral column, carried out for evaluating the state of an intervertebral disk prolapse. Although the images suggested a mesenteric tumor, attached to the intestinal wall, the finding of rostellar hooklets in the dense contents of the cyst, after surgical removal, revealed the parasitic nature of the lesion.

Exploring Disks Around Planets

NASA Astrophysics Data System (ADS)

Kohler, Susanna

2017-07-01

Giant planets are thought to form in circumstellar disks surrounding young stars, but material may also accrete into a smaller disk around the planet. Weve never detected one of these circumplanetary disks before but thanks to new simulations, we now have a better idea of what to look for.Image from previous work simulating a Jupiter-mass planet forming inside a circumstellar disk. The planet has its own circumplanetary disk of accreted material. [Frdric Masset]Elusive DisksIn the formation of giant planets, we think the final phase consists of accretion onto the planet from a disk that surrounds it. This circumplanetary disk is important to understand, since it both regulates the late gas accretion and forms the birthplace of future satellites of the planet.Weve yet to detect a circumplanetary disk thus far, because the resolution needed to spot one has been out of reach. Now, however, were entering an era where the disk and its kinematics may be observable with high-powered telescopes (like the Atacama Large Millimeter Array).To prepare for such observations, we need models that predict the basic characteristics of these disks like the mass, temperature, and kinematic properties. Now a researcher at the ETH Zrich Institute for Astronomy in Switzerland, Judit Szulgyi, has worked toward this goal.Simulating CoolingSzulgyi performs a series of 3D global radiative hydrodynamic simulations of 1, 3, 5, and 10 Jupiter-mass (MJ) giant planets and their surrounding circumplanetary disks, embedded within the larger circumstellar disk around the central star.Density (left column), temperature (center), and normalized angular momentum (right) for a 1 MJ planet over temperatures cooling from 10,000 K (top) to 1,000 K (bottom). At high temperatures, a spherical circumplanetary envelope surrounds the planet, but as the planet cools, the envelope transitions around 64,000 K to a flattened disk. [Szulgyi 2017]This work explores the effects of different planet temperatures and masses on the properties of the disks. Szulgyi specifically examines a range of planetary temperatures between 10,000 K and 1,000 K for the 1 MJ planet. Since the planet cools as it radiates away its formation heat, the different temperatures represent an evolutionary sequence over time.Predicted CharacteristicsSzulgyis work produced a number of intriguing observations, including the following:For the 1 MJ planet, a spherical circumplanetary envelope forms at high temperatures, flattening into a disk as the planet cools. Higher-mass planets form disks even at high temperatures.The disk has a steep temperature profile from inside to outside, and the whole disk is too hot for water to remain frozen. This suggests that satellites couldnt form in the disk earlier than 1 Myr after the planet birth. The outskirts of the disk cool first as the planet cools, indicating that satellites may eventually form in these outer parts and then migrate inward.The planets open gaps in the circumstellar disk as they orbit. As a planet radiates away its formation heat, the gap it opens becomes deeper and wider (though this is a small effect). For high-mass planets (5 MJ), the gap eccentricity increases, which creates a hostile environment for satellite formation.Szulgyi discusses a number of features of these disks that we can plan to search for in the future with our increasing telescope power including signatures in direct imaging and observations of their kinematics. The results from these simulations will help us both to detect these circumplanetary disks and to understand our observations when we do. These future observations will then allow us to learn about late-stage giant-planet formation as well as the formation of their satellites.CitationJ. Szulgyi 2017 ApJ 842 103. doi:10.3847/1538-4357/aa7515

Highly improved operation of monolithic BGO-PET blocks

NASA Astrophysics Data System (ADS)

Gonzalez-Montoro, A.; Sanchez, F.; Majewski, S.; Zanettini, S.; Benlloch, J. M.; Gonzalez, A. J.

2017-11-01

In PET scanners both scintillation crystals and photosensors are key components defining the system's performance and cost. Original PET systems used BGO or NaI(Tl) scintillators but achieved limited performance due to its slow decay and relatively low light output. Moreover, NaI(Tl) has low stopping power for 511 keV annihilation photons. In this study we report the possibility to reintroduce BGO crystals, and in particular in the form of monolithic blocks, especially suitable for low-dose large-size PET scanners, offering significantly improved sensitivity at a highly reduced cost compared to LYSO type fast scintillators. We have studied the performance of a monolithic BGO block as large as 50 × 50 × 15 mm3 with black-painted lateral walls to reduce lights spread, enabling accurate photon depth of interaction (DOI) measurements. A directional optical layer, called retro-reflector, was coupled to the entrance face bouncing back the scintillation light in the direction of the emission source and, therefore, adding to the light signal while preserving the narrow light cone distribution. Four configurations namely 12 × 12 and 16 × 16 SiPM arrays (3 mm × 3 mm each) as photosensors, with or without a nanopattern treatment at the crystal exit face, have been studied. This structure consisted of a thin layer of a specific high refractive index material shaped with a periodic nanopattern, increasing the scintillation light extraction. The readout returned information for each SiPM row and column, characterizing the X-Y light distribution projections. We have studied the detector spatial resolution using collimated 22Na sources at normal incidence. The DOI resolution was evaluated using collimated gamma beams with lateral incidence. The overall best detector performance was obtained for the 16× 16 SiPM array offering higher readout granularity. We have determined the spatial resolution for 3 separated DOI layers, obtaining the best results for the DOI region near to the photosensor.

A Low-metallicity Molecular Cloud in the Lower Galactic Halo

NASA Astrophysics Data System (ADS)

Hernandez, Audra K.; Wakker, Bart P.; Benjamin, Robert A.; French, David; Kerp, Juergen; Lockman, Felix J.; O'Toole, Simon; Winkel, Benjamin

2013-11-01

We find evidence for the impact of infalling, low-metallicity gas on the Galactic disk. This is based on FUV absorption line spectra, 21 cm emission line spectra, and far-infrared (FIR) mapping to estimate the abundance and physical properties of IV21 (IVC135+54-45), a galactic intermediate-velocity molecular cloud that lies ~300 pc above the disk. The metallicity of IV21 was estimated using observations toward the subdwarf B star PG1144+615, located at a projected distance of 16 pc from the cloud's densest core, by measuring ion and H I column densities for comparison with known solar abundances. Despite the cloud's bright FIR emission and large column densities of molecular gas as traced by CO, we find that it has a sub-solar metallicity of log (Z/Z ⊙) = -0.43 ± 0.12 dex. IV21 is thus the first known sub-solar metallicity cloud in the solar neighborhood. In contrast, most intermediate-velocity clouds (IVC) have near-solar metallicities and are believed to originate in the Galactic Fountain. The cloud's low metallicity is also atypical for Galactic molecular clouds, especially in light of the bright FIR emission which suggest a substantial dust content. The measured I 100 μm/N(H I) ratio is a factor of three below the average found in high latitude H I clouds within the solar neighborhood. We argue that IV21 represents the impact of an infalling, low-metallicity high-velocity cloud that is mixing with disk gas in the lower Galactic halo. Based on observations made with the NASA/ESA Hubble Space Telescope, obtained from MAST at the Space Telescope Science Institute, which is operated by the Association of Universities for Research in Astronomy, Inc., under NASA contract NAS 5-26555. These observations are associated with program No. 12275. The Green Bank Telescope is part of the National Radio Astronomy Observatory which is a Facility of the National Science Foundation, operated by Associated Universities, Inc.

The evidence for clumpy accretion in the Herbig Ae star HR 5999

NASA Technical Reports Server (NTRS)

Perez, M. R.; Grady, C. A.; The, P. S.

1993-01-01

Analysis of IUE high- and low-dispersion spectra of the young Herbig Ae star HR 5999 (HD 144668) covering 1978-1992 revealed dramatic changes in the Mg II h and k (2795.5, 2802.7 A) emission profiles, changes in the column density and distribution in radial velocity of accreting gas, and flux in the Ly(alpha), O I, and C IV emission lines, which are correlated with the UV excess luminosity. Variability in the spectral type inferred from the UV spectral energy distribution, ranging from A5 IV-III in high state to A7 III in the low state, was also observed. The trend of earlier inferred spectral type with decreasing wavelength and with increasing UV continuum flux has previously been noted as a signature of accretion disks in lower mass pre-main sequence stars (PMS) and in systems undergoing FU Orionis-type outbursts. Our data represent the first detection of similar phenomena in an intermediate mass (M greater than or equal to 2 solar mass) PMS star. Recent IUE spectra show gas accreting toward the star with velocities as high as plus 300 km/s, much as is seen toward beta Pic, and suggest that we also view this system through the debris disk. The absence of UV lines with the rotational broadening expected given the optical data (A7 IV, V sini=180 plus or minus 20 km/s for this system) also suggests that most of the UV light originates in the disk, even in the low continuum state. The dramatic variability in the column density of accreting gas, is consistent with clumpy accretion, such as has been observed toward beta Pic, is a hallmark of accretion onto young stars, and is not restricted to the clearing phase, since detectable amounts of accretion are present for stars with 0.5 Myr less than t(sub age) less than 2.8 Myr. The implications for models of beta Pic and similar systems are briefly discussed.

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

Rana, Vikram; Harrison, Fiona A.; Walton, Dominic J.

We present results for two ultraluminous X-ray sources (ULXs), IC 342 X-1 and IC 342 X-2, using two epochs of XMM-Newton and NuSTAR observations separated by ∼7 days. We observe little spectral or flux variability above 1 keV between epochs, with unabsorbed 0.3-30 keV luminosities being 1.04{sub −0.06}{sup +0.08}×10{sup 40} erg s{sup –1} for IC 342 X-1 and 7.40 ± 0.20 × 10{sup 39} erg s{sup –1} for IC 342 X-2, so that both were observed in a similar, luminous state. Both sources have a high absorbing column in excess of the Galactic value. Neither source has a spectrum consistent with a black hole binary in low/hard state, and both ULXsmore » exhibit strong curvature in their broadband X-ray spectra. This curvature rules out models that invoke a simple reflection-dominated spectrum with a broadened iron line and no cutoff in the illuminating power-law continuum. X-ray spectrum of IC 342 X-1 can be characterized by a soft disk-like blackbody component at low energies and a cool, optically thick Comptonization continuum at high energies, but unique physical interpretation of the spectral components remains challenging. The broadband spectrum of IC 342 X-2 can be fit by either a hot (3.8 keV) accretion disk or a Comptonized continuum with no indication of a seed photon population. Although the seed photon component may be masked by soft excess emission unlikely to be associated with the binary system, combined with the high absorption column, it is more plausible that the broadband X-ray emission arises from a simple thin blackbody disk component. Secure identification of the origin of the spectral components in these sources will likely require broadband spectral variability studies.« less

Herschel survey and modelling of externally-illuminated photoevaporating protoplanetary disks

NASA Astrophysics Data System (ADS)

Champion, J.; Berné, O.; Vicente, S.; Kamp, I.; Le Petit, F.; Gusdorf, A.; Joblin, C.; Goicoechea, J. R.

2017-08-01

Context. Protoplanetary disks undergo substantial mass-loss by photoevaporation, a mechanism that is crucial to their dynamical evolution. However, the processes regulating the gas energetics have not so far been well constrained by observations. Aims: We aim to study the processes involved in disk photoevaporation when it is driven by far-UV photons (I.e. 6 < E < 13.6 eV). Methods: We present a unique Herschel survey and new ALMA observations of four externally-illuminated photoevaporating disks (a.k.a. proplyds). To analyse these data, we developed a 1D model of the photodissociation region (PDR) of a proplyd, based on the Meudon PDR code. Using this model, we computed the far infrared line emission. Results: With this model, we successfully reproduce most of the observations and derive key physical parameters, that is, the densities at the disk surface of about 106 cm-3 and local gas temperatures of about 1000 K. Our modelling suggests that all studied disks are found in a transitional regime resulting from the interplay between several heating and cooling processes that we identify. These differ from those dominating in classical PDRs, meaning the grain photo-electric effect and cooling by [OI] and [CII] FIR lines. This specific energetic regime is associated to an equilibrium dynamical point of the photoevaporation flow: the mass-loss rate is self-regulated to keep the envelope column density at a value that maintains the temperature at the disk surface around 1000 K. From the physical parameters derived from our best-fit models, we estimate mass-loss rates - of the order of 10-7M⊙/yr - that are in agreement with earlier spectroscopic observation of ionised gas tracers. This holds only if we assume photoevaporation in the supercritical regime where the evaporation flow is launched from the disk surface at sound speed. Conclusions: We have identified the energetic regime regulating FUV-photoevaporation in proplyds. This regime could be implemented into models of the dynamical evolution of protoplanetary disks. Herschel is an ESA space observatory with science instruments provided by European-led Principal Investigator consortia and with important participation from NASA.Tables of observational data are only available at the CDS via anonymous ftp to http://cdsarc.u-strasbg.fr (http://130.79.128.5) or via http://cdsarc.u-strasbg.fr/viz-bin/qcat?J/A+A/604/A69

Microfluidic devices and methods including porous polymer monoliths

DOEpatents

Hatch, Anson V; Sommer, Gregory J; Singh, Anup K; Wang, Ying-Chih; Abhyankar, Vinay V

2014-04-22

Microfluidic devices and methods including porous polymer monoliths are described. Polymerization techniques may be used to generate porous polymer monoliths having pores defined by a liquid component of a fluid mixture. The fluid mixture may contain iniferters and the resulting porous polymer monolith may include surfaces terminated with iniferter species. Capture molecules may then be grafted to the monolith pores.

Microfluidic devices and methods including porous polymer monoliths

DOEpatents

Hatch, Anson V.; Sommer, Gregory j.; Singh, Anup K.; Wang, Ying-Chih; Abhyankar, Vinay

2015-12-01

Microfluidic devices and methods including porous polymer monoliths are described. Polymerization techniques may be used to generate porous polymer monoliths having pores defined by a liquid component of a fluid mixture. The fluid mixture may contain iniferters and the resulting porous polymer monolith may include surfaces terminated with iniferter species. Capture molecules may then be grafted to the monolith pores.

Preparation of novel beta-cyclodextrin functionalized monolith and its application in chiral separation.

PubMed

Lv, Yongqin; Mei, Danping; Pan, Xinxin; Tan, Tianwei

2010-09-15

A novel beta-cyclodextrin (beta-CD) functionalized organic polymer monolith was prepared by covalently bonding ethylenediamine-beta-CD (EDA-beta-CD) to poly(glycidyl methacrylate-co-ethylene glycol dimethacrylate) (poly(GMA-co-EGDMA)) monolith via ring opening reaction of epoxy groups. SEM characterization was performed to confirm the homogeneity of the monolithic polymer. The resulting monolith was then characterized by DSC and XPS elemental analysis to study the thermal stability of the monolith, and to prove the successful immobilization of beta-CD on the polymer substrate. The beta-CD ligand density of 0.68 mmol g(-1) was obtained for the modified monolith, indicating the high reactivity and efficiency of the EDA-beta-CD modifier. The ethylenediamine-beta-CD functionalized monoliths were used for the chiral separation of ibuprofen racemic mixture and showed promising results. Copyright (c) 2010 Elsevier B.V. All rights reserved.

Mechanically stable, hierarchically porous Cu3(btc)2 (HKUST-1) monoliths via direct conversion of copper(II) hydroxide-based monoliths.

PubMed

Moitra, Nirmalya; Fukumoto, Shotaro; Reboul, Julien; Sumida, Kenji; Zhu, Yang; Nakanishi, Kazuki; Furukawa, Shuhei; Kitagawa, Susumu; Kanamori, Kazuyoshi

2015-02-28

The synthesis of highly crystalline macro-meso-microporous monolithic Cu3(btc)2 (HKUST-1; btc(3-) = benzene-1,3,5-tricarboxylate) is demonstrated by direct conversion of Cu(OH)2-based monoliths while preserving the characteristic macroporous structure. The high mechanical strength of the monoliths is promising for possible applications to continuous flow reactors.

Designing Catalytic Monoliths For Closed-Cycle CO2 Lasers

NASA Technical Reports Server (NTRS)

Guinn, Keith; Herz, Richard K.; Goldblum, Seth; Noskowski, ED

1992-01-01

LASCAT (Design of Catalytic Monoliths for Closed-Cycle Carbon Dioxide Lasers) computer program aids in design of catalyst in monolith by simulating effects of design decisions on performance of laser. Provides opportunity for designer to explore tradeoffs among activity and dimensions of catalyst, dimensions of monolith, pressure drop caused by flow of gas through monolith, conversion of oxygen, and other variables. Written in FORTRAN 77.

Steam reforming of n-hexane on pellet and monolithic catalyst beds. A comparative study on improvements due to heat transfer

NASA Technical Reports Server (NTRS)

1981-01-01

Monolithic catalysts with higher available active surface areas and better thermal conductivity than conventional pellets beds, making possible the steam reforming of fuels heavier than naphtha, were examined. Performance comparisons were made between conventional pellet beds and honeycomb monolith catalysts using n-hexane as the fuel. Metal-supported monoliths were examined. These offer higher structural stability and higher thermal conductivity than ceramic supports. Data from two metal monoliths of different nickel catalyst loadings were compared to pellets under the same operating conditions. Improved heat transfer and better conversion efficiencies were obtained with the monolith having higher catalyst loading. Surface-gas interaction was observed throughout the length of the monoliths.

Revisiting resolution in hydrodynamic countercurrent chromatography: tubing bore effect.

PubMed

Berthod, A; Faure, K

2015-04-17

A major challenge in countercurrent chromatography (CCC), the technique that works with a support-free biphasic liquid system, is to retain the liquid stationary phase inside the CCC column (Sf parameter). Two solutions are commercially available: the hydrostatic CCC columns, also called centrifugal partition chromatographs (CPC), with disks of interconnected channels and rotary seals, and the hydrodynamic CCC columns with bobbins of coiled open tube and no rotary seals. It was demonstrated that the amount of liquid stationary phase retained by a coiled tube was higher with larger bore tubing than with small bore tubes. At constant column volume, small bore tubing will be longer producing more efficiency than larger bore tube that will better retain the liquid stationary phase. Since the resolution equation in CCC is depending on both column efficiency and stationary phase retention ratio, the influence of the tubing bore should be studied. This theoretical work showed that there is an optimum tubing bore size depending on solute partition coefficient and mobile phase flow rate. The interesting result of the theoretical study is that larger tubing bores allow for dramatically reduced experiment durations for all solutes: in reversed phase CCC (polar mobile phase), hydrophobic solutes are usually highly retained. These apolar solutes can be separated by the same coil at high flow rates and reduced Sf with similar retention times as polar solutes separated at smaller flow rates and much higher Sf. Copyright © 2015 Elsevier B.V. All rights reserved.

Chandra/ACIS-I Study of the X-Ray Properties of the NGC 6611 and M16 Stellar Populations

NASA Astrophysics Data System (ADS)

Guarcello, M. G.; Caramazza, M.; Micela, G.; Sciortino, S.; Drake, J. J.; Prisinzano, L.

2012-07-01

Mechanisms regulating the origin of X-rays in young stellar objects and the correlation with their evolutionary stage are under debate. Studies of the X-ray properties in young clusters allow us to understand these mechanisms. One ideal target for this analysis is the Eagle Nebula (M16), with its central cluster NGC 6611. At 1750 pc from the Sun, it harbors 93 OB stars, together with a population of low-mass stars from embedded protostars to disk-less Class III objects, with age <=3 Myr. We study an archival 78 ks Chandra/ACIS-I observation of NGC 6611 and two new 80 ks observations of the outer region of M16, one centered on the Column V and the other on a region of the molecular cloud with ongoing star formation. We detect 1755 point sources with 1183 candidate cluster members (219 disk-bearing and 964 disk-less). We study the global X-ray properties of M16 and compare them with those of the Orion Nebula Cluster. We also compare the level of X-ray emission of Class II and Class III stars and analyze the X-ray spectral properties of OB stars. Our study supports the lower level of X-ray activity for the disk-bearing stars with respect to the disk-less members. The X-ray luminosity function (XLF) of M16 is similar to that of Orion, supporting the universality of the XLF in young clusters. Eighty-five percent of the O stars of NGC 6611 have been detected in X-rays. With only one possible exception, they show soft spectra with no hard components, indicating that mechanisms for the production of hard X-ray emission in O stars are not operating in NGC 6611.

ALMA Resolves the Nuclear Disks of Arp 220

NASA Astrophysics Data System (ADS)

Scoville, Nick; Murchikova, Lena; Walter, Fabian; Vlahakis, Catherine; Koda, Jin; Vanden Bout, Paul; Barnes, Joshua; Hernquist, Lars; Sheth, Kartik; Yun, Min; Sanders, David; Armus, Lee; Cox, Pierre; Thompson, Todd; Robertson, Brant; Zschaechner, Laura; Tacconi, Linda; Torrey, Paul; Hayward, Christopher C.; Genzel, Reinhard; Hopkins, Phil; van der Werf, Paul; Decarli, Roberto

2017-02-01

We present 90 mas (37 pc) resolution ALMA imaging of Arp 220 in the CO (1-0) line and continuum at λ =2.6 {mm}. The internal gas distribution and kinematics of both galactic nuclei are well resolved for the first time. In the west nucleus, the major gas and dust emission extends out to 0.″2 radius (74 pc); the central resolution element shows a strong peak in the dust emission but a factor of 3 dip in the CO line emission. In this nucleus, the dust is apparently optically thick ({τ }2.6{mm}˜ 1) at λ =2.6 {mm} with a dust brightness temperature of ˜147 K. The column of interstellar matter at this nucleus is {N}{{H}2}≥slant 2× {10}26 cm-2, corresponding to ˜900 gr cm-2. The east nucleus is more elongated with radial extent 0.″3 or ˜111 pc. The derived kinematics of the nuclear disks provide a good fit to the line profiles, yielding the emissivity distributions, the rotation curves, and velocity dispersions. In the west nucleus, there is evidence of a central Keplerian component requiring a central mass of 8 × 108 {M}⊙ . The intrinsic widths of the emission lines are {{Δ }}v({FWHM})=250 (west) and 120 (east) km s-1. Given the very short dissipation timescales for turbulence (≲105 years), we suggest that the line widths may be due to semicoherent motions within the nuclear disks. The symmetry of the nuclear disk structures is impressive, implying the merger timescale is significantly longer than the rotation period of the disks.

Carbon-Based Honeycomb Monoliths for Environmental Gas-Phase Applications

PubMed Central

Moreno-Castilla, Carlos; Pérez-Cadenas, Agustín F.

2010-01-01

Honeycomb monoliths consist of a large number of parallel channels that provide high contact efficiencies between the monolith and gas flow streams. These structures are used as adsorbents or supports for catalysts when large gas volumes are treated, because they offer very low pressure drop, short diffusion lengths and no obstruction by particulate matter. Carbon-based honeycomb monoliths can be integral or carbon-coated ceramic monoliths, and they take advantage of the versatility of the surface area, pore texture and surface chemistry of carbon materials. Here, we review the preparation methods of these monoliths, their characteristics and environmental applications.

A search for ultraviolet circumstellar gas absorption features in alpha Piscis Austrinus (Fomalhaut), a possible Beta Pictoris-like system

NASA Technical Reports Server (NTRS)

Cheng, K.-P.; Bruhweiler, Fred C.; Kondo, Yoji

1994-01-01

Archival high-dispersion International Ultraviolet Explorer (IUE) spectra have been used to search for circumstellar gas absorption features in alpha PsA (A3 V), a nearby (6.7 pc) proto-planetary system candidate. Recent sub-millimeter mapping observations around the region of alpha PsA indicate a spatially resolved dust disk like the one seen around Beta Pic. To determine how closely this putative disk resembles that of Beta Pic, we have searched for signatures of circumstellar gaseous absorption in all the available IUE high-dispersion data of alpha PsA. Examination of co-added IUE spectra shows weak circumstellar absorptions from excited levels in the resonance multiplet of Fe II near 2600 A. We also conclude that the sharp C I feature near 1657 A, previously identified as interstellar absorption toward alpha PsA, likely has a circumstellar origin. However, because the weakness of these absorption features, we will consider the presence of circumstellar gas as tentative and should be verified by using the Goddard High-Resolution Spectrograph aboard the Hubble Space Telescope. No corresponding circumstellar absorption is detected in higher ionization Fe III and Al III. Since the collisionally ionized nonphotospheric Al III resonance absorption seen in Beta Pic is likely formed close to the stellar surface, its absence in the UV spectra of alpha PsA could imply that, in contrast with Beta Pic, there is no active gaseous disk infall onto the central star. In the alpha PsA gaseous disk, if we assume a solar abundance for iron and all the iron is in the form of Fe II, plus a disk temperature of 5000 K, the Fe II UV1 absorption at 2611.8743 A infers a total hydrogen column density along the line of sight through the circumstellar disk of N(H) approximately equals 3.8 x 10(exp 17)/cm.

Suzaku observations of spectral variations of the ultra-luminous X-ray source Holmberg IX X-1

NASA Astrophysics Data System (ADS)

Kobayashi, Shogo B.; Nakazawa, Kazuhiro; Makishima, Kazuo

2017-02-01

Observations of the ultra-luminous X-ray source (ULX) Holmberg IX X-1 were carried out with Suzaku twice, once on 2012 April 13 and then on 2012 October 24, with exposures of 180 ks and 217 ks, respectively. The source showed a hard power-law shaped spectrum with a mild cutoff at ˜8 keV, which is typical of ULXs when they are relatively dim. On both occasions, the 0.6-11 keV spectrum was explained successfully in terms of a cool (˜0.2 keV) multi-color disk blackbody emission model and thermal Comptonization emission produced by an electron cloud with a relatively low temperature and high optical depth, assuming that a large fraction of the disk-blackbody photons are Comptonized whereas the rest are observed directly. The 0.5-10 keV luminosity was 1.2 × 1040 erg s-1 in April, and ˜14% higher in October. This brightening was accompanied by spectral softening in ≥2 keV, with little change in the ≤2 keV spectral shape. This behavior can be understood if the accretion disk remains unchanged while the electron cloud covers a variable fraction of the disk. The absorbing column density was consistent with the galactic line-of sight value, and did not vary by more than 1.6 × 1021 cm-2. Together with the featureless spectra, these properties may not be reconciled easily with the super-critical accretion scenario of this source.

Fast Ionized X-Ray Absorbers in AGNs

NASA Technical Reports Server (NTRS)

Fukumura, K.; Tombesi, F.; Kazanas, D.; Shrader, C.; Behar, E.; Contopoulos, I.

2016-01-01

We investigate the physics of the X-ray ionized absorbers often identified as warm absorbers (WAs) and ultra-fast outflows (UFOs) in Seyfert AGNs from spectroscopic studies in the context of magnetically-driven accretion-disk wind scenario. Launched and accelerated by the action of a global magnetic field anchored to an underlying accretion disk around a black hole, outflowing plasma is irradiated and ionized by an AGN radiation field characterized by its spectral energy density (SED). By numerically solving the Grad-Shafranov equation in the magnetohydrodynamic (MHD) framework, the physical property of the magnetized disk-wind is determined by a wind parameter set, which is then incorporated into radiative transfer calculations with xstar photoionization code under heating-cooling equilibrium state to compute the absorber's properties such as column density N(sub H), line-of-sight (LoS) velocity v, ionization parameter xi, among others. Assuming that the wind density scales as n varies as r(exp. -1), we calculate theoretical absorption measure distribution (AMD) for various ions seen in AGNs as well as line spectra especially for the Fe K alpha absorption feature by focusing on a bright quasar PG 1211+143 as a case study and show the model's plausibility. In this note we demonstrate that the proposed MHD-driven disk-wind scenario is not only consistent with the observed X-ray data, but also help better constrain the underlying nature of the AGN environment in a close proximity to a central engine.

THE FATE OF PLANETESIMALS IN TURBULENT DISKS WITH DEAD ZONES. I. THE TURBULENT STIRRING RECIPE

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

Okuzumi, Satoshi; Ormel, Chris W., E-mail: okuzumi@geo.titech.ac.jp

2013-07-01

Turbulence in protoplanetary disks affects planet formation in many ways. While small dust particles are mainly affected by the aerodynamical coupling with turbulent gas velocity fields, planetesimals and larger bodies are more affected by gravitational interaction with gas density fluctuations. For the latter process, a number of numerical simulations have been performed in recent years, but a fully parameter-independent understanding has not been yet established. In this study, we present simple scaling relations for the planetesimal stirring rate in turbulence driven by magnetorotational instability (MRI), taking into account the stabilization of MRI due to ohmic resistivity. We begin with order-of-magnitudemore » estimates of the turbulence-induced gravitational force acting on solid bodies and associated diffusion coefficients for their orbital elements. We then test the predicted scaling relations using the results of recent ohmic-resistive MHD simulations by Gressel et al. We find that these relations successfully explain the simulation results if we properly fix order-of-unity uncertainties within the estimates. We also update the saturation predictor for the density fluctuation amplitude in MRI-driven turbulence originally proposed by Okuzumi and Hirose. Combination of the scaling relations and saturation predictor allows us to know how the turbulent stirring rate of planetesimals depends on disk parameters such as the gas column density, distance from the central star, vertical resistivity distribution, and net vertical magnetic flux. In Paper II, we apply our recipe to planetesimal accretion to discuss its viability in turbulent disks.« less

Dense clumps of ionized gas near Pi Scorpii, as revealed by the fine-structure excitation of N II

NASA Technical Reports Server (NTRS)

Bertoldi, Frank; Jenkins, Edward B.

1992-01-01

The column density and the emission of the ionized gas along the line of sight toward the B1 V + B2 V binary star Pi Sco are measured on the basis of the fine-structure absorption lines of the ground state N II. It is found that the bulk of this ionized gas must be clumped on a length scale of 0.025 pc, which is far smaller than the observed size of the diffuse H II region surrounding Pi Sco of about 6 pc. The observed column density of S III toward Pi Sco yields an upper limit on the distance of the absorbing, clumped gas from the star of less than about 0.02 pc, assuming that both the N II and S III absorption arise from the same gas. The possibility that the ionized gas originates from a photoevaporating circumstellar disk directly surrounding Pi Sco is excluded, since such a disk would have an unusual size of order 0.025 pc and would have had to survive for the estimated age of Pi Sco of 5-8 Myr. The derived mean density of the clumped gas is of order 40/cu cm, so that the gas is at a pressure that far exceeds the mean pressure in the H II region. It is concluded that the ionized gas could originate from evaporation flows off a cluster of compact neutral objects that evaporate due to the ionizing radiation of Pi Sco.

On-Line 1D and 2D PLOT/LC-ESI-MS Using 10 μm i.d. Poly(styrene–divinylbenzene) Porous Layer Open Tubular (PLOT) Columns For Ultrasensitive Proteomic Analysis

PubMed Central

Luo, Quanzhou; Yue, Guihua; Valaskovic, Gary A; Gu, Ye; Wu, Shiaw-Lin; Karger, Barry L.

2008-01-01

Following on our recent work, on-line one dimensional (1D) and two dimensional (2D) PLOT/LC-ESI-MS platforms using 3.2 m × 10 μm i.d. poly(styrenedivinylbenzene) (PS-DVB) porous layer open tubular (PLOT) columns have been developed to provide robust, high performance and ultrasensitive proteomic analysis. Using a PicoClear tee, the dead volume connection between a 50 μm i.d. PS-DVB monolithic microSPE column and the PLOT column was minimized. The microSPE/PLOT column assembly provided a separation performance similar to that obtained with direct injection onto the PLOT column at a mobile phase flow rate of 20 nL/min. The trace analysis potential of the platform was evaluated using an in-gel tryptic digest sample of a gel fraction (15 to 40 kDa) of a cervical cancer (SiHa) cell line. As an example of the sensitivity of the system, ∼2.5 ng of protein in 2 μL solution, an amount corresponding to 20 SiHa cells, was subjected to on-line microSPE-PLOT/LC-ESIMS/MS analysis using a linear ion trap MS. 237 peptides associated with 163 unique proteins were identified from a single analysis when using stringent criteria associated with a false positive rate less than 1% . The number of identified peptides and proteins increased to 638 and 343, respectively, as the injection amount was raised to ∼45 ng of protein, an amount corresponding to 350 SiHa cells. In comparison, only 338 peptides and 231 unique proteins were identified (false positive rate again less than 1%) from 750 ng of protein from the identical gel fraction, an amount corresponding to 6000 SiHa cells, using a typical 15 cm × 75 μm i.d. packed capillary column. The greater sensitivity, higher recovery, and higher resolving power of the PLOT column resulted in the increased number of identifications from only ∼5% of the injected sample amount. The resolving power of the microSPE/PLOT assembly was further extended by 2D chromatography via combination of the high-efficiency reversed phase PLOT column with strong cation exchange chromatography (SCX). As an example, 1071 peptides associated with 536 unique proteins were identified from 75 ng of protein from the same gel fraction, an amount corresponding to 600 cells, using 5 ion exchange fractions in online 2D SCX-PLOT/LC-MS. The 2D system, implemented in an automated format, led to simple and robust operation for proteomic analysis. These promising results demonstrate the potential of the PLOT column for ultratrace analysis. PMID:17625912

Void Formation/Elimination and Viscoelastic Response of Polyphenylsilsesquioxane Monolith.

PubMed

Daiko, Yusuke; Oda, Yuki; Honda, Sawao; Iwamoto, Yuji

2018-05-19

Polyphenylsilsesquioxane (PhSiO 3/2 ) particles as an organic-inorganic hybrid were prepared using sol-gel method, and monolithic samples were obtained via a warm-pressing. The reaction mechanism of particles' polymerization and transformation to the monolith under the warm-press were investigated using solid state 29 Si nuclear magnetic resonance (NMR) spectrometer, thermal gravimetric-differential thermal analyzer (TG-DTA), mass spectrometer (MS) and scanning electron microscope (SEM). Transparent and void-free monoliths are successfully obtained by warm-pressing above 180 °C. Both the terminal ⁻OH groups on particles' surface and warm-pressing are necessary for preparation of void-free PhSiO 3/2 monolith. From the load-displacement measurement at various temperatures, a viscoelastic deformation is seen for PhSiO 3/2 monolith with voids. On the other hand, an elastic deformation is seen for void-free PhSiO 3/2 monolith, and the void-free monolith shows much higher breakdown voltage.

Description and properties of a resistive network applied to emission tomography detector readouts

NASA Astrophysics Data System (ADS)

Boisson, F.; Bekaert, V.; Sahr, J.; Brasse, D.

2017-11-01

Over the last twenty years, PET systems have used discrete crystal detector modules coupled to multi-channel photodetectors, mostly to improve the spatial resolution. Although reading each readout channels individually would be of great interest, costs associated with the electronics would, in most cases, be too expensive. It is therefore essential to propose lower-cost solutions that do not degrade the overall system's performance. One possible solution to reduce the development costs of a PET system without degrading performance is the use of a resistive network which reduces the total number of readout channels. In this study, we present a symmetric charge division resistive network and associated software methods to assess the performance of a PET detector. Our approach consists in keeping the n lines and n columns information provided by a symmetric charge division circuit (SCD). We provided equations relative to output currents of the network, which enable estimation of the charge. We propose a novel approach to reconstruct the charge distribution from the lines and columns projection using a maximum likelihood expectation maximization (MLEM) approach which takes the non-uniformity of the photodetector channel gains into account. We also introduce a mathematical proof of the relation between the sigma of the reconstructed charge distribution and the Ratio between the line of interest (maximum value) and the background signal charges. To the best of our knowledge, this is the first study reporting these equations. Preliminary results obtained with a resistive network used in readout of a monolithic 50 × 50 × 8mm3 LYSO crystal coupled to a H9500 PMT validated the effectiveness of the reconstructed charge distribution to optimize both the x and y spatial resolution and the energy resolution. We obtained a mean x and y spatial resolution of 1.10 mm FWHM and a 14.7% energy resolution by calculating the integral of the reconstructed charge distribution. Finally, the relation between the ratio and the sigma of the reconstructed charge distribution may provide new opportunities in terms of Depth-of-Interaction estimation when using a monolithic crystal coupled to a multi-channel photodetector.

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

Rigliaco, Elisabetta; Pascucci, I.; Mulders, G. D.

In this paper we investigate the origin of the mid-infrared (IR) hydrogen recombination lines for a sample of 114 disks in different evolutionary stages (full, transitional, and debris disks) collected from the Spitzer archive. We focus on the two brighter H I lines observed in the Spitzer spectra, the H I (7-6) at 12.37 μm and the H I (9-7) at 11.32 μm. We detect the H I (7-6) line in 46 objects, and the H I (9-7) in 11. We compare these lines with the other most common gas line detected in Spitzer spectra, the [Ne II] at 12.81more » μm. We argue that it is unlikely that the H I emission originates from the photoevaporating upper surface layers of the disk, as has been found for the [Ne II] lines toward low-accreting stars. Using the H I (9-7)/H I (7-6) line ratios we find these gas lines are likely probing gas with hydrogen column densities of 10{sup 10}-10{sup 11} cm{sup –3}. The subsample of objects surrounded by full and transitional disks show a positive correlation between the accretion luminosity and the H I line luminosity. These two results suggest that the observed mid-IR H I lines trace gas accreting onto the star in the same way as other hydrogen recombination lines at shorter wavelengths. A pure chromospheric origin of these lines can be excluded for the vast majority of full and transitional disks. We report for the first time the detection of the H I (7-6) line in eight young (<20 Myr) debris disks. A pure chromospheric origin cannot be ruled out in these objects. If the H I (7-6) line traces accretion in these older systems, as in the case of full and transitional disks, the strength of the emission implies accretion rates lower than 10{sup –10} M {sub ☉} yr{sup –1}. We discuss some advantages of extending accretion indicators to longer wavelengths, and the next steps required pinning down the origin of mid-IR hydrogen lines.« less

Spine detection in CT and MR using iterated marginal space learning.

PubMed

Michael Kelm, B; Wels, Michael; Kevin Zhou, S; Seifert, Sascha; Suehling, Michael; Zheng, Yefeng; Comaniciu, Dorin

2013-12-01

Examinations of the spinal column with both, Magnetic Resonance (MR) imaging and Computed Tomography (CT), often require a precise three-dimensional positioning, angulation and labeling of the spinal disks and the vertebrae. A fully automatic and robust approach is a prerequisite for an automated scan alignment as well as for the segmentation and analysis of spinal disks and vertebral bodies in Computer Aided Diagnosis (CAD) applications. In this article, we present a novel method that combines Marginal Space Learning (MSL), a recently introduced concept for efficient discriminative object detection, with a generative anatomical network that incorporates relative pose information for the detection of multiple objects. It is used to simultaneously detect and label the spinal disks. While a novel iterative version of MSL is used to quickly generate candidate detections comprising position, orientation, and scale of the disks with high sensitivity, the anatomical network selects the most likely candidates using a learned prior on the individual nine dimensional transformation spaces. Finally, we propose an optional case-adaptive segmentation approach that allows to segment the spinal disks and vertebrae in MR and CT respectively. Since the proposed approaches are learning-based, they can be trained for MR or CT alike. Experimental results based on 42 MR and 30 CT volumes show that our system not only achieves superior accuracy but also is among the fastest systems of its kind in the literature. On the MR data set the spinal disks of a whole spine are detected in 11.5s on average with 98.6% sensitivity and 0.073 false positive detections per volume. On the CT data a comparable sensitivity of 98.0% with 0.267 false positives is achieved. Detected disks are localized with an average position error of 2.4 mm/3.2 mm and angular error of 3.9°/4.5° in MR/CT, which is close to the employed hypothesis resolution of 2.1 mm and 3.3°. Copyright © 2012 Elsevier B.V. All rights reserved.

Probing Stellar Accretion with Mid-infrared Hydrogen Lines

NASA Astrophysics Data System (ADS)

Rigliaco, Elisabetta; Pascucci, I.; Duchene, G.; Edwards, S.; Ardila, D. R.; Grady, C.; Mendigutía, I.; Montesinos, B.; Mulders, G. D.; Najita, J. R.; Carpenter, J.; Furlan, E.; Gorti, U.; Meijerink, R.; Meyer, M. R.

2015-03-01

In this paper we investigate the origin of the mid-infrared (IR) hydrogen recombination lines for a sample of 114 disks in different evolutionary stages (full, transitional, and debris disks) collected from the Spitzer archive. We focus on the two brighter H I lines observed in the Spitzer spectra, the H I (7-6) at 12.37 μm and the H I (9-7) at 11.32 μm. We detect the H I (7-6) line in 46 objects, and the H I (9-7) in 11. We compare these lines with the other most common gas line detected in Spitzer spectra, the [Ne II] at 12.81 μm. We argue that it is unlikely that the H I emission originates from the photoevaporating upper surface layers of the disk, as has been found for the [Ne II] lines toward low-accreting stars. Using the H I (9-7)/H I (7-6) line ratios we find these gas lines are likely probing gas with hydrogen column densities of 1010-1011 cm-3. The subsample of objects surrounded by full and transitional disks show a positive correlation between the accretion luminosity and the H I line luminosity. These two results suggest that the observed mid-IR H I lines trace gas accreting onto the star in the same way as other hydrogen recombination lines at shorter wavelengths. A pure chromospheric origin of these lines can be excluded for the vast majority of full and transitional disks. We report for the first time the detection of the H I (7-6) line in eight young (<20 Myr) debris disks. A pure chromospheric origin cannot be ruled out in these objects. If the H I (7-6) line traces accretion in these older systems, as in the case of full and transitional disks, the strength of the emission implies accretion rates lower than 10-10 M ⊙ yr-1. We discuss some advantages of extending accretion indicators to longer wavelengths, and the next steps required pinning down the origin of mid-IR hydrogen lines.

X ray spectra of cataclysmic variables

NASA Technical Reports Server (NTRS)

Patterson, Joseph; Halpern, Jules

1990-01-01

X ray spectral parameters of cataclysmic variables observed with the 'Einstein' imaging proportional counter were determined by fitting an optically thin, thermal bremsstrahlung spectrum to the raw data. Most of the sources show temperatures of order a few keV, while a few sources exhibit harder spectra with temperatures in excess of 10 keV. Estimated 0.1 to 3.5 keV luminosities are generally in the range from 10(exp 30) to 10(exp 32) erg/sec. The results are consistent with the x rays originating in a disk/white dwarf boundary layer of non-magnetic systems, or in a hot, post-shock region in the accretion column of DQ Her stars, with a negligible contribution from the corona of the companion. In a few objects column densities were found that are unusually high for interstellar material. It was suggested that the absorption occurs in the system itself.

Consolidation and densification methods for fibrous monolith processing

DOEpatents

Sutaria, Manish P.; Rigali, Mark J.; Cipriani, Ronald A.; Artz, Gregory J.; Mulligan, Anthony C.

2006-06-20

Methods for consolidation and densification of fibrous monolith composite structures are provided. Consolidation and densification of two- and three-dimensional fibrous monolith components having complex geometries can be achieved by pressureless sintering. The fibrous monolith composites are formed from filaments having at least a first material composition generally surrounded by a second material composition. The composites are sintered at a pressure of no more than about 30 psi to provide consolidated and densified fibrous monolith composites.

Synthesis of ordered mesoporous carbon monoliths with bicontinuous cubic pore structure of Ia3d symmetry.

PubMed

Yang, Haifeng; Shi, Qihui; Liu, Xiaoying; Xie, Songhai; Jiang, Decheng; Zhang, Fuqiang; Yu, Chengzhong; Tu, Bo; Zhao, Dongyuan

2002-12-07

Large-diameter-sized mesoporous carbon monoliths with bicontinuous cubic structure of Ia3d symmetry have been synthesized by using mesoporous silica monoliths as hard templates; such carbon monoliths show potential application of advanced electrodes and electrochemical double layer capacitors.

Consolidation and densification methods for fibrous monolith processing

DOEpatents

Sutaria, Manish P.; Rigali, Mark J.; Cipriani, Ronald A.; Artz, Gregory J.; Mulligan, Anthony C.

2004-05-25

Methods for consolidation and densification of fibrous monolith composite structures are provided. Consolidation and densification of two- and three-dimensional fibrous monolith components having complex geometries can be achieved by pressureless sintering. The fibrous monolith composites are formed from filaments having at least a first material composition generally surrounded by a second material composition. The composites are sintered in an inert gas or nitrogen gas at a pressure of no more than about 30 psi to provide consolidated and densified fibrous monolith composites.

Gas storage carbon with enhanced thermal conductivity

DOEpatents

Burchell, Timothy D.; Rogers, Michael Ray; Judkins, Roddie R.

2000-01-01

A carbon fiber carbon matrix hybrid adsorbent monolith with enhanced thermal conductivity for storing and releasing gas through adsorption and desorption is disclosed. The heat of adsorption of the gas species being adsorbed is sufficiently large to cause hybrid monolith heating during adsorption and hybrid monolith cooling during desorption which significantly reduces the storage capacity of the hybrid monolith, or efficiency and economics of a gas separation process. The extent of this phenomenon depends, to a large extent, on the thermal conductivity of the adsorbent hybrid monolith. This invention is a hybrid version of a carbon fiber monolith, which offers significant enhancements to thermal conductivity and potential for improved gas separation and storage systems.

An inorganic boronate affinity in-needle monolithic device for specific capture of cis-diol containing compounds.

PubMed

Jin, Shanxia; Zhang, Wei; Yang, Qin; Dai, Lili; Zhou, Ping

2018-02-01

In this work, inorganic boronate affinity monolith was prepared by in situ synthesis in 0.33mm i.d. stainless steel needle through sol-gel process using tetraethoxysilane and tetrabutyl orthotitanate as the co-precursors. The morphology, structure and composition of the monolith were characterized. In contrast to conventional boronate affinity materials, inorganic boric acid was used as affinity ligand. Different compounds were used for the evaluation of the boronate affinity of this inorganic monolithic material. The monolith exhibited good selectivity towards cis-diol containing compounds. Recovery of greater than 90% was achieved for in-needle extraction of catechol under neutral conditions. Owing to the hydrophilic property of the monolith, the procedure of affinity chromatography could be performed in aqueous solution. This monolithic in-needle device will be useful for boronate affinity extraction of small-volume samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Intense Ly-alpha emission from Uranus

NASA Technical Reports Server (NTRS)

Durrance, S. T.; Moos, H. W.

1982-01-01

The existence of intense atomic hydrogen Ly-alpha emission from Uranus is demonstrated here by utilizing the monochromatic imaging capabilities of the International Ultraviolet Explorer (IUE) spectrograph. Observations show increased emission in the vicinity of Uranus superimposed on the geocoronal/interplanetary background. If resonant scattering of solar Ly-alpha is the source of the 1.6 + or - 0.4 kR disk averaged brightness, then very high column densities of atomic H above the absorbing methane are required. Precipitation of trapped charged particles, i.e., aurora, could explain the emissions. This would imply a planetary magnetic field.

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

Kieffer, T. Forrest; Bogdanović, Tamara, E-mail: tkieffer3@gatech.edu, E-mail: tamarab@gatech.edu

Observations have revealed a relative paucity of red giant (RG) stars within the central 0.5 pc in the Galactic Center (GC). Motivated by this finding we investigate the hypothesis that collisions of stars with a fragmenting accretion disk are responsible for the observed dearth of evolved stars. We use three-dimensional hydrodynamic simulations to model a star with radius 10 R {sub ⊙} and mass 1 M {sub ⊙}, representative of the missing population of RGs, colliding with high density clumps. We find that multiple collisions with clumps of column density ≳10{sup 8} g cm{sup −2} can strip a substantial fractionmore » of the star’s envelope and in principle render it invisible to observations. Simulations confirm that repeated impacts are particularly efficient in driving mass loss as partially stripped RGs expand and have increased cross sections for subsequent collisions. Because the envelope is unbound on account of the kinetic energy of the star, any significant amount of stripping of the RG population in the GC should be mirrored by a systematic decay of their orbits and possibly by their enhanced rotational velocity. To be viable, this scenario requires that the total mass of the fragmenting disk has been several orders of magnitude higher than that of the early-type stars which now form the stellar disk in the GC.« less

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

Kudritzki, R. P.; Ho, I.-T.; Bresolin, F.

Low-resolution (4.5–5 Å) spectra of 58 blue supergiant stars distributed over the disk of the Magellanic spiral galaxy NGC 55 in the Sculptor group are analyzed by means of non-LTE techniques to determine stellar temperatures, gravities, and metallicities (from iron peak and α -elements). A metallicity gradient of −0.22 ± 0.06 dex/ R {sub 25} is detected. The central metallicity on a logarithmic scale relative to the Sun is [ Z ] = −0.37 ± 0.03. A chemical evolution model using the observed distribution of column densities of the stellar and interstellar medium gas mass reproduces the observed metallicity distributionmore » well and reveals a recent history of strong galactic mass accretion and wind outflows with accretion and mass-loss rates of the order of the star formation rate. There is an indication of spatial inhomogeneity in metallicity. In addition, the relatively high central metallicity of the disk confirms that two extraplanar metal-poor H ii regions detected in previous work 1.13 to 2.22 kpc above the galactic plane are ionized by massive stars formed in situ outside the disk. For a subsample of supergiants, for which Hubble Space Telescope photometry is available, the flux-weighted gravity–luminosity relationship is used to determine a distance modulus of 26.85 ± 0.10 mag.« less

Solid-phase assays for small molecule screening using sol-gel entrapped proteins.

PubMed

Lebert, Julie M; Forsberg, Erica M; Brennan, John D

2008-04-01

With compound libraries exceeding one million compounds, the ability to quickly and effectively screen these compounds against relevant pharmaceutical targets has become crucial. Solid-phase assays present several advantages over solution-based methods. For example, a higher degree of miniaturization can be achieved, functional- and affinity-based studies are possible, and a variety of detection methods can be used. Unfortunately, most protein immobilization methods are either too harsh or require recombinant proteins and thus are not amenable to delicate proteins such as kinases and membrane-bound receptors. Sol-gel encapsulation of proteins in an inorganic silica matrix has emerged as a novel solid-phase assay platform. In this minireview, we discuss the development of sol-gel derived protein microarrays and sol-gel based monolithic bioaffinity columns for the high-throughput screening of small molecule libraries and mixtures.

A high efficiency readout architecture for a large matrix of pixels.

NASA Astrophysics Data System (ADS)

Gabrielli, A.; Giorgi, F.; Villa, M.

2010-07-01

In this work we present a fast readout architecture for silicon pixel matrix sensors that has been designed to sustain very high rates, above 1 MHz/mm2 for matrices greater than 80k pixels. This logic can be implemented within MAPS (Monolithic Active Pixel Sensors), a kind of high resolution sensor that integrates on the same bulk the sensor matrix and the CMOS logic for readout, but it can be exploited also with other technologies. The proposed architecture is based on three main concepts. First of all, the readout of the hits is performed by activating one column at a time; all the fired pixels on the active column are read, sparsified and reset in parallel in one clock cycle. This implies the use of global signals across the sensor matrix. The consequent reduction of metal interconnections improves the active area while maintaining a high granularity (down to a pixel pitch of 40 μm). Secondly, the activation for readout takes place only for those columns overlapping with a certain fired area, thus reducing the sweeping time of the whole matrix and reducing the pixel dead-time. Third, the sparsification (x-y address labeling of the hits) is performed with a lower granularity with respect to single pixels, by addressing vertical zones of 8 pixels each. The fine-grain Y resolution is achieved by appending the zone pattern to the zone address of a hit. We show then the benefits of this technique in presence of clusters. We describe this architecture from a schematic point of view, then presenting the efficiency results obtained by VHDL simulations.

[Preparation and performance characterization of gold nanoparticles modified chiral capillary electrochromatography stationary phase].

PubMed

Xiong, Lele; Li, Ruijun; Ji, Yibing

2017-07-08

Gold nanoparticles (GNPs, 15 nm) were prepared and introduced to amino groups derived silica monolithic column. Bovine serum albumin (BSA) was immobilized via covalent modification method onto the carboxylic functionalized GNPs to afford chiral stationary phase (CSP) for enantioseparation. GNPs were well dispersed and successfully incorporated onto the columns with the contents as high as 17.18% by characterization method such as transmission electron microscopy (TEM), ultraviolet (UV)-visible absorption spectra and scanning electron microscopy (SEM). The preparation conditions of the BSA modified CSP were optimized and 10% (v/v) 3-aminopropyltriethoxysilane (APTES) and 15 g/L BSA were selected as appropriate reaction conditions. The enantioseparation performance of the BSA modified CSP has been investigated by capillary electrochromatography (CEC). Enantiomers of tryptophan, ephedrine and atenolol were resolved, and the baseline separation of tryptophan was achieved. Meanwhile, the influences of pH value, buffer concentrations and applied voltages used on the chiral separation were studied, and the optimal separation conditions were 10 mmol/L phosphate buffer at pH 7.4 and 15 kV applied voltages. In comparison with the BSA modified CSP prepared by physical adsorption, the CSP prepared by covalent modification method had better separation results, and the analytes could be separated directly without pre-column derivatization. In addition, the prepared BSA modified CSP exhibited good run to run repeatability with relative standard deviations (RSDs) of the migration times and selectivity factors not more than 2.3% and 0.96%, respectively. This work offers a good thinking for modification with other proteins or other types of chiral selectors.

Hydrogel coated monoliths for enzymatic hydrolysis of penicillin G

PubMed Central

Smeltink, M. W.; Straathof, A. J. J.; Paasman, M. A.; van de Sandt, E. J. A. X.; Kapteijn, F.; Moulijn, J. A.

2008-01-01

The objective of this work was to develop a hydrogel-coated monolith for the entrapment of penicillin G acylase (E. coli, PGA). After screening of different hydrogels, chitosan was chosen as the carrier material for the preparation of monolithic biocatalysts. This protocol leads to active immobilized biocatalysts for the enzymatic hydrolysis of penicillin G (PenG). The monolithic biocatalyst was tested in a monolith loop reactor (MLR) and compared with conventional reactor systems using free PGA, and a commercially available immobilized PGA. The optimal immobilization protocol was found to be 5 g l−1 PGA, 1% chitosan, 1.1% glutaraldehyde and pH 7. Final PGA loading on glass plates was 29 mg ml−1 gel. For 400 cpsi monoliths, the final PGA loading on functionalized monoliths was 36 mg ml−1 gel. The observed volumetric reaction rate in the MLR was 0.79 mol s−1 m−3monolith. Apart from an initial drop in activity due to wash out of PGA at higher ionic strength, no decrease in activity was observed after five subsequent activity test runs. The storage stability of the biocatalysts is at least a month without loss of activity. Although the monolithic biocatalyst as used in the MLR is still outperformed by the current industrial catalyst (immobilized preparation of PGA, 4.5 mol s−1 m−3catalyst), the rate per gel volume is slightly higher for monolithic catalysts. Good activity and improved mechanical strength make the monolithic bioreactor an interesting alternative that deserves further investigation for this application. Although moderate internal diffusion limitations have been observed inside the gel beads and in the gel layer on the monolith channel, this is not the main reason for the large differences in reactor performance that were observed. The pH drop over the reactor as a result of the chosen method for pH control results in a decreased performance of both the MLR and the packed bed reactor compared to the batch system. A different reactor configuration including an optimal pH profile is required to increase the reactor performance. The monolithic stirrer reactor would be an interesting alternative to improve the performance of the monolith-PGA combination. PMID:18427849

A PET Design Based on SiPM and Monolithic LYSO Crystals: Performance Evaluation

NASA Astrophysics Data System (ADS)

González, Antonio J.; Aguilar, Albert; Conde, Pablo; Hernández, Liczandro; Moliner, Laura; Vidal, Luis F.; Sánchez, Filomeno; Sánchez, Sebastián; Correcher, Carlos; Molinos, César; Barberá, Julio; Lankes, Konrad; Junge, Sven; Bruckbauer, Thomas; Bruyndonckx, Peter; Benlloch, Jose M.

2016-10-01

A new small animal PET based on SiPM and monolithic LYSO crystals has been developed. Eight detector modules form the PET ring, each mounting an array of 12 × 12 SiPMs coupled to a readout providing the summed signals of the pixels on each of the 12 rows and 12 columns of the SiPM array. This design makes it possible to accurately determine the centroid of the scintillation light distribution with about 1.6 mm full width at half maximum (FWHM) resolution without correction for the 1 mm source size, and the photon depth of interaction (DOI) with nearly 2 mm FWHM. This single ring PET system has a homogeneous spatial resolution across the entire 80 mm transaxial field of view (FOV) of about 1 mm FWHM. The noise equivalent count rate (NECR) peak is estimated to occur at around 39.2 MBq with a rate of approximately 82.7 kcps for the mouse-like phantom and 22 kcps at 48.1 MBq for the rat-like phantom. Following the NEMA protocol, the peak absolute sensitivity in the center of the FOV is 2.8% for a 30% peak energy window. A pilot test injecting NaF to a mouse of 20 grams is also presented. Finally, the PET ring has been tested in front of a high field 15.2 T Magnetic Resonance (MR). No significant variation on energy and spatial resolution across the FOV has been observed due to the presence of the magnetic field.

Investigation of protein adsorption performance of Ni2+-attached diatomite particles embedded in composite monolithic cryogels.

PubMed

Ünlü, Nuri; Ceylan, Şeyda; Erzengin, Mahmut; Odabaşı, Mehmet

2011-08-01

As a low-cost natural adsorbent, diatomite (DA) (2 μm) has several advantages including high surface area, chemical reactivity, hydrophilicity and lack of toxicity. In this study, the protein adsorption performance of supermacroporous composite cryogels embedded with Ni(2+)-attached DA particles (Ni(2+)-ADAPs) was investigated. Supermacroporous poly(2-hydroxyethyl methacrylate) (PHEMA)-based monolithic composite cryogel column embedded with Ni(2+)-ADAPs was prepared by radical cryo-copolymerization of 2-hydroxyethyl methacrylate (HEMA) with N,N'-methylene-bis-acrylamide (MBAAm) as cross-linker directly in a plastic syringe for affinity purification of human serum albumin (HSA) both from aqueous solutions and human serum. The chemical composition and surface area of DA was determined by XRF and BET method, respectively. The characterization of composite cryogel was investigated by SEM. The effect of pH, and embedded Ni(2+)-ADAPs amount, initial HSA concentration, temperature and flow rate on adsorption were studied. The maximum amount of HSA adsorption from aqueous solution at pH 8.0 phosphate buffer was very high (485.15 mg/g DA). It was observed that HSA could be repeatedly adsorbed and desorbed to the embedded Ni(2+)-ADAPs in poly(2-hydroxyethyl methacrylate) composite cryogel without significant loss of adsorption capacity. The efficiency of albumin adsorption from human serum before and after albumin adsorption was also investigated with SDS-PAGE analyses. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Synthesis of Porous Carbon Monoliths Using Hard Templates.

PubMed

Klepel, Olaf; Danneberg, Nina; Dräger, Matti; Erlitz, Marcel; Taubert, Michael

2016-03-21

The preparation of porous carbon monoliths with a defined shape via template-assisted routes is reported. Monoliths made from porous concrete and zeolite were each used as the template. The porous concrete-derived carbon monoliths exhibited high gravimetric specific surface areas up to 2000 m²·g -1 . The pore system comprised macro-, meso-, and micropores. These pores were hierarchically arranged. The pore system was created by the complex interplay of the actions of both the template and the activating agent as well. On the other hand, zeolite-made template shapes allowed for the preparation of microporous carbon monoliths with a high volumetric specific surface area. This feature could be beneficial if carbon monoliths must be integrated into technical systems under space-limited conditions.

Synthesis of Porous Carbon Monoliths Using Hard Templates

PubMed Central

Klepel, Olaf; Danneberg, Nina; Dräger, Matti; Erlitz, Marcel; Taubert, Michael

2016-01-01

The preparation of porous carbon monoliths with a defined shape via template-assisted routes is reported. Monoliths made from porous concrete and zeolite were each used as the template. The porous concrete-derived carbon monoliths exhibited high gravimetric specific surface areas up to 2000 m2·g−1. The pore system comprised macro-, meso-, and micropores. These pores were hierarchically arranged. The pore system was created by the complex interplay of the actions of both the template and the activating agent as well. On the other hand, zeolite-made template shapes allowed for the preparation of microporous carbon monoliths with a high volumetric specific surface area. This feature could be beneficial if carbon monoliths must be integrated into technical systems under space-limited conditions. PMID:28773338

Multichannel X-Band Dielectric-Resonator Oscillator

NASA Technical Reports Server (NTRS)

Mysoor, Narayan; Dennis, Matthew; Cook, Brian

2006-01-01

A multichannel dielectric-resonator oscillator (DRO), built as a prototype of a local oscillator for an X-band transmitter or receiver, is capable of being electrically tuned among and within 26 adjacent frequency channels, each 1.16 MHz wide, in a band ranging from 7,040 to 7,070 GHz. The tunability of this oscillator is what sets it apart from other DROs, making it possible to use mass-produced oscillator units of identical design in diverse X-band applications in which there are requirements to use different fixed frequencies or to switch among frequency channels. The oscillator (see figure) includes a custom-designed voltage-controlled-oscillator (VCO) monolithic microwave integrated circuit (MMIC), a dielectric resonator disk (puck), and two varactor-coupling circuits, all laid out on a 25-mil (0.635-mm)-thick alumina substrate having a length and width of 17.8 mm. The resonator disk has a diameter of 8.89 mm and a thickness of 4.01 mm. The oscillator is mounted in an 8.9-mm-deep cavity in a metal housing. The VCO MMIC incorporates a negative- resistance oscillator amplifier along with a buffer amplifier. The resonator disk is coupled to a microstrip transmission line connected to the negative-resistance port of the VCO MMIC. The two varactor-coupling circuits include microstrip lines, laid out orthogonally to each other, for coupling with the resonator disk. Each varactor microstrip line is DC-coupled to an external port via a microwave choke. One varactor is used for coarse tuning to select a channel; the other varactor is used (1) for fine tuning across the 1.16-MHz width of each channel and (2) as a feedback port for a phase-lock loop. The resonator disk is positioned to obtain (1) the most desirable bandwidth, (2) relatively tight coupling with the microstrip connected to the coarse-tuning varactor, and (3) relatively loose coupling with the microstrip connected to the fine-tuning varactor. Measurements of performance showed that the oscillator can be switched among any of the 26 channels and can be phase-locked to a nominal frequency in any channel. The degree of nonlinearity of tuning was found not to exceed 2.5 percent. The tuning sensitivity was found to be 6.15 MHz/V at a bias offset of -2 V on the phase-lock-loop varactor. The phase noise of the oscillator in free-running operation was found to be -107 dBc/Hz (where dBc signifies decibels relative to the carrier signal) at 100 kHz away from the carrier frequency.

A computer program for processing impedance cardiographic data: Improving accuracy through user-interactive software

NASA Technical Reports Server (NTRS)

Cowings, Patricia S.; Naifeh, Karen; Thrasher, Chet

1988-01-01

This report contains the source code and documentation for a computer program used to process impedance cardiography data. The cardiodynamic measures derived from impedance cardiography are ventricular stroke column, cardiac output, cardiac index and Heather index. The program digitizes data collected from the Minnesota Impedance Cardiograph, Electrocardiography (ECG), and respiratory cycles and then stores these data on hard disk. It computes the cardiodynamic functions using interactive graphics and stores the means and standard deviations of each 15-sec data epoch on floppy disk. This software was designed on a Digital PRO380 microcomputer and used version 2.0 of P/OS, with (minimally) a 4-channel 16-bit analog/digital (A/D) converter. Applications software is written in FORTRAN 77, and uses Digital's Pro-Tool Kit Real Time Interface Library, CORE Graphic Library, and laboratory routines. Source code can be readily modified to accommodate alternative detection, A/D conversion and interactive graphics. The object code utilizing overlays and multitasking has a maximum of 50 Kbytes.

Electrostatic ion-cyclotron waves in a nonuniform magnetic field

NASA Technical Reports Server (NTRS)

Cartier, S. L.; Dangelo, N.; Merlino, R. L.

1985-01-01

The properties of electrostatic ion-cyclotron waves excited in a single-ended cesium Q machine with a nonuniform magnetic field are described. The electrostatic ion-cyclotron waves are generated in the usual manner by drawing an electron current to a small exciter disk immersed in the plasma column. The parallel and perpendicular (to B) wavelengths and phase velocities are determined by mapping out two-dimensional wave phase contours. The wave frequency f depends on the location of the exciter disk in the nonuniform magnetic field, and propagating waves are only observed in the region where f is approximately greater than fci, where fci is the local ion-cyclotron frequency. The parallel phase velocity is in the direction of the electron drift. From measurements of the plasma properties along the axis, it is inferred that the electron drift velocity is not uniform along the entire current channel. The evidence suggests that the waves begin being excited at that axial position where the critical drift velocity is first exceeded, consistent with a current-driven excitation mechanism.

Development of High Interruption Capability Vacuum Circuit Breaker -Technology of Vacuum Arc Control-

NASA Astrophysics Data System (ADS)

Niwa, Yoshimitsu; Kaneko, Eiji

Vacuum circuit breakers (VCB) have been widely used for power distribution systems. Vacuum Interrupters, which are the current interruption unit, have been increased its interruption capability with the development of vacuum arc control technology by magnetic field. There are three major type electrodes: disk shaped electrodes, radial magnetic field electrodes, axial magnetic field (AMF) electrodes. In the disk shaped electrode, the vacuum arc between the electrodes is not controlled. In the AMF electrode, the vacuum arc is diffused and stabilized by an axial magnetic field, which is parallel to the arc current. In the last type of electrodes, the vacuum arc column is rotated by magnetic force generated by the current flowing in the electrodes. The interruption current and the voltage of one break VCB is increased to 100 kA, 144 kV respectively. This paper describes basic configurations and functions of VCB, vacuum arc control technology in vacuum interrupters, recent researches and applications of VCB.

Unveiling the X-ray/UV properties of disk winds in active galactic nuclei using broad and mini-broad absorption line quasars

NASA Astrophysics Data System (ADS)

Giustini, M.

2016-05-01

We present the results of the uniform analysis of 46 XMM-Newton observations of six BAL and seven mini-BAL QSOs belonging to the Palomar-Green Quasar catalogue. Moderate-quality X-ray spectroscopy was performed with the EPIC-pn, and allowed to characterise the general source spectral shape to be complex, significantly deviating from a power law emission. A simple power law analysis in different energy bands strongly suggests absorption to be more significant than reflection in shaping the spectra. If allowing for the absorbing gas to be either partially covering the continuum emission source or to be ionised, large column densities of the order of 1022-1024 cm-2 are inferred. When the statistics was high enough, virtually every source was found to vary in spectral shape on various time scales, from years to hours. All in all these observational results are compatible with radiation driven accretion disk winds shaping the spectra of these intriguing cosmic sources.

Nonlinear radiated MHD flow of nanoliquids due to a rotating disk with irregular heat source and heat flux condition

NASA Astrophysics Data System (ADS)

Mahanthesh, B.; Gireesha, B. J.; Shehzad, S. A.; Rauf, A.; Kumar, P. B. Sampath

2018-05-01

This research is made to visualize the nonlinear radiated flow of hydromagnetic nano-fluid induced due to rotation of the disk. The considered nano-fluid is a mixture of water and Ti6Al4V or AA7072 nano-particles. The various shapes of nanoparticles like lamina, column, sphere, tetrahedron and hexahedron are chosen in the analysis. The irregular heat source and nonlinear radiative terms are accounted in the law of energy. We used the heat flux condition instead of constant surface temperature condition. Heat flux condition is more relativistic and according to physical nature of the problem. The problem is made dimensionless with the help of suitable similarity constraints. The Runge-Kutta-Fehlberg scheme is adopted to find the numerical solutions of governing nonlinear ordinary differential systems. The solutions are plotted by considering the various values of emerging physical constraints. The effects of various shapes of nanoparticles are drawn and discussed.

Catalytic Ignition and Upstream Reaction Propagation in Monolith Reactors

NASA Technical Reports Server (NTRS)

Struk, Peter M.; Dietrich, Daniel L.; Miller, Fletcher J.; T'ien, James S.

2007-01-01

Using numerical simulations, this work demonstrates a concept called back-end ignition for lighting-off and pre-heating a catalytic monolith in a power generation system. In this concept, a downstream heat source (e.g. a flame) or resistive heating in the downstream portion of the monolith initiates a localized catalytic reaction which subsequently propagates upstream and heats the entire monolith. The simulations used a transient numerical model of a single catalytic channel which characterizes the behavior of the entire monolith. The model treats both the gas and solid phases and includes detailed homogeneous and heterogeneous reactions. An important parameter in the model for back-end ignition is upstream heat conduction along the solid. The simulations used both dry and wet CO chemistry as a model fuel for the proof-of-concept calculations; the presence of water vapor can trigger homogenous reactions, provided that gas-phase temperatures are adequately high and there is sufficient fuel remaining after surface reactions. With sufficiently high inlet equivalence ratio, back-end ignition occurs using the thermophysical properties of both a ceramic and metal monolith (coated with platinum in both cases), with the heat-up times significantly faster for the metal monolith. For lower equivalence ratios, back-end ignition occurs without upstream propagation. Once light-off and propagation occur, the inlet equivalence ratio could be reduced significantly while still maintaining an ignited monolith as demonstrated by calculations using complete monolith heating.

Preparation of monomeric and polymeric β-cyclodextrin functionalized monoliths for rapid isolation and purification of puerarin from Radix puerariae.

PubMed

Lv, Yongqin; Hughes, Timothy C; Hao, Xiaojuan; Mei, Danping; Tan, Tianwei

2011-08-01

Monomeric and epichlorohydrin polymerized β-CD functionalized monoliths were prepared for the rapid isolation and purification of the isoflavonoid puerarin, a well-known traditional Chinese drug, from a crude extract of Radix puerariae (root of the plant Pueraria lobata). Two copolymers poly(isocyanatoethyl methacrylate-co-methyl methacrylate-co-ethylene dimethacrylate) (poly(IEM-co-MMA-co-EDMA)) and poly(glycidyl methacrylate-co-EDMA) (poly(GMA-co-EDMA)) were developed as facile, highly reactive and versatile monolithic matrix. SEM characterization demonstrated that the modified monoliths had homogenous porous structure and morphology. The success of the chemical modification of the monolithic matrix was confirmed by Fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), solid-state (13) C NMR and elemental analysis. It was demonstrated that polymeric β-CD modified monoliths had better separation and selectivity for puerarin, recovering puerarin with a purity of 96% (m%) and a yield of 93% (m%). Compared with poly(glycidyl methacrylate-co-EDMA), poly(isocyanatoethyl methacrylate-co-methyl methacrylate-co-EDMA) monolithic matrix had higher reactivity, which significantly improved the β-CD ligand density and thus the selectivity of the monoliths. Puerarin with a purity of 96% (m%) and with a yield of 89% (m%) was recovered on the monolith. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A novel surface modification technique for forming porous polymer monoliths in poly(dimethylsiloxane).

PubMed

Burke, Jeffrey M; Smela, Elisabeth

2012-03-01

A new method of surface modification is described for enabling the in situ formation of homogenous porous polymer monoliths (PPMs) within poly(dimethylsiloxane) (PDMS) microfluidic channels that uses 365 nm UV illumination for polymerization. Porous polymer monolith formation in PDMS can be challenging because PDMS readily absorbs the monomers and solvents, changing the final monolith morphology, and because PDMS absorbs oxygen, which inhibits free-radical polymerization. The new approach is based on sequentially absorbing a non-hydrogen-abstracting photoinitiator and the monomers methyl methacrylate and ethylene diacrylate within the walls of the microchannel, and then polymerizing the surface treatment polymer within the PDMS, entangled with it but not covalently bound. Four different monolith compositions were tested, all of which yielded monoliths that were securely anchored and could withstand pressures exceeding the bonding strength of PDMS (40 psi) without dislodging. One was a recipe that was optimized to give a larger average pore size, required for low back pressure. This monolith was used to concentrate and subsequently mechanical lyse B lymphocytes.

Coupling effects in the modal emission of colloidal quantum dot microdisk lasers.

NASA Astrophysics Data System (ADS)

Lafalce, Evan; Zheng, Qingji; Lin, Chunhao; Smith, Marcus; Malak, Sidney; Jung, Jaehan; Yoon, Young; Lin, Zhiqun; Tsukruk, Vladimir; Vardeny, Z. Valy

Solution-processed semiconductors such as colloidal quantum dots (CQD) are particularly suited materials for monolithic fabrication of laser microstructures because of their ease of fabrication and compatibility with conventional lithographic techniques. We use the functionality of core/alloyed-shell CQDs to fabricate microdisk lasers of variable size and study the resulting whispering-gallery mode laser emission. In particular we study the effects of near-field coupling on resonant modes of pairs of these lasers with sub-micrometer spacing. We demonstrate the occurrence of lasing modes that originate from the interaction between two such microdisks by means of varying the spatial distribution and magnitude of the gain and loss in the coupled-pair. The transition from emission of modes localized on a single disk to those of the interacting pair is accompanied by coalescence of eigen-frequencies and pump-induced turn-off of lasing, highlighting the role of parity-time symmetry and exceptional point physics. This work was funded by AFOSR through MURI Grant RA 9550-14-1-0037.

Polymer network/carbon layer on monolith support and monolith catalytic reactor

DOEpatents

Nordquist, Andrew Francis; Wilhelm, Frederick Carl; Waller, Francis Joseph; Machado, Reinaldo Mario

2003-08-26

The present invention relates to an improved monolith catalytic reactor and a monolith support. The improvement in the support resides in a polymer network/carbon coating applied to the surface of a porous substrate and a catalytic metal, preferably a transition metal catalyst applied to the surface of the polymer network/carbon coating. The monolith support has from 100 to 800 cells per square inch and a polymer network/carbon coating with surface area of from 0.1 to 15 m.sup.2 /gram as measured by adsorption of N.sub.2 or Kr using the BET method.

X-Ray Reflection and an Exceptionally Long Thermonuclear Helium Burst from IGR J17062-6143

NASA Technical Reports Server (NTRS)

Keek, L.; Iwakiri, W.; Serino, M.; Ballantyne, D. R.; in’t Zand, J. J. M.; Strohmayer, T. E.

2017-01-01

Thermonuclear X-ray bursts from accreting neutron stars power brief but strong irradiation of their surroundings, providing a unique way to study accretion physics. We analyze MAXI/Gas Slit Camera and Swift/XRT spectra of a day-long flash observed from IGR J17062-6143 in 2015. It is a rare case of recurring bursts at a low accretion luminosity of 0.15% Eddington. Spectra from MAXI, Chandra, and NuSTAR observations taken between the 2015 burst and the previous one in 2012 are used to determine the accretion column. We find it to be consistent with the burst ignition column of 5x10(exp 10) g cm (exp -2), which indicates that it is likely powered by burning in a deep helium layer. The burst flux is observed for over a day, and decays as a straight power law: F gamma t (exp -1.15). The burst and persistent spectra are well described by thermal emission from the neutron star, Comptonization of this emission in a hot optically thin medium surrounding the star, and reflection off the photoionized accretion disk. At the burst peak, the Comptonized component disappears, when the burst may dissipate the Comptonizing gas, and it returns in the burst tail. The reflection signal suggests that the inner disk is truncated at approximately 102 gravitational radii before the burst, but may move closer to the star during the burst. At the end of the burst, the flux drops below the burst cooling trend for 2 days, before returning to the pre-burst level.

Variably porous structures

DOEpatents

Braun, Paul V [Savoy, IL; Yu, Xindi [Urbana, IL

2011-01-18

A method of making a monolithic porous structure, comprises electrodepositing a material on a template; removing the template from the material to form a monolithic porous structure comprising the material; and electropolishing the monolithic porous structure.

Solar XUV Imaging and Non-dispersive Spectroscopy for Solar-C Enabled by Scientific CMOS APS Arrays

NASA Astrophysics Data System (ADS)

Stern, Robert A.; Lemen, J. R.; Shing, L.; Janesick, J.; Tower, J.

2009-05-01

Monolithic CMOS Advanced Pixel Sensor (APS) arrays are showing great promise as eventual replacements for the current workhorse of solar physics focal planes, the scientific CCD. CMOS APS devices have individually addressable pixels, increased radiation tolerance compared to CCDs, and require lower clock voltages, and thus lower power. However, commercially available CMOS chips, while suitable for use with intensifiers or fluorescent coatings, are generally not optimized for direct detection of EUV and X-ray photons. A high performance scientific CMOS array designed for these wavelengths will have significant new capabilities compared to CCDs, including the ability to read out small regions of the solar disk at high (sub sec) cadence, count single X-ray photons with Fano-limited energy resolution, and even operate at room temperature with good noise performance. Such capabilities will be crucial for future solar X-ray and EUV missions such as Solar-C. Sarnoff Corporation has developed scientific grade, monolithic CMOS arrays for X-ray imaging and photon counting. One prototype device, the "minimal" array, has 8 um pixels, is 15 to 25 um thick, is fabricated on high-resistivity ( 10 to 20 kohm-cm) Si wafers, and can be back-illuminated. These characteristics yield high quantum efficiency and high spatial resolution with minimal charge sharing among pixels, making it ideal for the detection of keV X-rays. When used with digital correlated double sampling, the array has demonstrated noise performance as low as 2 e, allowing single photon counting of X-rays over a range of temperatures. We report test results for this device in X-rays, and discuss the implications for future solar space missions.

UTSA-16 Growth within 3D-Printed Co-Kaolin Monoliths with High Selectivity for CO2/CH4, CO2/N2, and CO2/H2 Separation.

PubMed

Lawson, Shane; Al-Naddaf, Qasim; Krishnamurthy, Anirduh; Amour, Marc St; Griffin, Connor; Rownaghi, Ali A; Knox, James C; Rezaei, Fateme

2018-06-06

Honeycomb monoliths loaded with metal-organic frameworks (MOFs) are highly desirable adsorption contactors because of their low-pressure drop, rapid mass-transfer kinetics, and high-adsorption capacity. Moreover, three-dimensional (3D)-printing technology renders direct material modification a realistic and economic prospect. In this study, 3D printing was utilized to impregnate kaolin-based monolith with UTSA-16 metal formation precursor (Co), whereupon an internal growth was facilitated via a solvothermal synthesis approach. The cobalt weight loading in the kaolin support was varied systematically to optimize the MOF growth while retaining monolith mechanical integrity. The obtained UTSA-16 monolith with 90 wt % loading exhibited similar textural features and adsorption characteristics to its powder analogue while improving upon structural integrity. In comparison to previously developed 3D-printed UTSA-16 monoliths, the UTSA-16-kaolin monolith not only showed higher MOF loading but also higher compression stress, indicative of its robust structure. Furthermore, the 3D-printed UTSA-16-kaolin monolith displayed a comparable CO 2 adsorption capacity to the UTSA-16 powder (3.1 vs 3.5 mmol/g at 25 °C and 1 bar), which was proportional to its loading. Selectivity values of 49, 238, and 3725 were obtained for CO 2 /CH 4 , CO 2 /N 2 , and CO 2 /H 2 , respectively, demonstrating good separation potential of the 3D-printed MOF monolith for various gas mixtures, as determined by both equilibrium and dynamic adsorption measurements. Overall, this study provides a novel route for the fabrication of UTSA-16-loaded monoliths, which demonstrate both high MOF loading and mechanical integrity that could be readily applied to various CO 2 capture applications.

The molecular chemistry of diffuse and translucent clouds in the line-of-sight to Sgr B2: Absorption by simple organic and inorganic molecules in the GBT PRIMOS survey

NASA Astrophysics Data System (ADS)

Corby, J. F.; McGuire, B. A.; Herbst, E.; Remijan, A. J.

2018-02-01

The 1-50 GHz PRebiotic Interstellar MOlecular Survey (PRIMOS) contains 50 molecular absorption lines observed in clouds located in the line-of-sight to Sgr B2(N). The line-of-sight material is associated with diffuse and translucent clouds located in the Galactic center, bar, and spiral arms in the disk. We measured the column densities and estimate abundances, relative to H2, of 11 molecules and additional isotopologues observed in this material. We used absorption by optically thin transitions of c-C3H2 to estimate the molecular hydrogen columns, and argue that this method is preferable to more commonly used methods. We discuss the kinematic structure and abundance patterns of small molecules including the sulfur-bearing species CS, SO, CCS, H2CS, and HCS+; oxygen-bearing molecules OH, SiO, and H2CO; and simple hydrocarbon molecules c-C3H2, l-C3H, and l-C3H+. Finally, we discuss the implications of the observed chemistry for the structure of the gas and dust in the ISM. Highlighted results include the following. First, whereas gas in the disk has a molecular hydrogen fraction of 0.65, clouds on the outer edge of the Galactic bar and in or near the Galactic center have molecular fractions of 0.85 and >0.9, respectively. Second, we observe trends in isotope ratios with Galactocentric distance; while carbon and silicon show enhancement of the rare isotopes at low Galactocentric distances, sulfur exhibits no trend with Galactocentric distance. We also determine that the ratio of c-C3H2/c-H13CCCH provides a good estimate of the 12C/13C ratio, whereas H2CO/H213CO exhibits fractionation. Third, we report the presence of l-C3H+ in diffuse clouds for the first time. Finally, we suggest that CS has an enhanced abundance within higher density clumps of material in the disk, and therefore may be diagnostic of cloud conditions. If this holds, the diffuse clouds in the Galactic disk contain multiple embedded hyperdensities in a clumpy structure, and the density profile is not a simple function of AV. The reduced spectra (FITS files) are only available at the CDS via anonymous ftp to http://cdsarc.u-strasbg.fr (http://130.79.128.5) or via http://cdsarc.u-strasbg.fr/viz-bin/qcat?J/A+A/610/A10

Multi-wavelength simulations of atmospheric radiation from Io with a 3-D spherical-shell backward Monte Carlo radiative transfer model

NASA Astrophysics Data System (ADS)

Gratiy, Sergey L.; Walker, Andrew C.; Levin, Deborah A.; Goldstein, David B.; Varghese, Philip L.; Trafton, Laurence M.; Moore, Chris H.

2010-05-01

Conflicting observations regarding the dominance of either sublimation or volcanism as the source of the atmosphere on Io and disparate reports on the extent of its spatial distribution and the absolute column abundance invite the development of detailed computational models capable of improving our understanding of Io's unique atmospheric structure and origin. Improving upon previous models, Walker et al. (Walker, A.C., Gratiy, S.L., Levin, D.A., Goldstein, D.B., Varghese, P.L., Trafton, L.M., Moore, C.H., Stewart, B. [2009]. Icarus) developed a fully 3-D global rarefied gas dynamics model of Io's atmosphere including both sublimation and volcanic sources of SO 2 gas. The fidelity of the model is tested by simulating remote observations at selected wavelength bands and comparing them to the corresponding astronomical observations of Io's atmosphere. The simulations are performed with a new 3-D spherical-shell radiative transfer code utilizing a backward Monte Carlo method. We present: (1) simulations of the mid-infrared disk-integrated spectra of Io's sunlit hemisphere at 19 μm, obtained with TEXES during 2001-2004; (2) simulations of disk-resolved images at Lyman- α obtained with the Hubble Space Telescope (HST), Space Telescope Imaging Spectrograph (STIS) during 1997-2001; and (3) disk-integrated simulations of emission line profiles in the millimeter wavelength range obtained with the IRAM-30 m telescope in October-November 1999. We found that the atmospheric model generally reproduces the longitudinal variation in band depth from the mid-infrared data; however, the best match is obtained when our simulation results are shifted ˜30° toward lower orbital longitudes. The simulations of Lyman- α images do not reproduce the mid-to-high latitude bright patches seen in the observations, suggesting that the model atmosphere sustains columns that are too high at those latitudes. The simulations of emission line profiles in the millimeter spectral region support the hypothesis that the atmospheric dynamics favorably explains the observed line widths, which are too wide to be formed by thermal Doppler broadening alone.

Nanoparticle-Functionalized Porous Polymer Monolith Detection Elements for Surface-Enhanced Raman Scattering

PubMed Central

Liu, Jikun; White, Ian; DeVoe, Don L.

2011-01-01

The use of porous polymer monoliths functionalized with silver nanoparticles is introduced in this work for high-sensitivity surface-enhanced Raman scattering (SERS) detection. Preparation of the SERS detection elements is a simple process comprising the synthesis of a discrete polymer monolith section within a silica capillary, followed by physically trapping silver nanoparticle aggregates within the monolith matrix. A SERS detection limit of 220 fmol for Rhodamine 6G (R6G) is demonstrated, with excellent signal stability over a 24 h period. The capability of the SERS-active monolith for label-free detection of biomolecules was demonstrated by measurements of bradykinin and cyctochrome c. The SERS-active monoliths can be readily integrated into miniaturized micro-total-analysis systems for on-line and label-free detection for a variety of biosensing, bioanalytical, and biomedical applications. PMID:21322579

Probing the Effects of Templating on the UV and Visible Light Photocatalytic Activity of Porous Nitrogen-Modified Titania Monoliths for Dye Removal.

PubMed

Nursam, Natalita M; Wang, Xingdong; Tan, Jeannie Z Y; Caruso, Rachel A

2016-07-13

Porous nitrogen-modified titania (N-titania) monoliths with tailored morphologies were prepared using phase separation and agarose gel templating techniques. The doping and templating process were simultaneously carried out in a one-pot step using alcohol amine-assisted sol-gel chemistry. The amount of polymer used in the monoliths that were prepared using phase separation was shown to affect both the physical and optical properties: higher poly(ethylene glycol) content increased the specific surface area, porosity, and visible light absorption of the final materials. For the agarose-templated monoliths, the infiltration conditions affected the monolith morphology. A porous monolith with high surface area and the least shrinkage was obtained when the N containing alkoxide precursor was infiltrated into the agarose scaffolds at 60 °C. The effect of the diverse porous morphologies on the photocatalytic activity of N-titania was studied for the decomposition of methylene blue (MB) under visible and UV light irradiation. The highest visible light activity was achieved by the agarose-templated N-titania monolith, in part due to higher N incorporation. This sample also showed better UV activity, partly because of the higher specific surface area (up to 112 m(2) g(-1)) compared to the phase separation-induced monoliths (up to 103 m(2) g(-1)). Overall, agarose-templated, porous N-titania monoliths provided better features for effectively removing the MB contaminant.

Less common applications of monoliths III. Gas chromatography

PubMed Central

Svec, Frantisek; Kurganov, Alexander A.

2008-01-01

Porous polymer monoliths emerged about two decades ago. Despite this short time, they are finding applications in a variety of fields. In addition to the most common and certainly best known use of this new category of porous media as stationary phases in liquid chromatography, monolithic materials also found their applications in other areas. This review article focuses on monoliths in capillaries designed for separations in gas chromatography. PMID:17645884

Photoinitiated grafting of porous polymer monoliths and thermoplastic polymers for microfluidic devices

DOEpatents

Frechet, Jean M. J. [Oakland, CA; Svec, Frantisek [Alameda, CA; Rohr, Thomas [Leiden, NL

2008-10-07

A microfluidic device preferably made of a thermoplastic polymer that includes a channel or a multiplicity of channels whose surfaces are modified by photografting. The device further includes a porous polymer monolith prepared via UV initiated polymerization within the channel, and functionalization of the pore surface of the monolith using photografting. Processes for making such surface modifications of thermoplastic polymers and porous polymer monoliths are set forth.

Ultralow Noise Monolithic Quantum Dot Photonic Oscillators

DTIC Science & Technology

2013-10-28

HBCU/MI) ULTRALOW NOISE MONOLITHIC QUANTUM DOT PHOTONIC OSCILLATORS LUKE LESTER UNIVERSITY OF NEW MEXICO 10/28/2013 Final Report DISTRIBUTION A...TELEPHONE NUMBER (Include area code) 24-10-2013 Final 01-06-2010 to 31-05-2013 Ultralow Noise Monolithic Quantum Dot Photonic Oscillators FA9550-10-1-0276...277-7647 Reset Grant Title: ULTRALOW NOISE MONOLITHIC QUANTUM DOT PHOTONIC OSCILLATORS Grant/Contract Number: FA9550-10-1-0276 Final Performance

Carbon nanotube-based benzyl polymethacrylate composite monolith as a solid phase extraction adsorbent and a stationary phase material for simultaneous extraction and analysis of polycyclic aromatic hydrocarbon in water.

PubMed

Al-Rifai, Asma'a; Aqel, Ahmad; Wahibi, Lamya Al; ALOthman, Zeid A; Badjah-Hadj-Ahmed, Ahmed-Yacine

2018-02-02

A composite of multi-walled carbon nanotubes incorporated into a benzyl methacrylate-co-ethylene dimethacrylate porous monolith was prepared, characterized and used as solid phase adsorbent and as stationary phase for simultaneous extraction and separation of ten polycyclic aromatic hydrocarbons, followed by nano-liquid chromatography analysis. The extraction and chromatographic parameters were optimized with regard to the extraction efficiency and the quality of chromatographic analytes separation. Under the optimized conditions, all PAHs were separated in 13 min with suitable resolution values (Rs = 1.74-3.98). Addition of a small amount of carbon nanotubes (0.1% with respect to monomers) to the polymerization mixture increased the efficiency for the separation column to over 41,700 plates m -1 for chrysene at flow rate of 0.5 μL min -1 . The method showed a wide linear range (1-500 μg L -1 with R 2 more than 0.9938), acceptable extraction repeatability (RSDs < 6.4%, n = 3) and reproducibility (RSDs < 12.6%, five parallel-made solid phase extraction cartridges) and satisfactory detection limits (0.02-0.22 μg L -1 ). Finally, the proposed method was successfully applied to the detection of polycyclic aromatic hydrocarbons in environmental water samples. After a simple extraction procedure with preconcentration factor equal to 100, the average recovery values in ultra-pure, tap and sea water samples were found to be in the range 81.3-95.4% with %RSD less than 6.4. Again, the presence of carbon nanotubes (0.3% relatively to monomers) in native polymer enhanced the extraction performance for the solid phase adsorbent up to 78.4%. The application of the monoliths modified with CNTs in extraction and nano-scale liquid chromatography for analysis of environmental samples offered several advantages; it demonstrated an acceptable precision, low detection limits, good reproducibility, satisfying recoveries and wide dynamic linear ranges. Copyright © 2018. Published by Elsevier B.V.

Layered storage of biogenic methane-enriched gas bubbles in peat: A lumped capacitance model controlled by soil structure

NASA Astrophysics Data System (ADS)

Chen, X.; Comas, X.; Binley, A. M.; Slater, L. D.

2017-12-01

Methane can accumulate in the gaseous phase in peats, and enter the atmosphere as gas bubbles with a mass flux higher than that via diffusion and plant-mediated pathways. A complete understanding of the mechanisms regulating bubble storage in peats remains incomplete. We developed a layered model to quantify the storage of gas bubbles over a peat column based on a general lumped capacitance model. This conceptual model was applied to explain the effects of peat structure on bubble storage at different depths observed in a laboratory experiment. A peat monolith was collected from the Everglades, a subtropical wetland located in Florida (USA), and kept submerged in a cuboid chamber over 102 days until gas bubble saturation was achieved. Time-lapse ground-penetrating radar (GPR) was used to estimate changes in gas content of each layer and the corresponding average dimensions of stored gas bubbles. The results highlight a hotspot layer of bubble accumulation at depths between 5 and 10 cm below the monolith surface. Bubbles in this shallow hotspot layer were larger relative to those in deeper layers, whilst the degree of decomposition of the upper layers was generally smaller than that of the lower layers based on von Post humification tests. X-ray Computer tomography (CT) was applied to resin-impregnated peat sections from different depths and the results showed that a higher porosity promotes bubbles storage. The stored gas bubbles were released by changing water levels and the air CH4 concentrations above the peat monolith were measured using a flow-through chamber system to confirm the high CH4 concentration in the stored bubbles. Our findings suggest that bubble capacitance is related to the difference in size between gas bubbles and peat pores. This work has implications for better understanding how changes in water table elevation associated with climate change and sea level rise (particularly for freshwater wetlands near coastal areas like the Everglades) may potentially alter bubble sizes, thus bubble storage in peats.

A dust and water disk in AFGL 2591

NASA Astrophysics Data System (ADS)

van der Tak, Floris; Walmsley, Malcolm; Herpin, Fabrice; Ceccarelli, Cecilia

High-mass stars may form by disk accretion like low-mass stars, but observational evidence for massive circumstellar disks remains sparse even after intense searches. We present Plateau de Bure observations of dust continuum and H218O line emission at 1.3 mm wavelength which show a rotating disk around the nearby (d=1 kpc) high-mass (L = 2 × 104 Lsol) protostar AFGL 2591. The 205 GHz map shows three sources. Comparison with OVRO 86 GHz images in- dicates that the strongest source is due to dust, while the other two are dominated by ionized gas. The dust source is compact (? ≍ 800 AU) and somewhat elongated (axis ratio ≍ 0.8). Its flux density indicates a mass of ≍ 0.8 Msol which is ≍ 5% of the mass of the central star. The dust opacity index β ≍ 1, suggesting grain growth. These observations suggest a disk at an inclination of ≍ 32◦ (almost face-on), but spectral line data are needed to test this idea. H218O line emission is only detected toward the dust source. The size and shape of the emission are very similar to that of the continuum. All of the single-dish line flux is recovered, so that there is probably little extended flux missing. Radiative transfer models indicate a H2O abundance of ~10-4, similar to the H2O ice abundance measured in the mid-infrared. The origin of the H2O thus seems to be evaporation of grain mantles. The position of the H218O emission peak shows a systematic shift with velocity. Such a gradient could arise in a bipolar outflow, but the high column densities (N(H2O) ~ 3 × 1019 cm-2; N(H2) ~ 2 × 1024 cm-2) argue against this. Moreover, the velocity gradient is not oriented East-West like the large-scale outflow from AFGL 2591. Thus the H218O velocity gradient probably traces a rotating disk. The magnitude of the velocity gradient is consistent with Keplerian rotation around the central star. In the near future, we plan to use more extended array configurations to resolve the velocity field.

ROSAT detection of diffuse hot gas in the edge-on galaxy NGC 4631

NASA Technical Reports Server (NTRS)

Wang, Q. David; Walterbos, Rene A. M.; Steakley, Michael F.; Norman, Colin A.; Braun, Robert

1994-01-01

ROSAT observation is presented of the edge-on spiral galaxy NGC 4631, a nearby Sc/SBd galaxy best known for its extended radio halo. Because of the low foreground Galactic X-ray-absorbing gas column density, N(sub H) approximately 1.4 x 10(exp 20)cm(exp -2), this observation is sensitive to gas of temperature greater than or equal to a few times 10(exp 5) K. A soft (approximately 0.25 keV) X-ray radiation out to more than 8 kpc above the midplane of the galaxy was detected. The strongest X-ray emission in the halo is above the central disk, a region of about 3 kpc radius which shows high star formation activity. The X-ray emission in the halo is bordered by two extended filaments of radio continuum emission. Diffuse X-ray emission from hot gas in the galaxy's disk was found. The spectrum of the radiation can be characterized by a thermal plasma with a temperature of 3 x 10(exp 6) K and a radiative cooling rate of approximately 8 x 10(exp 39) ergs s(exp -1). This rate is only a few percent of the estimated supernova energy release in the interstellar medium of the galaxy. Analysis of the X-ray spectrum shows evidence for the presence of a cooler (several times 10(exp 5) K) halo gas component that could consume a much larger fraction of the supernova energy. Strong evidence was found for disk/halo interaction. Hot gas apparently blows out from supershells in the galaxy's disk at a rate of approximately 1 solar mass yr(exp -1). This outflow of hot gas drags magnetic field lines up in the halo and forms a magnetized gaseous halo. If the magnetic field lines are still anchored to the disk gas at large disk radii, the outflowing gas may be confined high above the disk by magnetic pressure. A strong X-ray source which coincides spatially with an H I supershell has been identified. However, the source is likely an extremely luminous X-ray binary with L(sub chi)(0.1 - 2 keV) approximately 5 x 10(exp 39) ergs s(exp -1), which makes it a stellar mass black hole candidate.

The vertical structure and stability of accretion disks surrounding black holes and neutron stars

NASA Technical Reports Server (NTRS)

Milsom, J. A.; Chen, Xingming; Taam, Ronald E.

1994-01-01

The structure and stability of the inner regions of accretion disks surrounding neutron stars and black holes have been investigated. Within the framework of the alpha viscosity prescription for optically thick disks, we assume the viscous stress scales with gas pressure only, and the alpha parameter, which is less than or equal to unity, is formulated as alpha(sub 0)(h/r)(exp n), where h is the local scale height and n and alpha(sub 0) are constants. We neglect advective energy transport associated with radial motions and construct the vertical structure of the disks by assuming a Keplerian rotation law and local hydrostatic and thermal equilibrium. The vertical structures have been calculated with and without convective energy transport, and it has been demonstrated that convection is important especially for mass accretion rates, M-dot, greater than about 0.1 times the Eddington value, M-dot(sub Edd). Although the efficiency of convection is not high, convection significantly modifies the vertical structure of the disk (as compared with a purely radiative model) and leads to lower temperatures at a given M-dot. The results show that the disk can be locally unstable and that for n greater than or = 0.75, an S-shaped relation can exist between M-dot and the column density, sigma, at a given radius. While the lower stable branch (derivative of M-dot/derivative of sigma greater than 0) and middle unstable branch (derivative of M-dot/derivative of sigma less than 0) represent structures for which the gas and radiation pressure dominate respectively, the stable upper branch (derivative of M-dot/derivative of sigma greater than 0) is a consequence of the saturation of alpha. This saturation of alpha can occur for large alpha(sub 0) and at M-dot less than or = M-dot(sub Edd). The instability is found to occur at higher mass accretion rates for neutron stars than for black holes. In particular, the disk is locally unstable for M-dot greater than or = 0.5 M-dot(sub Edd) for neutron stars and for M-dot greater than or = M-dot(sub Edd) for black holes for a viscosity prescription characterized by n = 1 and alpha(sub 0) = 10.

CHANDRA/ACIS-I STUDY OF THE X-RAY PROPERTIES OF THE NGC 6611 AND M16 STELLAR POPULATIONS

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

Guarcello, M. G.; Drake, J. J.; Caramazza, M.

2012-07-10

Mechanisms regulating the origin of X-rays in young stellar objects and the correlation with their evolutionary stage are under debate. Studies of the X-ray properties in young clusters allow us to understand these mechanisms. One ideal target for this analysis is the Eagle Nebula (M16), with its central cluster NGC 6611. At 1750 pc from the Sun, it harbors 93 OB stars, together with a population of low-mass stars from embedded protostars to disk-less Class III objects, with age {<=}3 Myr. We study an archival 78 ks Chandra/ACIS-I observation of NGC 6611 and two new 80 ks observations of themore » outer region of M16, one centered on the Column V and the other on a region of the molecular cloud with ongoing star formation. We detect 1755 point sources with 1183 candidate cluster members (219 disk-bearing and 964 disk-less). We study the global X-ray properties of M16 and compare them with those of the Orion Nebula Cluster. We also compare the level of X-ray emission of Class II and Class III stars and analyze the X-ray spectral properties of OB stars. Our study supports the lower level of X-ray activity for the disk-bearing stars with respect to the disk-less members. The X-ray luminosity function (XLF) of M16 is similar to that of Orion, supporting the universality of the XLF in young clusters. Eighty-five percent of the O stars of NGC 6611 have been detected in X-rays. With only one possible exception, they show soft spectra with no hard components, indicating that mechanisms for the production of hard X-ray emission in O stars are not operating in NGC 6611.« less

A Simple Approach to Enhance the Water Stability of a Metal-Organic Framework.

PubMed

Shih, Yung-Han; Kuo, Yu-Ching; Lirio, Stephen; Wang, Kun-Yun; Lin, Chia-Her; Huang, Hsi-Ya

2017-01-01

A facile method to improve the feasibility of water-unstable metal-organic frameworks in an aqueous environment has been developed that involves imbedding in a polymer monolith. The effect of compartment type during polymerization plays a significant role in maintaining the crystalline structure and thermal stability of the MOFs, which was confirmed by powder X-ray diffraction (PXRD) and thermogravimetric analysis (TGA), respectively. The MOF-polymer composite prepared in a narrow compartment (column, ID 0.8 mm) has better thermal and chemical stability than that prepared in a broad compartment (vial, ID 7 mm). The developed MOF-polymer composite was applied as an adsorbent in solid-phase microextraction of nine non-steroidal anti-inflammatory drugs (NSAIDs) and could be used for extraction more than 30 times, demonstrating that the proposed approach has potential for industrial applications. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Graphene-supported metal oxide monolith

DOEpatents

Worsley, Marcus A.; Baumann, Theodore F.; Biener, Juergen; Biener, Monika A.; Wang, Yinmin; Ye, Jianchao; Tylski, Elijah

2017-01-10

A composition comprising at least one graphene-supported metal oxide monolith, said monolith comprising a three-dimensional structure of graphene sheets crosslinked by covalent carbon bonds, wherein the graphene sheets are coated by at least one metal oxide such as iron oxide or titanium oxide. Also provided is an electrode comprising the aforementioned graphene-supported metal oxide monolith, wherein the electrode can be substantially free of any carbon-black and substantially free of any binder.

Synthesis and applications of crack-free SiO2 monolith containing CdSe/ZnS quantum dots as passive lighting sources.

PubMed

Yi, Dong Kee

2008-09-01

A reverse microemulsion technique has been used to synthesize quantum dot nanocomposites within a SiO2 surface coating. With this approach, the unique optical properties of the CdSe/ZnS quantum dots were preserved. CdSe/ZnS/SiO2 nanoparticles were homogeneously distributed in a tetramethyl orthosilicate ethanol solution and gelation process was initiated within a 10 min, and was left over night at room temperature and dried fully to achieve a solid SiO, monolith. The resulting monolith was transparent and fluorescent under ultraviolet (UV) lamp. Moreover the monolith produced was crack-free. Further studies on the photo stability of the monolith were performed using a high power UV LED device. Remarkably, quantum dots in the SiO, monolith showed better photo stability compared with those dispersed in a polymer matrix.

Monolithic in-based III-V compound semiconductor focal plane array cell with single stage CCD output

NASA Technical Reports Server (NTRS)

Fossum, Eric R. (Inventor); Cunningham, Thomas J. (Inventor); Krabach, Timothy N. (Inventor); Staller, Craig O. (Inventor)

1994-01-01

A monolithic semiconductor imager includes an indium-based III-V compound semiconductor monolithic active layer of a first conductivity type, an array of plural focal plane cells on the active layer, each of the focal plane cells including a photogate over a top surface of the active layer, a readout circuit dedicated to the focal plane cell including plural transistors formed monolithically with the monolithic active layer and a single-stage charge coupled device formed monolithically with the active layer between the photogate and the readout circuit for transferring photo-generated charge accumulated beneath the photogate during an integration period to the readout circuit. The photogate includes thin epitaxial semiconductor layer of a second conductivity type overlying the active layer and an aperture electrode overlying a peripheral portion of the thin epitaxial semiconductor layer, the aperture electrode being connectable to a photogate bias voltage.

Polarization cancellation in the two-component winds from Wolf-Rayet stars

NASA Technical Reports Server (NTRS)

Taylor, M.; Cassinelli, J. P.

1992-01-01

In this paper we explore the possibility that there can be at least partial cancellation of the equatorial disk polarization as a result of scattering from the electrons that are present in the strong polar wind of WR stars. In order to achieve the cancellation necessary to explain the wavelength-dependent polarization, the polar wind must have a mass-loss rate that is near the maximum that is supported by radiation-driven wind theory. In addition, we find that it is possible to derive important new information regarding the relative column masses of the polar and equatorial winds.

Crack-free polydimethylsiloxane-bioactive glass-poly(ethylene glycol) hybrid monoliths with controlled biomineralization activity and mechanical property for bone tissue regeneration.

PubMed

Chen, Jing; Du, Yuzhang; Que, Wenxiu; Xing, Yonglei; Chen, Xiaofeng; Lei, Bo

2015-12-01

Crack-free organic-inorganic hybrid monoliths with controlled biomineralization activity and mechanical property have an important role for highly efficient bone tissue regeneration. Here, biomimetic and crack-free polydimethylsiloxane (PDMS)-modified bioactive glass (BG)-poly(ethylene glycol) (PEG) (PDMS-BG-PEG) hybrids monoliths were prepared by a facile sol-gel technique. Results indicate that under the assist of co-solvents, BG sol and PDMS and PEG could be hybridized at a molecular level, and effects of the PEG molecular weight on the structure, biomineralization activity, and mechanical property of the as-prepared hybrid monoliths were also investigated in detail. It is found that an addition of low molecular weight PEG can significantly prevent the formation of cracks and speed up the gelation of the hybrid monoliths, and the surface microstructure of the hybrid monoliths can be changed from the porous to the smooth as the PEG molecular weight increases. Additionally, the hybrid monoliths with low molecular weight PEG show the high formation of the biological apatite layer, while the hybrids with high molecular weight PEG exhibit negligible biomineralization ability in simulated body fluid (SBF). Furthermore, the PDMS-BG-PEG 600 hybrid monolith has significantly high compressive strength (32 ± 3 MPa) and modulus (153 ± 11 MPa), as well as good cell biocompatibility by supporting osteoblast (MC3T3-E1) attachment and proliferation. These results indicate that the as-prepared PDMS-BG-PEG hybrid monoliths may have promising applications for bone tissue regeneration. Copyright © 2015 Elsevier B.V. All rights reserved.

Improvements in sparse matrix operations of NASTRAN

NASA Technical Reports Server (NTRS)

Harano, S.

1980-01-01

A "nontransmit" packing routine was added to NASTRAN to allow matrix data to be refered to directly from the input/output buffer. Use of the packing routine permits various routines for matrix handling to perform a direct reference to the input/output buffer if data addresses have once been received. The packing routine offers a buffer by buffer backspace feature for efficient backspacing in sequential access. Unlike a conventional backspacing that needs twice back record for a single read of one record (one column), this feature omits overlapping of READ operation and back record. It eliminates the necessity of writing, in decomposition of a symmetric matrix, of a portion of the matrix to its upper triangular matrix from the last to the first columns of the symmetric matrix, thus saving time for generating the upper triangular matrix. Only a lower triangular matrix must be written onto the secondary storage device, bringing 10 to 30% reduction in use of the disk space of the storage device.

Tracking the complex absorption in NGC 2110 with two Suzaku observations

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

Rivers, Elizabeth; Markowitz, Alex; Rothschild, Richard

2014-05-10

We present spectral analysis of two Suzaku observations of the Seyfert 2 galaxy, NGC 2110. This source has been known to show complex, variable absorption which we study in depth by analyzing these two observations set 7 yr apart and by comparing them to previously analyzed observations with the XMM-Newton and Chandra observatories. We find that there is a relatively stable, full-covering absorber with a column density of ∼3× 10{sup 22} cm{sup –2}, with an additional patchy absorber that is likely variable in both column density and covering fraction over timescales of years, consistent with clouds in a patchy torusmore » or in the broad line region. We model a soft emission line complex, likely arising from ionized plasma and consistent with previous studies. We find no evidence for reflection from an accretion disk in this source with contribution from neither relativistically broadened Fe Kα line emission, nor from a Compton reflection hump.« less

GaAs monolithic R.F. modules for SARSAT distress beacons

NASA Technical Reports Server (NTRS)

Cauley, Michael A.

1991-01-01

Monolithic GaAs UHF components for use in SARSAT Emergency Distress beacons are under development by Microwave Monolithics, Inc., Simi Valley, CA. The components include a bi-phase modulator, driver amplifier, and a 5 watt power amplifier.

GaAs monolithic RF modules for SARSAT distress beacons

NASA Technical Reports Server (NTRS)

Cauley, Michael A.

1991-01-01

Monolithic GaAs UHF components for use in SARSAT Emergency Distress beacons are under development by Microwave Monolithics, Inc., Simi Valley, CA. The components include a bi-phase modulator, driver amplifier, and a 5 watt power amplifier.

Monolithic Domes.

ERIC Educational Resources Information Center

Lanham, Carol

2002-01-01

Describes how the energy savings, low cost, and near-absolute protection from tornadoes provided by monolithic domes is starting to appeal to school districts for athletic and other facilities, including the Italy (Texas) Independent School District. Provides an overview of monolithic dome construction. (EV)

The FUSE Survey of Algol-Type Interacting Binary Systems

NASA Astrophysics Data System (ADS)

Peters, Geraldine J.; Andersson, B.; Ake, T. B.; Sankrit, R.

2006-12-01

A survey of Algol binaries at random phases is currently being carried through with the FUSE spacecraft as part of the FUSE survey and supplemental program. A similar program was undertaken in FUSE Cycle 3. Both programs have produced multiple observations of 12 Algol systems with periods ranging from 1.2 37 d and include direct-impact and disk systems. We report on the status of the program. The absence of O VI absorption in the systems observed to date allows us to place an upper limit on the column density and temperature of the High Temperature Accretion Region, HTAR ( 100,000 K) confirmed in some Algols from earlier IUE data. The HTAR plasma component appears to be distinct from an O VI-emitting polar plasma discovered in FUSE totality observations of RY Per, V356 Sgr, and TT Hya. New observations of the direct-impact system U Cep have provided more information on the geometry and mass flow (including a splash plasma) in the vicinity of a hot spot at phase 0.90 that was discovered earlier. The extent of disk asymmetries in the long period ( 33 d) systems SX Cas and RX Cas is discussed. Models for direct-impact and the disk systems will be presented. The authors appreciate support from NASA grants NAG5-12253, NNG04GL17G, and NAS5-32985.

Green analytical method development for statin analysis.

PubMed

Assassi, Amira Louiza; Roy, Claude-Eric; Perovitch, Philippe; Auzerie, Jack; Hamon, Tiphaine; Gaudin, Karen

2015-02-06

Green analytical chemistry method was developed for pravastatin, fluvastatin and atorvastatin analysis. HPLC/DAD method using ethanol-based mobile phase with octadecyl-grafted silica with various grafting and related-column parameters such as particle sizes, core-shell and monolith was studied. Retention, efficiency and detector linearity were optimized. Even for column with particle size under 2 μm, the benefit of keeping efficiency within a large range of flow rate was not obtained with ethanol based mobile phase compared to acetonitrile one. Therefore the strategy to shorten analysis by increasing the flow rate induced decrease of efficiency with ethanol based mobile phase. An ODS-AQ YMC column, 50 mm × 4.6 mm, 3 μm was selected which showed the best compromise between analysis time, statin separation, and efficiency. HPLC conditions were at 1 mL/min, ethanol/formic acid (pH 2.5, 25 mM) (50:50, v/v) and thermostated at 40°C. To reduce solvent consumption for sample preparation, 0.5mg/mL concentration of each statin was found the highest which respected detector linearity. These conditions were validated for each statin for content determination in high concentrated hydro-alcoholic solutions. Solubility higher than 100mg/mL was found for pravastatin and fluvastatin, whereas for atorvastatin calcium salt the maximum concentration was 2mg/mL for hydro-alcoholic binary mixtures between 35% and 55% of ethanol in water. Using atorvastatin instead of its calcium salt, solubility was improved. Highly concentrated solution of statins offered potential fluid for per Buccal Per-Mucous(®) administration with the advantages of rapid and easy passage of drugs. Copyright © 2014 Elsevier B.V. All rights reserved.