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Sample records for surfactant-bound monolithic columns

  1. Surfactant-bound monolithic columns for CEC.

    Science.gov (United States)

    Gu, Congying; He, Jun; Jia, Jinping; Fang, Nenghu; Shamsi, Shahab A

    2009-11-01

    A novel anionic surfactant bound monolithic stationary phase based on 11-acrylaminoundecanoic acid is designed for CEC. The monolith possessing bonded undecanoyl groups (hydrophobic sites) and carboxyl groups (weak cationic ion-exchange sites) were evaluated as a mixed-mode stationary phase in CEC for the separation of neutral and polar solutes. Using a multivariate D-optimal design the composition of the polymerization mixture was modeled and optimized with five alkylbenzenes and seven alkyl phenyl ketones as test solutes. The D-optimal design indicates a strong dependence of electrochromatographic parameters on the concentration of 11-acrylaminoundecanoic acid monomer and porogen (water) in the polymerization mixture. A difference of 6, 8 and 13% RSD between the predicted and the experimental values in terms of efficiency, resolution and retention time, respectively, indeed confirmed that the proposed approach is practical. The physical (i.e. morphology, porosity and permeability) and chromatographic properties of the monolithic columns were thoroughly investigated. With the optimized monolithic column, high efficiency separation of N-methylcarbamates pesticides and positional isomers was successfully achieved. It appears that this type of mixed-mode monolith (containing both chargeable and hydrophobic sites) may have a great potential as a new generation of CEC stationary phase.

  2. Surfactant-Bound Monolithic Columns for Capillary Electrochromatography

    Science.gov (United States)

    Gu, Congying; He, Jun; Jia, Jinping; Fang, Nenghu; Shamsi, Shahab A.

    2010-01-01

    A novel anionic surfactant bound monolithic stationary phase based on 11-acrylaminoundecanoic acid (AAUA) is designed for capillary electrochromatography (CEC). The monolith possessing bonded undecanoyl groups (hydrophobic sites) and carboxyl groups (weak cationic ion-exchange sites) was evaluated as a mixed-mode stationary phase in CEC for the separation of neutral and polar solutes. Using a multivariate D-optimal design the composition of the polymerization mixture was modeled and optimized with five alkylbenzenes (ABs) and seven alkyl phenyl ketones (APKs) as test solutes. The D-optimal design indicates a strong dependence of electrochromatographic parameters on the concentration of AAUA monomer and porogen (water) in the polymerization mixture. A difference of 6%, 8% and 13% RSD between the predicted and the experimental values in terms of efficiency, resolution, and retention time, respectively, indeed confirmed that the proposed approach is practical. The physical (i.e., morphology, porosity and permeability) and chromatographic properties of the monolithic columns were thoroughly investigated. With the optimized monolithic column, high efficiency separation of N-methylcarbamates (NMCs) pesticides and positional isomers was successfully achieved. It appears that this type of mixed-mode monolith (containing both chargeable and hydrophobic sites) may have a great potential as a new generation of CEC stationary phase. PMID:19885887

  3. Surfactant-bound monolithic columns for separation of proteins in capillary high performance liquid chromatography.

    Science.gov (United States)

    Gu, Congying; He, Jun; Jia, Jinping; Fang, Nenghu; Simmons, Robert; Shamsi, Shahab A

    2010-01-22

    A surfactant-bound monolithic stationary phase based on the co-polymerization of 11-acrylamino-undecanoic acid (AAUA) is designed for capillary high performance liquid chromatography (HPLC). Using D-optimal design, the effect of the polymerization mixture (concentrations of monomer, crosslinker and porogens) on the chromatographic performance (resolution and analysis time) of the AAUA-EDMA monolithic column was evaluated. The polymerization mixture was optimized using three proteins as model test solutes. The D-optimal design indicates a strong dependence of chromatographic parameters on the concentration of porogens (1,4-butanediol and water) in the polymerization mixture. Optimized solutions for fast separation and high resolution separation, respectively, were obtained using the proposed multivariate optimization. Differences less than 6.8% between the predicted and the experimental values in terms of resolution and retention time indeed confirmed that the proposed approach is practical. Using the optimized column, fast separation of proteins could be obtained in 2.5 min, and a tryptic digest of myoglobin was successfully separated on the high resolution column. The physical properties (i.e., morphology, porosity and permeability) of the optimized monolithic column were thoroughly investigated. It appears that this surfactant-bound monolith may have a great potential as a new generation of capillary HPLC stationary phase. Copyright 2009 Elsevier B.V. All rights reserved.

  4. Surfactant-Bound Monolithic Columns for Separation of Proteins in Capillary High Performance Liquid Chromatography

    Science.gov (United States)

    Gu, Congying; He, Jun; Jia, Jinping; Fang, Nenghu; Simmons, Robert; Shamsi, Shahab A.

    2011-01-01

    A surfactant bound monolithic stationary phase based on the co-polymerization of 11-acrylamino-undecanoic acid (AAUA) is designed for capillary high performance liquid chromatography (HPLC). Using D-optimal design, the effect of the polymerization mixture (concentrations of monomer, crosslinker and porogens) on the chromatographic performance (resolution and analysis time) of the AAUA-EDMA monolithic column was evaluated. The polymerization mixture was optimized using three proteins as model test solutes. The D-optimal design indicates a strong dependence of chromatographic parameters on the concentration of porogens (1,4-butanediol and water) in the polymerization mixture. Optimized solutions for fast separation and high resolution separation, respectively, were obtained using the proposed multivariate optimization. Differences less than 6.8% between the predicted and the experimental values in terms of resolution and retention time indeed confirmed that the proposed approach is practical. Using the optimized column, fast separation of proteins could be obtained in 2.5 min, and a tryptic digest of myoglobin was successfully separated on the high resolution column. The physical properties (i.e. morphology, porosity and permeability) of the optimized monolithic column were thoroughly investigated. It appears that this surfactant-bound monolith may have a great potential as a new generation of capillary HPLC stationary phase. PMID:20031139

  5. Monolithic column in gas chromatography.

    Science.gov (United States)

    Kurganov, A

    2013-05-02

    Monolithic columns invented in chromatographic praxis almost 40 years ago gained nowadays a lot of popularity in separations by liquid chromatographic technique. At the same time, application of monolithic columns in gas chromatography is less common and only a single review published by Svec et al. covers this field of research. Since that time a lot of new findings on application and properties of monolithic columns in gas chromatography have been published in the literature deserving consideration and discussion. This review considers preparation of monolithic columns for GC, an impact of preparation conditions on column performance, optimization of separation conditions for GC analysis on monolithic columns and other important aspects of preparation and usage of monolithic capillary columns in GC. A final part of the review discusses the modern trends and possible applications in the future of capillary monolithic columns in GC. Copyright © 2013 Elsevier B.V. All rights reserved.

  6. Preparation and application of hydrophilic monolithic columns.

    Science.gov (United States)

    Jiang, Zhengjin; Smith, Norman William; Liu, Zhenghua

    2011-04-29

    Hydrophilic interaction chromatography (HILIC) has experienced increasing attention in recent years. Much research has been carried out in the area of HILIC separation mechanisms, column techniques and applications. Because of their good permeability, low resistance to mass transfer and easy preparation within capillaries, hydrophilic monolithic columns represent a trend among novel HILIC column techniques. This review attempts to present an overview of the preparation and applications of HILIC monolithic columns carried out in the past decade. The separation mechanism of various hydrophilic monolithic stationary phases is also reviewed. Copyright © 2011 Elsevier B.V. All rights reserved.

  7. Optimization of monolithic columns for microfluidic devices

    Science.gov (United States)

    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.

  8. Applications of silica-based monolithic HPLC columns.

    Science.gov (United States)

    Cabrera, Karin

    2004-07-01

    The recent invention and successive commercial introduction of monolithic silica columns has motivated many scientists from both academia and industry to study their use in HPLC. The first paper on monolithic silica columns appeared in 1996. Currently about 200 papers have been published relating to applications and characterization of monolithic silica columns, including monolithic capillaries. This review attempts to give an overview covering various aspects of this new column type in the field of high throughput analysis of drugs and metabolites, chiral separations, analysis of pollutants and food-relevant compounds, as well as in bioanalytical separations such as in proteomics. Some of the applications are described in greater detail. The numerous publications dealing with the physicochemical and chromatographic characterization of monolithic silica columns are briefly summarized.

  9. Applications of monolithic silica capillary columns in proteomics

    NARCIS (Netherlands)

    Barroso, B.; Lubda, D; Bischoff, Rainer

    2003-01-01

    The use and applicability of silica based capillary monolithic reversed-phase columns in proteomic analysis has been evaluated by liquid chromatography-mass spectrometry (LC-MS). Chromatographic performance of the monolithic capillaries was evaluated with a tryptic digest of cytochrome C showing

  10. Microchip-based monolithic column for high performance liquid chromatography

    Data.gov (United States)

    National Aeronautics and Space Administration — We have developed microchip based monolithic columns that can be used for liquid chromatography of small organic molecules, as well as, macromolecules such as...

  11. Post-Polymerization Modifications of Polymeric Monolithic Columns: A Review

    Directory of Open Access Journals (Sweden)

    Sinéad Currivan

    2014-02-01

    Full Text Available The vast cache of methods used in polymeric monolithic column modification is presented herein, with specific attention to post-polymerization modification reactions. The modification of polymeric monolithic columns is defined and can include the modification of pre-existing surface groups, the addition of polymeric chains or indeed the addition of structures such as nano-particles and nano-structures. The use of these modifications can result in the specific patterning of monoliths, useful in microfluidic device design or in the investigation of modification optimization.

  12. Comparison of monolithic silica and polymethacrylate capillary columns for LC

    Czech Academy of Sciences Publication Activity Database

    Moravcová, D.; Jandera, P.; Urban, J.; Planeta, Josef

    2004-01-01

    Roč. 27, 10-11 (2004), s. 789-800 ISSN 1615-9306 R&D Projects: GA ČR(CZ) GA203/02/0023 Keywords : monolithic column s * capillary HPLC * column testing Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 1.927, year: 2004

  13. Methacrylate monolithic capillary columns for gradient peptide separations

    NARCIS (Netherlands)

    Pruim, P.; Öhman, M.; Huo, Y.; Schoenmakers, P.J.; Kok, W.Th.

    2008-01-01

    For the separation of peptides with gradient-elution liquid chromatography a poly(butyl methacrylate-co-ethylene dimethacrylate) (BMA) monolithic capillary column was prepared and tested. The conditional peak capacity was used as a metric for the performance of this column, which was compared with a

  14. Numerical Simulation of Fluid Dynamics in a Monolithic Column

    Directory of Open Access Journals (Sweden)

    Kazuhiro Yamamoto

    2017-01-01

    Full Text Available As for the measurement of polycyclic aromatic hydrocarbons (PAHs, ultra-performance liquid chromatography (UPLC is used for PAH identification and densitometry. However, when a solvent containing a substance to be identified passes through a column of UPLC, a dedicated high-pressure-proof device is required. Recently, a liquid chromatography instrument using a monolithic column technology has been proposed to reduce the pressure of UPLC. The present study tested five types of monolithic columns produced in experiments. To simulate the flow field, the lattice Boltzmann method (LBM was used. The velocity profile was discussed to decrease the pressure drop in the ultra-performance liquid chromatography (UPLC system.

  15. Cyclodextrin-Functionalized Monolithic Capillary Columns: Preparation and Chiral Applications.

    Science.gov (United States)

    Adly, Frady G; Antwi, Nana Yaa; Ghanem, Ashraf

    2016-02-01

    In this review, the recently reported approaches for the preparation of cyclodextrin-functionalized capillary monolithic columns are highlighted, with few applications in chiral separations using capillary liquid chromatography (CLC) and capillary electrochromatography (CEC). Chirality 28:97-109, 2016. © 2015 Wiley Periodicals, Inc. © 2015 Wiley Periodicals, Inc.

  16. Dopamine-imprinted monolithic column for capillary electrochromatography.

    Science.gov (United States)

    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.

  17. Monolithic and Small Particle Column Materials for Application in Proteomics

    NARCIS (Netherlands)

    Rozenbrand, J.

    2012-01-01

    In this thesis the influence of the capillary liquid chromatography separation on the identification of protein digests is studied. In the first part the chromatographic parameters for silica monolithic columns are optimized to obtain a high throughput or a high separation performance. in the second

  18. Silver-coated monolithic columns for separation in radiopharmaceutical applications.

    Science.gov (United States)

    Sedlacek, Ondrej; Kucka, Jan; Svec, Frantisek; Hruby, Martin

    2014-04-01

    In this study, we demonstrate the preparation of a macroporous monolithic column containing anchored silver nanoparticles and its use for the elimination of excess radioiodine from the radiolabeled pharmaceutical. The poly(glycidyl methacrylate-co-ethylene dimethacrylate) monolith was first functionalized with cystamine and the free thiol groups liberated by reaction with borohydride. In-house-prepared silver nanoparticles were then attached by interaction with the surface thiols. The deiodization process was demonstrated with the commonly used radiopharmaceutical m-iodobenzylguanidine labeled with radionuclide iodine-125. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. Ionic liquids monolithic columns for protein separation in capillary electrochromatography.

    Science.gov (United States)

    Liu, Cui-Cui; Deng, Qi-Liang; Fang, Guo-Zhen; Liu, Hui-Lin; Wu, Jian-Hua; Pan, Ming-Fei; Wang, Shuo

    2013-12-04

    A series of ionic liquids (ILs) monolithic capillary columns based on 1-vinyl-3-octylimidazolium (ViOcIm(+)) were prepared by two approaches ("one-pot" approach and "anion-exchange" approach). The effects of different anions (bromide, Br(-); tetrafluoroborate, BF4(-); hexafluorophosphate, PF6(-); and bis-trifluoromethanesulfonylimide, NTf2(-)) on chromatography performance of all the resulting columns were investigated systematically under capillary electrochromatography (CEC) mode. The results indicated that all these columns could generate a stable reversed electroosmotic flow (EOF) over a wide pH range from 2.0 to 12.0. For the columns prepared by "one-pot" approach, the EOF decreased in the order of ViOcIm(+)Br(-)>ViOcIm(+)BF4(-)>ViOcIm(+)PF6(-)>ViOcIm(+)NTf2(-) under the same CEC conditions; the ViOcIm(+)Br(-) based column exhibited highest column efficiencies for the test small molecules; the ViOcIm(+)NTf2(-) based column possessed the strongest retention for aromatic hydrocarbons; and baseline separation of four standard proteins was achieved on ViOcIm(+)NTf2(-) based column corresponding to the highest column efficiency of 479,000 N m(-1) for cytochrome c (Cyt c). These results indicated that the property of ILs based columns could be tuned successfully by changing anions, which gave these columns potential to separate both small molecules and macro biomolecules. Crown Copyright © 2013. Published by Elsevier B.V. All rights reserved.

  20. Short monolithic columns for purification and fractionation of peptide samples

    Czech Academy of Sciences Publication Activity Database

    Moravcová, Dana; Kahle, Vladislav; Řehulková, Helena; Chmelík, Jan; Řehulka, Pavel

    2009-01-01

    Roč. 1216, č. 17 (2009), s. 3629-3636 ISSN 0021-9673 R&D Projects: GA MŠk LC06023; GA MŠk 1M06030; GA ČR GA203/06/1179; GA AV ČR IAAX00310701 Institutional research plan: CEZ:AV0Z40310501 Keywords : proteomics * monolithic capillary columns * sample pre-treatment Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 4.101, year: 2009

  1. [Recent developments in preparation of monolithic columns and their applications in proteomic analysis].

    Science.gov (United States)

    Zou, Hanfa; Wu, Minghuo; Wang, Fangjun; Wu, Renan; Ye, Mingliang

    2009-09-01

    Monolithic column is a continuous unitary porous structure prepared by in-situ polymerization or consolidation inside the column tubing. Monolithic columns have been attracted great attention due to their simple preparation procedure, high permeability and high mass transfer rate. Big progress on the technology and methods for the preparation of monolithic columns and their applications to the highly efficient separation and pretreatment of biological samples have been made in last decade. This review summarizes the developments in the preparation of the monolithic columns and their applications to the proteomic analysis during the last five years.

  2. Evaluation of C18 monolithic columns for radiochemical purity measurement.

    Science.gov (United States)

    Schenk, David J; Welch, Christopher J; Antonucci, Vincent

    2016-08-01

    Speeding the analysis of reaction aliquots, high-performance liquid chromatography (HPLC) fractions and final products continue to be an area of great interest in the study of radiopharmaceuticals. Translating recently developed rapid HPLC and ultra high-performance liquid chromatography analysis approaches to radio-HPLC can sometimes be fraught with peril, owing to specific peculiarities of online radiochemical chromatographic detection (notably, a proportionally large system volume for the radio-HPLC detector). In this study, we investigate an alternate approach for rapid radio-HPLC analysis where a 150-cm C18 monolithic column is used with a 15-min run time. To ascertain this method's ability to distinguish between radiolabeled compounds with acceptable (≥97%) and unacceptable purity, the results were compared with results from a conventional HPLC 45-min method using a 25-cm C18 column, where a large radiodetector cell volume is of lower impact. Overall, for the 54 radiolabeled compounds assayed by the two methods, there were similar measured radiochemical purities, but cases were also found where there were significantly large differences between the results (>1%). A calculated confidence of ~85% was found for the 15-min monolithic method's ability to accurately reproduce the corresponding result from the 25-cm column method. Copyright © 2016 John Wiley & Sons, Ltd.

  3. A hybrid FIA/HPLC system incorporating monolithic column chromatography

    International Nuclear Information System (INIS)

    Adcock, Jacqui L.; Francis, Paul S.; Agg, Kent M.; Marshall, Graham D.; Barnett, Neil W.

    2007-01-01

    We have combined the generation of solvent gradients using milliGAT pumps, chromatographic separations with monolithic columns and chemiluminescence detection in an instrument manifold that approaches the automation and separation efficiency of HPLC, whilst maintaining the positive attributes of flow injection analysis (FIA), such as manifold versatility, speed of analysis and portability. As preliminary demonstrations of this hybrid FIA/HPLC system, we have determined six opiate alkaloids (morphine, pseudomorphine, codeine, oripavine, ethylmorphine and thebaine) and four biogenic amines (vanilmandelic acid, serotonin, 5-hydroxyindole-3-acetic acid and homovanillic acid) in human urine, using tris(2,2'-bipyridyl)ruthenium(III) and acidic potassium permanganate chemiluminescence detection

  4. Polymethacrylate Monolithic and Hybrid Particle-Monolithic Columns for Reversed-Phase and Hydrophilic Interaction Capillary Liquid Chromatography

    Czech Academy of Sciences Publication Activity Database

    Jandera, P.; Urban, J.; Škeříková, V.; Langmeier, P.; Kubíčková, R.; Planeta, Josef

    2010-01-01

    Roč. 1217, č. 1 (2010), s. 22-33 ISSN 0021-9673 R&D Projects: GA ČR GA203/08/1536 Institutional research plan: CEZ:AV0Z40310501 Keywords : particle-monolithic columns * hybrid columns * polymethacrylate monoliths * capillary HPLC * HILIC * proteins * phenolic acids Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 4.194, year: 2010

  5. Preparation and application of organic-silica hybrid monolithic capillary columns.

    Science.gov (United States)

    Wu, Minghuo; Wu, Ren'an; Zhang, Zhenbin; Zou, Hanfa

    2011-01-01

    Organic-silica hybrid monolithic columns have drawn more and more attention due to the ease of preparation and good mechanical stability in recent years. Many synthetic approaches have been developed and a variety of hybrid monolithic capillary columns have been prepared. The sol-gel process is well recognized in the fabrication of hybrid monolithic columns, which can be mainly classified as one-step, acid/base two-step procedures. The new approaches such as the "one-pot" and nano-scaled inorganic-organic hybrid reagent of polyhedral oligomeric silsesquioxane used as a cross-linker have also emerged for the preparation of hybrid monolithic columns. The applications of the organic-silica hybrid monolithic capillary columns for capillary electrochromatography, micro high-performance liquid chromatography, solid-phase micro-extraction and enzymatic reactor etc. are included in this review. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Separation of intact proteins by using polyhedral oligomeric silsesquioxane based hybrid monolithic capillary columns.

    Science.gov (United States)

    Liu, Zheyi; Ou, Junjie; Liu, Zhongshan; Liu, Jing; Lin, Hui; Wang, Fangjun; Zou, Hanfa

    2013-11-22

    High-efficient separation of intact proteins is still a huge challenge in proteome analysis of complex biological samples by using capillary columns. In this study, four POSS-based hybrid monolithic capillary columns were prepared and applied in nano-flow liquid chromatography (Nano-LC) separation of intact proteins. It was observed that the POSS-based hybrid monolithic columns exhibit high permeability, good LC separation reproducibility and column efficiency for intact protein separation. The effects of different LC separation conditions such as flow rate, gradient steepness, column length and mobile phase additives on the LC separation efficiency of the POSS-based hybrid monolithic column were systematically examined. Finally, fast LC separation of 7 proteins mixture was realized in 2.5 min by using the optimized conditions on the 100 μm i.d. POSS-based hybrid monolithic capillary column. Copyright © 2013. Published by Elsevier B.V.

  7. [Preparation of divinylbenzene polymer monolithic columns and their applications in gas chromatography].

    Science.gov (United States)

    Tian, Hongxu; Li, Yun; Chen, Jiping

    2010-11-01

    The preparation of divinylbenzene polymer monolithic columns and their applications in gas chromatography (GC) are discussed. Based on liquid chromatographic (LC) monolithic columns, the high-permeable monolithic columns can be applied in GC through changing the ratio of toluene and dodecanol. It is shown that the monolithic columns possess fastness configuration and good mechanical intensity via the bonding of 3-(trimethoxysilyl) propyl methacrylate (TMP) to the capillary wall and the polymerization of the crosslinker itself. Compared with a commercial porous layer open tube (PLOT) column and a PEG-20M column, the monolithic columns demonstrate good performance in the analysis of low carbon alcohols in water, the analysis of mixed solvents and the standard liquor sample. In the mixed solvents, the peak symmetries of alcohols, ketones, esters and aromatics precede those on the PLOT column. The separation of methanol, acetaldehyde and ethyl acetate in the standard liquor sample on the monolithic column is much more convenient than that on PEG-20M columns.

  8. Comparing monolithic and fused core HPLC columns for fast chromatographic analysis of fat-soluble vitamins.

    Science.gov (United States)

    Kurdi, Said El; Muaileq, Dina Abu; Alhazmi, Hassan A; Bratty, Mohammed Al; Deeb, Sami El

    2017-06-27

    HPLC stationary phases of monolithic and fused core type can be used to achieve fast chromatographic separation as an alternative to UPLC. In this study, monolithic and fused core stationary phases are compared for fast separation of four fat-soluble vitamins. Three new methods on the first and second generation monolithic silica RP-18e columns and a fused core pentafluoro-phenyl propyl column were developed. Application of three fused core columns offered comparable separations of retinyl palmitate, DL-α-tocopheryl acetate, cholecalciferol and menadione in terms of elution speed and separation efficiency. Separation was achieved in approx. 5 min with good resolution (Rs > 5) and precision (RSD ≤ 0.6 %). Monolithic columns showed, however, a higher number of theoretical plates, better precision and lower column backpressure than the fused core column. The three developed methods were successfully applied to separate and quantitate fat-soluble vitamins in commercial products.

  9. Comparing monolithic and fused core HPLC columns for fast chromatographic analysis of fat-soluble vitamins

    Directory of Open Access Journals (Sweden)

    Kurdi Said El

    2017-06-01

    Full Text Available HPLC stationary phases of monolithic and fused core type can be used to achieve fast chromatographic separation as an alternative to UPLC. In this study, monolithic and fused core stationary phases are compared for fast separation of four fat-soluble vitamins. Three new methods on the first and second generation monolithic silica RP-18e columns and a fused core pentafluoro-phenyl propyl column were developed. Application of three fused core columns offered comparable separations of retinyl palmitate, DL-α-tocopheryl acetate, cholecalciferol and menadione in terms of elution speed and separation efficiency. Separation was achieved in approx. 5 min with good resolution (Rs > 5 and precision (RSD ≤ 0.6 %. Monolithic columns showed, however, a higher number of theoretical plates, better precision and lower column backpressure than the fused core column. The three developed methods were successfully applied to separate and quantitate fat-soluble vitamins in commercial products.

  10. [Preparation of chiral monolithic column with covalently bonded cellulose and their application to rapid enantioseparation].

    Science.gov (United States)

    Wang, Jiabin; Wang, Xiao; Li, Jianhua; Lü, Haixia; Lin, Xucong; Xie, Zenghong; Zhang, Qiqing

    2011-12-01

    A chiral monolithic capillary column for rapid enantioseparation was prepared by covalently bonding of cellulose tris(4-methylbenzoate) (CTMB) on N-acryloxysuccinimide-based monolith. The preparation and derivatization conditions of the monolithic column were optimized. The successful grafting of CTMB was confirmed on the characterizations of the infrared spectrum and the cathodic electroosmotic flow (EOF). The effects of acetic acid concentration and methanol content on the enantioseparation were studied. The solvent resistance, reproducibility and stability of the monolithic column have also been investigated. The rapid enantioseparation of the five solutes (phenylalanine, tyrosine, tryptophan, propranolol and phenylethanol) with resolution (R(s)) values up to 1.31 was achieved within 1.2 min on the prepared chiral capillary monolithic column by capillary electrochromatography.

  11. Applications of monolithic columns in liquid chromatography-based clinical chemistry assays.

    Science.gov (United States)

    Bunch, Dustin R; Wang, Sihe

    2011-08-01

    Monolithic columns have slowly been applied to HPLC methods for clinical chemistry testing in the last 10 years. The application areas include therapeutic drug monitoring, drugs of abuse, vitamins, porphyrins, and steroids. In comparison with conventional particulate columns, the monolithic columns may offer shorter chromatography time, more robustness, and better resolution for certain analytes. The potential drawback of large mobile phase consumption may be improved with smaller id columns, which are currently on the market. Methods covered in this review are those searchable in PubMed up to December 2010. This review highlights the emergence of monolithic column technology in HPLC methods used for clinical chemistry testing. The goals of this review are threefold: (i) To identify the areas of clinical chemistry that analytical monolithic columns have been used in HPLC methods. (ii) To demonstrate the application of analytical monolithic columns in HPLC methods using different detection systems. (iii) To discuss the advantages and limitations of the monolithic columns compared with particulate columns in the clinical chemistry applications. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. Investigating the Effect of Column Geometry on Separation Efficiency using 3D Printed Liquid Chromatographic Columns Containing Polymer Monolithic Phases.

    Science.gov (United States)

    Gupta, Vipul; Beirne, Stephen; Nesterenko, Pavel N; Paull, Brett

    2018-01-16

    Effect of column geometry on the liquid chromatographic separations using 3D printed liquid chromatographic columns with in-column polymerized monoliths has been studied. Three different liquid chromatographic columns were designed and 3D printed in titanium as 2D serpentine, 3D spiral, and 3D serpentine columns, of equal length and i.d. Successful in-column thermal polymerization of mechanically stable poly(BuMA-co-EDMA) monoliths was achieved within each design without any significant structural differences between phases. Van Deemter plots indicated higher efficiencies for the 3D serpentine chromatographic columns with higher aspect ratio turns at higher linear velocities and smaller analysis times as compared to their counterpart columns with lower aspect ratio turns. Computational fluid dynamic simulations of a basic monolithic structure indicated 44%, 90%, 100%, and 118% higher flow through narrow channels in the curved monolithic configuration as compared to the straight monolithic configuration at linear velocities of 1, 2.5, 5, and 10 mm s -1 , respectively. Isocratic RPLC separations with the 3D serpentine column resulted in an average 23% and 245% (8 solutes) increase in the number of theoretical plates as compared to the 3D spiral and 2D serpentine columns, respectively. Gradient RPLC separations with the 3D serpentine column resulted in an average 15% and 82% (8 solutes) increase in the peak capacity as compared to the 3D spiral and 2D serpentine columns, respectively. Use of the 3D serpentine column at a higher flow rate, as compared to the 3D spiral column, provided a 58% reduction in the analysis time and 74% increase in the peak capacity for the isocratic separations of the small molecules and the gradient separations of proteins, respectively.

  13. Recent advances in the preparation and application of monolithic capillary columns in separation science

    Energy Technology Data Exchange (ETDEWEB)

    Hong, Tingting; Yang, Xi; Xu, Yujing [Department of Analytical Chemistry, China Pharmaceutical University, Nanjing, 210009 (China); Key Laboratory of Drug Quality Control and Pharmacovigilance, Ministry of Education, Nanjing, 210009 (China); Ji, Yibing, E-mail: jiyibing@msn.com [Department of Analytical Chemistry, China Pharmaceutical University, Nanjing, 210009 (China); Key Laboratory of Drug Quality Control and Pharmacovigilance, Ministry of Education, Nanjing, 210009 (China)

    2016-08-10

    Novel column technologies involving various materials and efficient reactions have been investigated for the fabrication of monolithic capillary columns in the field of analytical chemistry. In addition to the development of these miniaturized systems, a variety of microscale separation applications have achieved noteworthy results, providing a stepping stone for new types of chromatographic columns with improved efficiency and selectivity. Three novel strategies for the preparation of capillary monoliths, including ionic liquid-based approaches, nanoparticle-based approaches and “click chemistry”, are highlighted in this review. Furthermore, we present the employment of state-of-the-art capillary monolithic stationary phases for enantioseparation, solid-phase microextraction, mixed-mode separation and immobilized enzyme reactors. The review concludes with recommendations for future studies and improvements in this field of research. - Highlights: • Preparation of novel monolithic capillary columns have shown powerful potential in analytical chemistry field. • Various materials including ionic liquids and nanoparticles involved into capillary monolithic micro-devices are concluded. • Click chemistry strategy applied for preparing monolithic capillary columns is reviewed. • Recent strategies utilized in constructing different capillary monoliths for enantiomeric separation are summarized. • Advancement of capillary monoliths for complex samples analysis is comprehensively described.

  14. Preparation and application of novel zwitterionic monolithic column for hydrophilic interaction chromatography.

    Science.gov (United States)

    Liu, Zhenghua; Peng, Yongbo; Wang, Tingting; Yuan, Guangxin; Zhang, Qiaoxuan; Guo, Jialiang; Jiang, Zhengjin

    2013-01-01

    A novel zwitterionic hydrophilic porous monolithic stationary phase was prepared based on the thermal-initiated copolymerization of N,N-dimethyl-N-(3-methacryl-amidopropyl)-N-(3-(sulfopropyl)ammonium betaine and ethylene glycol dimethacrylate. A typical hydrophilic separation mechanism was observed at a highly organic mobile phase (ACN >60%) on this optimized zwitterionic hydrophilic interaction chromatography (HILIC) monolithic stationary phase. Good permeability, stability, and column efficiency were observed on the final monolithic column. Additionally, a weak electrostatic interaction for charged analytes was confirmed in analysis of six benzoic acids by studying the influence of mobile phase pH and salt concentration on their retention behaviors on the obtained zwitterionic HILIC monolithic column. The optimized zwitterionic HILIC monolith exhibited good selectivity for a range of polar test analytes. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Methacrylate monolithic columns functionalized with epinephrine for capillary electrochromatography applications.

    Science.gov (United States)

    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.

  16. Preparation of organic monolithic columns in polytetrafluoroethylene tubes for reversed-phase liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Catalá-Icardo, M., E-mail: mocaic@qim.upv.es [Research Institute for Integrated Management of Coastal Areas, Universitat Politècnica de València, Paranimf 1, 46730, Grao de Gandía, Valencia (Spain); Torres-Cartas, S.; Meseguer-Lloret, S.; Gómez-Benito, C. [Research Institute for Integrated Management of Coastal Areas, Universitat Politècnica de València, Paranimf 1, 46730, Grao de Gandía, Valencia (Spain); Carrasco-Correa, E.; Simó-Alfonso, E.F.; Ramis-Ramos, G. [Department of Analytical Chemistry, Universitat de València, Dr. Moliner 50, 46100, Burjassot, Valencia (Spain); Herrero-Martínez, J.M., E-mail: jmherrer@uv.es [Department of Analytical Chemistry, Universitat de València, Dr. Moliner 50, 46100, Burjassot, Valencia (Spain)

    2017-04-01

    In this work, a method for the preparation and anchoring of polymeric monoliths in a polytetrafluoroethylene (PTFE) tubing as a column housing for microbore HPLC is described. In order to assure a covalent attachment of the monolith to the inner wall of the PTFE tube, a two-step procedure was developed. Two surface etching reagents, a commercial sodium naphthalene solution (Fluoroetch{sup ®}), or mixtures of H{sub 2}O{sub 2} and H{sub 2}SO{sub 4}, were tried and compared. Then, the obtained hydroxyl groups on the PTFE surface were modified by methacryloylation. Attenuated total reflectance Fourier-transform infrared (ATR-FTIR) spectroscopy and scanning electron microscopy (SEM) confirmed the successful modification of the tubing wall and the stable anchorage of monolith to the wall, respectively. Special emphasis was also put on the reduction of the unwanted effects of shrinking of monolith during polymerization, by using an external proper mold and by selecting the adequate monomers in order to increase the flexibility of the polymer. Poly(glycidyl methacrylate-co-divinylbenzene) monoliths were in situ synthesized by thermal polymerization within the confines of surface-vinylized PTFE tubes. The modified PTFE tubing tightly held the monolith, and the monolithic column exhibited good pressure resistance up to 20 MPa. The column performance was also evaluated via the isocratic separation of a series of alkylbenzenes in the reversed-phase mode. The optimized monolithic columns gave plate heights ranged between 70 and 80 μm. The resulting monoliths were also satisfactorily applied to the separation of proteins. - Highlights: • Successful surface etching of PTFE inner wall tubing was done. • The modified PTFE support was next methacryloylated with GMA. • Organic polymeric monolith was in situ prepared in the functionalized PTFE tube. • The monolithic columns gave suitable pressure resistance and separation of proteins.

  17. Temperature control in large-internal-diameter scaffolded monolithic columns operated at ultra-high pressures

    NARCIS (Netherlands)

    Vonk, R.J.; Aalbers, T.; Eeltink, S.; Schoenmakers, P.J.

    2015-01-01

    Scaffolding makes it feasible to create organic-polymer monoliths in large confinements, such as wide-bore columns. By creating the scaffold from a metal good heat conductivity inside the column is obtained, which renders the relatively large columns (comparable with 4.6 mm id.) suitable for

  18. A Butyl Methacrylate Monolithic Column Prepared In-Situ on a Microfluidic Chip and its Applications

    Directory of Open Access Journals (Sweden)

    Qiang Cao

    2009-05-01

    Full Text Available A butyl methacrylate (BMA monolithic column was polymerized in-situ with UV irradiation in an ultraviolet transparent PDMS micro-channel on a homemade micro-fluidic chip. Under the optimized conditions and using a typical polymerization mixture consisting of 75% porogenic solvents and 25% monomers, the BMA monolithic column was obtained as expected. The BET surface area ratio of the BMA monolithic column was 366 m2·g-1. The corresponding SEM images showed that the monolithic column material polymerized in a glass channel was composed of uniform pores and spherical particles with diameters ranging from 3 to 5 μm. The promethazine–luminal–potassium ferricyanide chemiluminescence system was selected for testing the capability of the column. A flow injection analytical technique–chemiluminescence (FIA–CL system on the microfluidic chip with a BMA monolithic column pretreatment unit was established to determine promethazine. Trace promethazine was enriched by the BMA monolithic column, with more than a 10-fold average enrichment ratio. The proposed method has a linear response concentration range of 1.0×10-8 - 1.0×10-6g·mL-1 and the detection limit was 1.6×10-9g·mL-1.

  19. A butyl methacrylate monolithic column prepared in-situ on a microfluidic chip and its applications.

    Science.gov (United States)

    Xu, Yi; Zhang, Wenpin; Zeng, Ping; Cao, Qiang

    2009-01-01

    A butyl methacrylate (BMA) monolithic column was polymerized in-situ with UV irradiation in an ultraviolet transparent PDMS micro-channel on a homemade micro-fluidic chip. Under the optimized conditions and using a typical polymerization mixture consisting of 75% porogenic solvents and 25% monomers, the BMA monolithic column was obtained as expected. The BET surface area ratio of the BMA monolithic column was 366 m(2)·g(-1). The corresponding SEM images showed that the monolithic column material polymerized in a glass channel was composed of uniform pores and spherical particles with diameters ranging from 3 to 5 μm. The promethazine-luminal-potassium ferricyanide chemiluminescence system was selected for testing the capability of the column. A flow injection analytical technique-chemiluminescence (FIA-CL) system on the microfluidic chip with a BMA monolithic column pretreatment unit was established to determine promethazine. Trace promethazine was enriched by the BMA monolithic column, with more than a 10-fold average enrichment ratio. The proposed method has a linear response concentration range of 1.0×10(-8) - 1.0×10(-6)g·mL(-1) and the detection limit was 1.6×10(-9)g·mL(-1).

  20. A Butyl Methacrylate Monolithic Column Prepared In-Situ on a Microfluidic Chip and its Applications

    Science.gov (United States)

    Xu, Yi; Zhang, Wenpin; Zeng, Ping; Cao, Qiang

    2009-01-01

    A butyl methacrylate (BMA) monolithic column was polymerized in-situ with UV irradiation in an ultraviolet transparent PDMS micro-channel on a homemade micro-fluidic chip. Under the optimized conditions and using a typical polymerization mixture consisting of 75% porogenic solvents and 25% monomers, the BMA monolithic column was obtained as expected. The BET surface area ratio of the BMA monolithic column was 366 m2·g-1. The corresponding SEM images showed that the monolithic column material polymerized in a glass channel was composed of uniform pores and spherical particles with diameters ranging from 3 to 5 μm. The promethazine–luminal–potassium ferricyanide chemiluminescence system was selected for testing the capability of the column. A flow injection analytical technique–chemiluminescence (FIA–CL) system on the microfluidic chip with a BMA monolithic column pretreatment unit was established to determine promethazine. Trace promethazine was enriched by the BMA monolithic column, with more than a 10-fold average enrichment ratio. The proposed method has a linear response concentration range of 1.0×10-8 - 1.0×10-6g·mL-1 and the detection limit was 1.6×10-9g·mL-1. PMID:22412320

  1. Behavior of macroporous vinyl silica and silica monolithic columns in high pressure gas chromatography.

    Science.gov (United States)

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

    2017-06-30

    80% vinyltrimethoxysilane-based hybrid silica monoliths (80-VTMS), which have been initially developed for separation in reversed-phase liquid chromatography, have been investigated in high pressure gas chromatography separations (carrier gas pressure up to 60bar) and compared to silica monolithic columns. The behavior of both silica and 80-VTMS monolithic columns was investigated using helium, nitrogen and carbon dioxide as carrier gas. The efficiency of 80-VTMS monolithic columns was shown to vary differently than silica monolithic columns according to the temperature and the carrier gas used. Carrier gas nature was a significant parameter on the retention for both silica and vinyl columns in relation to its adsorption onto the stationary phase in such high pressure conditions. The comparison of retention and selectivity between 80-VTMS monoliths and silica was performed under helium using the logarithm of the retention factor according to the number of carbon atoms combined to Kovats indexes. The very good performances of these columns were demonstrated, allowing the separation of 8 compounds in less than 1min. Copyright © 2017 Elsevier B.V. All rights reserved.

  2. P61-S Multidimensional Liquid Chromatography of Proteins Using Monolithic Weak Anion Exchange and Reversed-Phase Columns

    OpenAIRE

    Sneekes, E.; van Ling, R.; de Haan, B.; Dolman, B.; Swart, R.; van Gils, M.

    2007-01-01

    Recent developments in monolithic column technology have yielded significant improvements in the biopolymer analysis field. Monolithic columns offer several advantages over particulate columns due to their macroporous structure, which provides fast mass transfer, low back pressure and high resolution. Polystyrene divinylbenzene (PS-DVB) monolithic columns are chemically inert; they offer high pH stability and excellent chromatographic performance in reversed-phase LC. While the application of...

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

    Science.gov (United States)

    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.

  4. Monolithic columns with immobilized monomeric avidin: preparation and application for affinity chromatography.

    Science.gov (United States)

    Spross, Jens; Sinz, Andrea

    2012-03-01

    A poly(glycidyl methacrylate-co-acrylamide-co-ethylene dimethacrylate) monolith and a poly(glycidyl methacrylate-co-ethylene dimethacrylate) monolith were prepared in fused silica capillaries (100 μm ID) and modified with monomeric avidin using the glutaraldehyde technique. The biotin binding capacity of monolithic affinity columns with immobilized monomeric avidin (MACMAs) was determined by fluorescence spectroscopy using biotin (5-fluorescein) conjugate, as well as biotin- and fluorescein-labeled bovine serum albumin (BSA). The affinity columns were able to bind 16.4 and 3.7 μmol biotin/mL, respectively. Columns prepared using the poly(glycidyl methacrylate-co-ethylene dimethacrylate) monolith retained 7.1 mg BSA/mL, almost six times more than commercially available monomeric avidin beads. Protocols based on MALDI-TOF mass spectrometry monitoring were optimized for the enrichment of biotinylated proteins and peptides. A comparison of enrichment efficiencies between MACMAs and commercially available monomeric avidin beads yielded superior results for our novel monolithic affinity columns. However, the affinity medium presented in this work suffers from a significant degree of nonspecific binding, which might hamper the analysis of more complex mixtures. Further modifications of the monolith's surface are envisaged for the future development of monoliths with improved enrichment characteristics.

  5. Highly stable surface modification of hypercrosslinked monolithic capillary columns and their application in hydrophilic interaction chromatography.

    Science.gov (United States)

    Škeříková, Veronika; Urban, Jiří

    2013-09-01

    A two-step surface modification of poly(styrene-co-vinylbenzyl chloride-co-divinylbenzene) monolithic stationary phases, including hypercrosslinking and thermally initiated surface grafting of [2-(methacryloyloxy)ethyl]dimethyl(3-sulfopropyl)ammonium hydroxide, has been used to prepare capillary columns for the isocratic separation of small polar compounds in hydrophilic interaction chromatography (HILIC). The prepared monolithic columns provided a dual retention mechanism, combining RP and hydrophilic interaction chromatography, controlled by the composition of the mobile phase. By the optimization of the surface grafting reaction using response surface methodology, we have found that the grafting time is the main synergistic effect controlling the retention of polar compounds in HILIC. The prepared monolithic columns achieved long column lifetimes and did not lose their separation power following >10,000 injections. Finally, hypercrosslinked columns have been used in the 1- and 2D LC of phenolic compounds. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. A novel ionic liquid monolithic column and its separation properties in capillary electrochromatography.

    Science.gov (United States)

    Wang, Yu; Deng, Qi-Liang; Fang, Guo-Zhen; Pan, Ming-Fei; Yu, Yang; Wang, Shuo

    2012-01-27

    A novel ionic liquid (IL) monolithic capillary column was successfully prepared by thermal free radical copolymerization of IL (1-vinyl-3-octylimidazolium chloride, ViOcIm(+)Cl(-)) together with lauryl methacrylate (LMA) as the binary functional monomers and ethylene dimethacrylate (EDMA) as the cross-linker in binary porogen. The proportion of monomers, porogens and cross-linker in the polymerization mixture was optimized in detail. The resulting IL-monolithic column could not only generate a stable reversed electroosmotic flow (EOF) in a wide pH range (2.0-12.0), but also effectively eliminate the wall adsorption of the basic analytes. The obtained IL-monolithic columns were examined by scanning electron microscopy (SEM) and Fourier transform infrared (FT-IR). These results indicated that the IL-monolithic capillary column possessed good pore properties, mechanical stability and permeability. The column performance was also evaluated by separating different kinds of compounds, such as alkylbenzenes, thiourea and its analogues, and amino acids. The lowest plate height of ~6.8 μm was obtained, which corresponded to column efficiency (theoretical plates, N) of ~147,000 plates m(-1) for thiourea. ILs, as a new type of functional monomer, present a promising option in the fabrication of the organic polymer-based monolithic columns in CEC. Copyright © 2011 Elsevier B.V. All rights reserved.

  7. [Preparation and application of mixed-mode capillary polymer monolithic column].

    Science.gov (United States)

    Dou, Abo; Zou, Cunjie; Shan, Yuanhong; Shi, Xianzhe; Xu, Guowang

    2014-05-01

    Based on the diversity of the retention mechanism, mixed-mode capillary monolithic columns have broad application prospect. In this work, a novel capillary polymer monolithic column was prepared with [2-(methacryloyloxy) ethyl] dimethyl-(3-sulfopropyl) ammonium hydroxide (SPE) as monomer, ethylene dimethacrylate (EDMA) as crosslinking agent, azobisisobutyronitrile (AIBN) as initiator and butylalcohol/1, 4-butanediol/water as ternary porogens. Under the optimized reaction conditions including the proportion of monomer and porogens, amount of initiator, reaction temperature and polymerization time, the monolithic column showed good mechanical strength up to 10 MPa, high permeability of 2. 17 x 10(-14) m2 and good repeatability. The peak area RSDs of column-to-column and batch-to-batch reproducibility were 1.0% and 4.6%, respectively. Finally, the capillary monolithic column was evaluated with polar and non-polar test mixtures. It showed hydrophilic interaction under high organic phase while hydrophobic interaction under low organic phase, indicating it a mixed-mode monolithic column.

  8. Application of a Fast Separation Method for Anti-diabetics in Pharmaceuticals Using Monolithic Column: Comparative Study With Silica Based C-18 Particle Packed Column.

    Science.gov (United States)

    Hemdan, A; Abdel-Aziz, Omar

    2018-04-01

    Run time is a predominant factor in HPLC for quality control laboratories especially if there is large number of samples have to be analyzed. Working at high flow rates cannot be attained with silica based particle packed column due to elevated backpressure issues. The use of monolithic column as an alternative to traditional C-18 column was tested for fast separation of pharmaceuticals, where the results were very competitive. The performance comparison of both columns was tested for separation of anti-diabetic combination containing Metformin, Pioglitazone and Glimepiride using Gliclazide as an internal standard. Working at high flow rates with less significant backpressure was obtained with the monolithic column where the run time was reduced from 6 min in traditional column to only 1 min in monolithic column with accepted resolution. The structure of the monolith contains many pores which can adapt the high flow rate of the mobile phase. Moreover, peak symmetry and equilibration time were more efficient with monolithic column.

  9. Preparation and characterization of alkyl methacrylate-based monolithic columns for capillary gas chromatography applications.

    Science.gov (United States)

    Yusuf, Kareem; Aqel, Ahmad; A L Othman, Zeid; Badjah-Hadj-Ahmed, Ahmed Yacine

    2013-08-02

    Gas chromatography (GC) is considered the least common application of both polymer and silica-based monolithic columns. This study describes the fabrication of alkyl methacrylate monolithic materials for use as stationary phases in capillary gas chromatography. Following the deactivation of the capillary surface with 3-(trimethoxysilyl)propyl methacrylate (TMSM), the monoliths were formed by the co-polymerization of either hexyl methacrylate (HMA) or lauryl methacrylate (LMA) with different percentage of ethylene glycol dimethacrylate (EDMA) in presence of an initiator (azobisisobutyronitrile, AIBN) and a mixture of porogens include 1-propanol, 1,4-butanediol and water. The monoliths were prepared in 500mm length capillaries possessing inner diameters of 250μm. The efficiencies of the monolithic columns for low molecular weight compounds significantly improved as the percentage of crosslinker was increased, because of the greater proportion of pores less than 50nm. The columns containing lower percentages of crosslinker were able to rapidly separate a series of 8 alkane members in 0.7min, but the separation was less efficient for the light alkanes. Columns prepared with the lauryl methacrylate monomer yielded a different morphology for the monolith-interconnected channels. The channels were more branched, which increased the separation time, and unlike the other columns, allowed for temperature programming. Copyright © 2013 Elsevier B.V. All rights reserved.

  10. A novel ionic liquid monolithic column and its separation properties in capillary electrochromatography

    International Nuclear Information System (INIS)

    Wang Yu; Deng Qiliang; Fang Guozhen; Pan Mingfei; Yu Yang; Wang Shuo

    2012-01-01

    Highlights: ► ILs as functional monomer for capillary monolithic column. ► Separation of alkylbenzenes, thiourea analogues, and amino acids. ► The column generate a stable reversed EOF from pH 2.0 to 12.0. ► The column efficiency of 147,000 plates m −1 was obtained for thiourea. - Abstract: A novel ionic liquid (IL) monolithic capillary column was successfully prepared by thermal free radical copolymerization of IL (1-vinyl-3-octylimidazolium chloride, ViOcIm + Cl − ) together with lauryl methacrylate (LMA) as the binary functional monomers and ethylene dimethacrylate (EDMA) as the cross-linker in binary porogen. The proportion of monomers, porogens and cross-linker in the polymerization mixture was optimized in detail. The resulting IL-monolithic column could not only generate a stable reversed electroosmotic flow (EOF) in a wide pH range (2.0–12.0), but also effectively eliminate the wall adsorption of the basic analytes. The obtained IL-monolithic columns were examined by scanning electron microscopy (SEM) and Fourier transform infrared (FT-IR). These results indicated that the IL-monolithic capillary column possessed good pore properties, mechanical stability and permeability. The column performance was also evaluated by separating different kinds of compounds, such as alkylbenzenes, thiourea and its analogues, and amino acids. The lowest plate height of ∼6.8 μm was obtained, which corresponded to column efficiency (theoretical plates, N) of ∼147,000 plates m −1 for thiourea. ILs, as a new type of functional monomer, present a promising option in the fabrication of the organic polymer-based monolithic columns in CEC.

  11. Robust naphthyl methacrylate monolithic column for high performance liquid chromatography of a wide range of solutes.

    Science.gov (United States)

    Jonnada, Murthy; El Rassi, Ziad

    2015-08-28

    An organic monolithic column based on the co-polymerization of 2-naphthyl methacrylate (NAPM) as the functional monomer and trimethylolpropane trimethacrylate (TRIM) as the crosslinker was introduced for high performance reversed-phase liquid chromatography (RPC). The co-polymerization was performed in situ in a stainless steel column of 4.6mm i.d. in the presence of a ternary porogen consisting of 1-dodecanol and cyclohexanol. This monolithic column (referred to as naphthyl methacrylate monolithic column or NMM column) showed high mechanical stability at relatively high mobile phase flow velocity indicating that the column has excellent hydrodynamic characteristics. To characterize the NMM column, different probe molecules including alkyl benzenes, and aniline, benzene, toluene and phenol derivatives were chromatographed on the column and the results in terms of k, selectivity and plate counts were compared to those obtained on an octadecyl silica (ODS) column in order to assess the presence of π-π and hydrophobic interactions on the NMM column under otherwise the same elution conditions. The NMM column offered additional π-π interactions with aromatic molecules in addition to hydrophobic interactions under RPC elution conditions. Run-to-run and column-to-column reproducibility of solute k values were evaluated, and percent relative standard deviation of column using shallow (30min at 1.0mL/min), steep (10min at 1.0mL/min) and ultra steep (1min at 3.0mL/min) linear gradient elution at increasing ACN concentration in the mobile phase using a 10cm×4.6mm i.d. column in case of shallow and steep linear gradients and a 3cm×4.6mm i.d. column for ultra steep linear gradient. Copyright © 2015 Elsevier B.V. All rights reserved.

  12. Recent Advances and Uses of Monolithic Columns for the Analysis of Residues and Contaminants in Food

    Directory of Open Access Journals (Sweden)

    Mónica Díaz-Bao

    2015-02-01

    Full Text Available Monolithic columns are gaining interest as excellent substitutes to conventional particle-packed columns. These columns show higher permeability and lower flow resistance than conventional liquid chromatography columns, providing high-throughput performance, resolution and separation in short run times. Monoliths possess also great potential for the clean-up and preparation of complex mixtures. In situ polymerization inside appropriate supports allows the development of several microextraction formats, such as in-tube solid-phase and pipette tip-based extractions. These techniques using porous monoliths offer several advantages, including miniaturization and on-line coupling with analytical instruments. Additionally, monoliths are ideal support media for imprinting template-specific sites, resulting in the so-called molecularly-imprinted monoliths, with ultra-high selectivity. In this review, time-saving LC columns and preparative applications applied to the analysis of residues and contaminants in food in 2010–2014 are described, focusing on recent improvements in design and with emphasis in automated on-line systems and innovative materials and formats.

  13. Fractionation separation of human plasma proteins using HPLC with a homemade iron porphyrin based monolithic column.

    Science.gov (United States)

    Zhang, Doudou; Zhao, Yu; Lan, Dandan; Pang, Xiaomin; Bai, Ligai; Liu, Haiyan; Yan, Hongyuan

    2017-11-15

    In this work a polymer monolithic column was fabricated within the confines of a stainless steel column (50×4.6mm i.d.) via radical polymerization by using iron porphyrin and butyl methacrylate as co-monomers, ethylene glycol dimethacrylate as crosslinking agent, ethylene glycol, isopropyl alcohol and N, N-dimethylformamide as tri-porogens, benzoyl peroxide and N,N-dimethylaniline as initiators. The resulting monolithic column was characterized by elemental analysis, scanning electron microscopy, nitrogen adsorption BET surface area, and mercury intrusion porosimetry, respectively. Results showed that the homemade monolith occupied relatively uniform pore structure, low back pressure, and enhanced selectivity for proteins in complex bio-samples. The present work described a simple and efficient method for "fractionation separation" of human plasma proteins, and it is a promising separation method for complex bio-samples in proteomic research. Copyright © 2017 Elsevier B.V. All rights reserved.

  14. Recent advances in the preparation and application of monolithic capillary columns in separation science.

    Science.gov (United States)

    Hong, Tingting; Yang, Xi; Xu, Yujing; Ji, Yibing

    2016-08-10

    Novel column technologies involving various materials and efficient reactions have been investigated for the fabrication of monolithic capillary columns in the field of analytical chemistry. In addition to the development of these miniaturized systems, a variety of microscale separation applications have achieved noteworthy results, providing a stepping stone for new types of chromatographic columns with improved efficiency and selectivity. Three novel strategies for the preparation of capillary monoliths, including ionic liquid-based approaches, nanoparticle-based approaches and "click chemistry", are highlighted in this review. Furthermore, we present the employment of state-of-the-art capillary monolithic stationary phases for enantioseparation, solid-phase microextraction, mixed-mode separation and immobilized enzyme reactors. The review concludes with recommendations for future studies and improvements in this field of research. Copyright © 2016 Elsevier B.V. All rights reserved.

  15. Monolithic and core-shell columns in comprehensive two-dimensional HPLC: a review.

    Science.gov (United States)

    Jandera, Pavel; Hájek, Tomáš; Staňková, Magda

    2015-01-01

    The crucial point affecting the separation time in comprehensive two-dimensional liquid chromatography is the performance of the column used in the second dimension, which should allow highly efficient fast chromatographic separations in the short time available for the analysis of fractions transferred from the first to the second dimension (often 1 min or less). This can be accomplished on short columns packed with sub-2-μm particles, at the cost of very high operation pressure. Core-shell or silica monolithic columns have better permeability, and their use in the second dimension of comprehensive two-dimensional liquid chromatography with conventional liquid chromatography instrumentation is continuously increasing. Monolithic columns based on organic polymer matrices offer a wide selection of stationary phase chemistries, including new hydrophilic interaction liquid chromatography materials, which can be used in the design of novel two-dimensional separations. Some organic polymer monolithic materials offer a dual retention mechanism (reversed-phase hydrophilic interaction liquid chromatography), so a single column can be used in alternating runs for highly orthogonal off-line two-dimensional and even three-dimensional separations. In the present work, the properties of core-shell and silica gel monolithic columns are briefly summarized and their applications in two-dimensional separations of peptides, proteins, oligomer surfactants, fats and oils, carotenoids, phenolic and flavone compounds in plant extracts, food, and beverages are reviewed.

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

    Science.gov (United States)

    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

  17. Recent developments and applications of molecularly imprinted monolithic column for HPLC and CEC.

    Science.gov (United States)

    Zheng, Chao; Huang, Yan-Ping; Liu, Zhao-Sheng

    2011-08-01

    As a new generation of stationary phases, monolithic supports have attracted significant interest in high-performance liquid chromatography (HPLC) and capillary electrochromatography (CEC) because of their ease of preparation, high reproducibility, versatile surface chemistry and rapid mass transport. Molecularly imprinted polymers (MIPs) are synthetic materials with high specific recognition ability to template molecule. The combination of monolithic column and MIPs integrates the high efficiency of modern chromatography and the high selectivity provided by MIPs. This review focuses on the recent developments and applications of all kinds of monolithic matrix, i.e. organic polymer-based and silica-based MIP monolith in HPLC and CEC mode. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. On-chip cell lysis by antibacterial non-leaching reusable quaternary ammonium monolithic column.

    Science.gov (United States)

    Aly Saad Aly, Mohamed; Gauthier, Mario; Yeow, John

    2016-02-01

    Reusable antibacterial non-leaching monolithic columns polymerized in microfluidic channels designed for on-chip cell lysis applications were obtained by the photoinitiated free radical copolymerization of diallyldimethylammonium chloride (DADMAC) and ethylene glycol diacrylate (EGDA) in the presence of a porogenic solvent. The microfluidic channels were fabricated in cross-linked poly(methyl methacrylate) (X-PMMA) substrates by laser micromachining. The monolithic columns have the ability to inhibit the growth of, kill and efficiently lyse Gram-positive Micrococcus luteus (Schroeter) (ATCC 4698) and Kocuria rosea (ATCC 186), and Gram-negative bacteria Pseudomonas putida (ATCC 12633) and Escherichia coli (ATCC 35218) by mechanically shearing the bacterial membrane when forcing the cells to pass through the narrow pores of the monolithic column, and simultaneously disintegrating the cell membrane by physical contact with the antibacterial surface of the column. Cell lysis was confirmed by off-chip PCR without the need for further purification. The influence of the cross-linking monomer on bacterial growth inhibition, leaching, lysis efficiency of the monolithic column and its mechanical stability within the microfluidic channel were investigated and analyzed for three different cross-linking monomers: ethylene glycol dimethacrylate (EGDA), ethylene glycol dimethacrylate (EGDMA) and 1,6-hexanediol dimethacrylate (1,6-HDDMA). Furthermore, the bonding efficiency of two X-PMMA substrates with different cross-linking levels was studied. The monolithic columns were shown to be stable, non-leaching, and reusable for over 30 lysis cycles without significant performance degradation or DNA carryover when they were back-flushed between lysis cycles.

  19. Preparation of phenylboronic acid-silica hybrid monolithic column with one-pot approach for capillary liquid chromatography of biomolecules.

    Science.gov (United States)

    Lin, Zian; Huang, Hui; Li, Shihua; Wang, Juan; Tan, Xiaoqing; Zhang, Lan; Chen, Guonan

    2013-01-04

    A phenylboronic acid-silica hybrid monolithic column for capillary liquid chromatography (cLC) was prepared through one-pot process by using 4-vinylphenylboronic acid (VPBA) and alkoxysilanes simultaneously. The effects of the molar ratio of tetramethyloxysilane/γ-methacryloxypropyltrimethoxysilane (TMOS/γ-MAPS), amount of VPBA, and the volume of diethylene glycol (DEG) on the morphologies, permeabilities and pore properties of the prepared VPBA-silica hybrid monolithic columns were studied in detail. A relatively uniform monolithic structure with high porosity was obtained with optimized ingredients. A series of cis-diol-containing compounds, alkylbenzenes, amides, and anilines were utilized to evaluate the retention behaviors of the VPBA-silica hybrid monolithic column. The result demonstrated that the prepared VPBA-silica hybrid monolithic column exhibited multiple interactions including hydrophobicity, hydrophilicity, as well as cation exchange apart from the expected affinity interaction. The run-to-run, column-to-column and batch-to-batch reproducibility of the VPBA-silica hybrid monolith were satisfactory with the relative standard deviations (RSDs) less than 1.63% (n=5), 2.02% (n=3) and 2.90% (n=5), respectively, indicating the effectiveness and practicability of the proposed method. In addition, the VPBA-silica hybrid monolithic column was further applied to the separation of proteins and tryptic digest of bovine serum albumin (BSA), respectively. The successful applications suggested the potential of the VPBA-silica hybrid monolith in proteome analysis. Copyright © 2012 Elsevier B.V. All rights reserved.

  20. Silica monolithic columns : Synthesis, characterisation and applications to the analysis of biological molecules

    NARCIS (Netherlands)

    Rieux, Laurent; Niederländer, Harm; Verpoorte, Elisabeth; Bischoff, Rainer

    In recent years, proteomics has been a subject of intense research. The complexity of proteomics samples has fostered technological developments. One of these addresses the need for more efficient and faster separations. Monolithic columns prepared from organic and silica monomers offer very

  1. Investigation of chromatographic behavior and porous properties of butyl methacrylate monolithic columns

    Czech Academy of Sciences Publication Activity Database

    Širc, Jakub; Bosáková, Z.; Coufal, P.; Michálek, Jiří; Guryča, Vilém

    2008-01-01

    Roč. 23, č. 6 (2008), s. 591-596 ISSN 1042-6914 R&D Projects: GA MŠk 1M0538 Institutional research plan: CEZ:AV0Z40500505 Keywords : capillary HPLC * monolithic columns * morphology Subject RIV: CD - Macromolecular Chemistry Impact factor: 0.706, year: 2008

  2. Novel approach to determine ghrelin analogs by liquid chromatography with mass spectrometry using a monolithic column

    Czech Academy of Sciences Publication Activity Database

    Zemenová, Jana; Sýkora, D.; Adámková, H.; Maletínská, Lenka; Elbert, Tomáš; Marek, Aleš; Blechová, Miroslava

    2017-01-01

    Roč. 40, č. 5 (2017), s. 1032-1039 ISSN 1615-9306 Institutional support: RVO:61388963 Keywords : enzyme-linked immunosorbent assay * ghrelin * lipopeptides * liquid chromatography mass spectrometry * monolithic columns Subject RIV: CB - Analytical Chemistry, Separation OBOR OECD: Analytical chemistry Impact factor: 2.557, year: 2016

  3. Applicability of analytical and preparative monolithic columns to the separation and isolation of major whey proteins.

    Science.gov (United States)

    Albreht, Alen; Vovk, Irena

    2012-03-02

    The separation and isolation of major whey proteins is already extensively covered in the literature although no study has been published in which monolithic columns were used. In our research we present, for the first time, the use of short convective interaction media (CIM) monolithic columns for the separation of all major whey proteins and isolation of β-lactoglobulin variant A and B (β-LgA and β-LgB) from a commercial product whey isolate (WI). Although our primary interest was directed towards finding a proper monolithic column and chromatographic conditions for the purification and isolation of β-LgA and β-LgB, three additional analytical LC methods, each having its own potential application target, were also developed in the course of our research. On the monolithic diethylaminoethyl convective interaction media analytical column (CIMac DEAE), the separation of major whey proteins was achieved by gradually lowering the pH of the mobile phase. The ever-so-hard obtainable linear external pH gradient was very linear in the range of pH 5.5-3 and the developed ion-exchange (IE) high-performance liquid chromatographic (HPLC) method was amenable to mass spectrometry (MS). A very fast baseline separation, with UV detection, of all major whey proteins was achieved on a prototype CIMac reversed-phase styrene-divinylbenzene (RP-SDVB) monolithic column in only 4 min and the performance of this column proved superior in comparison with the packed particle POROS perfusion column. The developed RP-HPLC-MS method is fast and, due to the MS detector, can offer low limits of detection and quantitation. Finally, in order to fulfill our primary interest, a scale-up method was developed, using a prototype 8 mL analogue of the CIMac RP-SDVB column, for the isolation of native and chemically unmodified β-LgA and β-LgB from WI with purities higher than 90% and 81%, respectively. The proteins were to be used in further protein-ligand binding studies. The developed methods

  4. Trimethyl-β-cyclodextrin-encapsulated monolithic capillary columns: Preparation, characterization and chiral nano-LC application.

    Science.gov (United States)

    Ghanem, Ashraf; Adly, Frady G; Sokerik, Yasser; Antwi, Nana Yaa; Shenashen, Mohamed A; El-Safty, Sherif A

    2017-07-01

    Trimethylated-β-cyclodextrin (TM-β-CD) was encapsulated within several polymer monolithic capillary columns for reversed-phase chiral nano-liquid chromatography (nano-LC). The monolithic phases were prepared using the one-pot in situ copolymerization of ethylene glycol dimethacrylate (EDMA), glycidyl methacrylate (GMA) monomers and 1-propanol, 1,4-butanediol as progenic solvents in presence of TM-β-CD solution within fused silica capillaries (150µm I.D.). The obtained chiral monolithic stationery phases were characterized by scanning electron microscopy (SEM), N 2 adsorption/desorption isotherms, wide angle x-ray diffraction (WAXRD), thermogravimetric analysis (TGA) and differential thermal analysis (DTA). The materials characterization demonstrated that monolithic phases with higher concentration of TM-β-CD have relatively larger surface area, smaller pore size and larger total pore volume compared to those with lower concentration TM-β-CD. The prepared columns were tested for their enantioseparation efficiency of a range of racemic pharmaceuticals. The screening results demonstrated the potential of functionalizing polymer monolithic stationary phases with TM-β-CD using the in situ encapsulation approach. Crown Copyright © 2016. Published by Elsevier B.V. All rights reserved.

  5. [Preparation of C18-silica hybrid monolithic capillary column by "one-pot" process and its application].

    Science.gov (United States)

    Zhang, Zhenbin; Ou, Junjie; Dong, Jing; Wang, Fangjun; Wu, Minghuo; Lin, Hui; Zou, Hanfa

    2011-09-01

    A "one-pot" process for the preparation of organic-silica hybrid capillary monolithic column by concurrently using tetramethoxysilane (TMOS), vinyltrimethoxysilane (VTMS) and the organic monomer, N-(2-(methacryloyloxy) ethyl) dimethyl-octadecylammonium bromide (MDOAB), is described. The polycondensation of alkoxysilanes and the copolymerization of MDOAB and VTMS were subsequently carried out within the confines of a capillary under the proper reaction conditions. The performance of the C18-silica hybrid monolithic column was investigated by capillary electrochromatography and capillary liquid chromatography. In addition, the C18-silica hybrid capillary monolithic column was also applied in the analysis of tryptic digests of bovine serum albumin by capillary liquid chromatography/tandem mass spectrometry (CLC-MS/MS) for demonstrating its potential in proteome analysis. This in situ process of incorporating functional groups into silica monolith provides a new way for the preparation of the organic-silica hybrid monolithic column.

  6. Fabrication of single-walled carbon nanohorns incorporated a monolithic column for capillary electrochromatography.

    Science.gov (United States)

    Zhao, Hongyan; Wang, Yizhou; Cheng, Heyong; Wang, Yuanchao

    2017-08-01

    Single-walled carbon nanohorns have received great interest for their unique properties and diverse potential applications. Herein, we demonstrated the feasibility of single-walled carbon nanohorns incorporated poly(styrene-divinylbenzene) monolith as the stationary phase for capillary electrochromatography, which were prepared by one-step in situ copolymerization. Single-walled carbon nanohorns were dispersed in styrene to give a stable and homogeneous suspension. The monolithic column gave effective separation for a wide range of aromatic compounds, which was based on hydrophobicity and π-π electrostatic stacking of single-walled carbon nanohorns. The precisions of migration time and peak area varied in the ranges of 1.4-1.9% for intraday trials and 1.7-3.5% for interday trials, and 3.2-6.7% for intraday trials and 4.1-7.4% for interday trials, and 3.6-7.2% for inter-column trials and 5.2-21.3% for inter-column trials, respectively, indicating the good reproducibility of single-walled carbon nanohorns embedded monolithic columns. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Zwitterionic silica-based monolithic capillary columns for isocratic and gradient hydrophilic interaction liquid chromatography.

    Science.gov (United States)

    Moravcová, Dana; Planeta, Josef; Kahle, Vladislav; Roth, Michal

    2012-12-28

    This study introduces zwitterionic monolithic capillary columns intended for isocratic and gradient HILIC separations. Silica-based monolithic capillary columns (100 μm × 150 mm) prepared by acidic hydrolysis of tetramethoxysilane in the presence of polyethylene glycol and urea were modified by a sulfoalkylbetaine zwitterion ([2-(methacryloyloxy)ethyl]-dimethyl-(3-sulfopropyl)-ammonium hydroxide) to HILIC stationary phase. The prepared columns were evaluated under the isocratic and gradient separation conditions using a standard mixture containing nucleic acid bases, nucleosides, and 2-deoxynucleosides. Mobile phases contained high concentration of acetonitrile (95-85%, v/v) and 5-50mM ammonium acetate or ammonium formate in the pH range of 3-6. The synthesized columns showed a long-term stability under the separation conditions while the high permeability and efficiency originating from dual structure of the silica monolith were preserved. The relative standard deviations (RSDs) for the retention times of tested solutes were lower than 2% under the isocratic conditions and lower than 3.5% under the gradient conditions. Copyright © 2012 Elsevier B.V. All rights reserved.

  8. Preparation of polymer monolithic column functionalized by arsonic acid groups for mixed-mode capillary liquid chromatography.

    Science.gov (United States)

    Qin, Zhang-Na; Yu, Qiong-Wei; Wang, Ren-Qi; Feng, Yu-Qi

    2018-04-27

    A mixed-mode polymer monolithic column functionalized by arsonic acid groups was prepared by single-step in situ copolymerization of monomers p-methacryloylaminophenylarsonic acid (p-MAPHA) and pentaerythritol triacrylate (PETA). The prepared poly(p-MAPHA-co-PETA) monolithic column has a homogeneous monolithic structure with good permeability and mechanical stability. Zeta potential measurements reveal that the monolithic stationary phase holds a negative surface charge when the mobile phase resides in the pH range of 3.0-8.0. The retention mechanisms of prepared monolithic column are explored by the separation of selected polycyclic aromatic hydrocarbons (PAHs), nucleosides, and three basic compounds. The results indicate that the column functions in three different separation modes associated with reversed-phase chromatography based on hydrophobic interaction, hydrophilic interaction chromatography, and cation-exchange chromatography. The column efficiency of prepared monolithic column is estimated to be 70,000 and 76,000 theoretical plates/m for thiourea and naphthalene, respectively, at a linear flow velocity of 0.85 mm/s using acetonitrile/H 2 O (85/15, v/v) as the mobile phase. Furthermore, an analysis of the retention factors obtained for the PAHs indicates that the prepared monolithic column exhibits good reproducibility with relative standard deviations of 2.9%, 4.0%, and 4.7% based on run-to-run injections, column-to-column preparation, and batch-to-batch preparation, respectively. Finally, we investigate the separation performance of the proposed monolithic column for select phenols, sulfonamides, nucleobases and nucleosides. Copyright © 2018 Elsevier B.V. All rights reserved.

  9. Preparation of organic-silica hybrid monolithic columns via crosslinking of functionalized mesoporous carbon nanoparticles for capillary liquid chromatography.

    Science.gov (United States)

    Liu, Shengju; Peng, Jiaxi; Zhang, Hongyan; Li, Xin; Liu, Zheyi; Kang, Xiaohui; Wu, Minghuo; Wu, Ren'an

    2017-05-19

    An organic-silica hybrid monolithic capillary column was fabricated by crosslinking (3-aminopropyl)trimethoxysilane (APTMS) modified mesoporous carbon nanoparticles (AP-MCNs) with tetramethoxysilane (TMOS) and n-butyltrimethoxysilane (C4-TriMOS). Scanning electron microscopy (SEM), X-ray photoelectron spectroscopy, mercury intrusion porosimetry and inverse size-exclusion chromatography characterization proved the successful immobilization of mesoporous carbon nanoparticles (MCNs). The crosslinking of AP-MCNs into the hybrid monolithic matrix has significantly increased the reversed-phase retention of alkylbenzenes and chromatographic performance for small molecules separations in comparison with the neat one without MCNs. The resulting column efficiency of the mesoporous carbon nanoparticle-based butyl-silica hybrid monolithic column (MCN-C4-monolith) was up to ca. 116,600N/m for the capillary liquid chromatography (cLC) separation of butylbenzene. Enhanced performance of proteins separation was achieved on the MCN-C4-monolith in comparison with the butyl-silica hybrid monolithic column without MCN (C4-monolith). The separation of peptides from bovine serum albumin (BSA) digest was carried out on the MCN-C4-monolith by capillary liquid chromatography-tandem mass spectrometry (cLC-MS/MS) with protein sequence coverage of 81.9%, suggesting its potential application in proteomics. Copyright © 2017 Elsevier B.V. All rights reserved.

  10. Zwitterionic silica-based monolithic capillary columns for isocratic and gradient hydrophilic interaction liquid chromatography

    Czech Academy of Sciences Publication Activity Database

    Moravcová, Dana; Planeta, Josef; Kahle, Vladislav; Roth, Michal

    2012-01-01

    Roč. 1270, DEC 28 (2012), s. 178-185 ISSN 0021-9673 R&D Projects: GA MV VG20112015021; GA ČR(CZ) GAP206/11/0138; GA ČR(CZ) GAP106/12/0522 Institutional support: RVO:68081715 Keywords : HILIC * Monolithic silica column * Nucleoside separation * Nucleic acid base Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 4.612, year: 2012

  11. Bridged polysilsesquioxane-based wide-bore monolithic capillary columns for hydrophilic interaction chromatography

    Czech Academy of Sciences Publication Activity Database

    Šesták, Jozef; Moravcová, Dana; Křenková, Jana; Planeta, Josef; Roth, Michal; Foret, František

    2017-01-01

    Roč. 1479, JAN (2017), s. 204-209 ISSN 0021-9673 R&D Projects: GA ČR(CZ) GA14-06319S; GA ČR(CZ) GA16-03749S Institutional support: RVO:68081715 Keywords : silica monolithic column * HILIC * oligosaccharides * nucleosides Subject RIV: CB - Analytical Chemistry, Separation OBOR OECD: Analytical chemistry Impact factor: 3.981, year: 2016

  12. Preparation, characterization and application of organic-inorganic hybrid ractopamine multi-template molecularly imprinted capillary monolithic column.

    Science.gov (United States)

    He, Jinxing; Fang, Guozhen; Deng, Qiliang; Wang, Shuo

    2011-04-29

    Four isomers of ractopamine used as multi-template molecule, a molecularly imprinted capillary monolithic column was prepared by organic-inorganic hybrid method. The prepared imprinting capillary monolithic columns were characterized by SEM and FTIR, evaluated under capillary electrochromatograhy and the effect of electroosmotic flow and selectivity were studied in detail. It was found that the prepared imprinted monolithic column had good flow-through property when the ratio of methanol and toluene was 3:2. The result indicated that the imprinted monolithic column has good selectivity for four isomers of ractopamine, and under the conditions of pH value of buffer solution was 7 and 10% acetonitrile content in buffer, four isomers of ractopamine could be separated completely. Copyright © 2011 Elsevier B.V. All rights reserved.

  13. Development of a gel monolithic column polydimethylsiloxane microfluidic device for rapid electrophoresis separation.

    Science.gov (United States)

    Zeng, Hu-Lie; Li, Hai-Fang; Wang, Xu; Lin, Jin-Ming

    2006-03-15

    A beta-cyclodextrin (beta-CD)-bonded gel monolithic column polydimethylsiloxane (PDMS) microfluidic device was developed in a simple and feasible way. Before preparation of gel monolithic column in PDMS microchannel, PDMS surface was activated by UV light to create silanol groups, which is an active molecule to covalently bond 3-(trimethoxysilyl)-propyl methacrylate (Bind-Silane) and seal microfluidic device. By the way, Bind-Silane is a bifunctional molecule to link polyacrylamide (PAA) gel and inner wall of PDMS microchannel covalently. Allyl-beta-CD was used not only as a multifunctional crosslinker in PAA gel to control the size of the pores, but also as a chiral selector for the enantioseparation. The stability, transferring heat and optical characteristic of the microfluidic device were examined. The separation capability of the gel monolithic column was confirmed by the successful separation of fluorescein isothiocyanate (FITC)-labeled arginine (Arg), glutamine acid (Glu), tryptophan (Try), cysteine (Cysteine) and phenylalanine (Phe) in the PDMS microfluidic device less than 100 s at 36 mm effective separation length. A maximum of 2.06 x 10(5) theoretical plates was obtained by the potential strength of 490 V/cm. A pair of FITC-labeled dansyl-D,L-threonine (Dns-Thr) was separated absolutely.

  14. Separation of human immunoglobulin G subclasses on a protein A monolith column.

    Science.gov (United States)

    Leblebici, Pelin; Leblebici, M Enis; Ferreira-da-Silva, Frederico; Rodrigues, Alírio E; Pais, Luís S

    2014-07-01

    Monolithic columns have attracted significant attention for the purification of large biomolecules. In the present study, a step gradient elution method was evaluated for the separation of human immunoglobulin G (hIgG) into its subclasses on CIM (convective interaction media) r-protein A (recombinant protein A) monolithic column. hIgG was loaded onto the column and bound protein was eluted with a pH gradient. The subclass content of the eluted fractions was analyzed by enzyme-linked immunosorbent assay (ELISA). Results showed that separation of IgG3 from the other three subclasses can be successfully achieved with high selectivity (100%) and throughput on monolithic media. It was also revealed that enriched fractions of IgG1 and IgG2 could be obtained from purified hIgG in a 28min long chromatographic run. Three fractions with high IgG1 content (89.1%, 94.3% and 88.8%) were recovered. Furthermore, IgG2 was enriched to 64% successfully. A rapid step gradient elution scheme without any additives in buffers was proven to obtain enriched preparations of the two important subclasses with high throughput. The separation time can be reduced even more by increasing the flow rate without any loss in selectivity, which will be beneficial in industrial scale applications. Copyright © 2014 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

    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.

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

    Science.gov (United States)

    Huang, Ke; Zhou, Naiyuan; Chen, Bo

    2011-10-01

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

  17. Poly[hydroxyethyl acrylate-co-poly(ethylene glycol) diacrylate] monolithic column for efficient hydrophobic interaction chromatography of proteins.

    Science.gov (United States)

    Li, Yuanyuan; Tolley, H Dennis; Lee, Milton L

    2009-11-15

    Rigid poly[hydroxyethyl acrylate-co-poly(ethylene glycol) diacrylate] monoliths were synthesized inside 75 mum i.d. capillaries by one-step UV-initiated copolymerization using methanol and ethyl ether as porogens. The optimized monolithic column was evaluated for hydrophobic interaction chromatography (HIC) of standard proteins. Six proteins were separated within 20 min with high resolution using a 20 min elution gradient, resulting in a peak capacity of 54. The effect of gradient rate and initial salt concentration on the retention of proteins were investigated. Mass recovery was found to be greater than 96%, indicating the biocompatibility of this monolith. The monolith was mechanically stable and showed nearly no swelling or shrinking in different polarity solvents. The preparation of this in situ polymerized acrylate monolithic column was highly reproducible. The run-to-run and column-to-column reproducibilities were less than 2.0% relative standard deviation (RSD) on the basis of the retention times of protein standards. The performance of this monolithic column for HIC was comparable or superior to the performance of columns packed with small particles.

  18. Characterization of polymer monolithic columns for small-molecule separations using total-pore-blocking conditions.

    Science.gov (United States)

    Stassen, Catherine; Desmet, Gert; Broeckhoven, Ken; Van Lokeren, Luk; Eeltink, Sebastiaan

    2014-01-17

    This study involves the investigation of the meso- and micropores in polymer monolithic materials and the performance characterization of polymer monoliths for the separation of small molecules. Pore-blocking experiments, that involve the blocking of the stagnant pores with a solvent which is immiscible with the mobile phase, were conducted to determine interstitial volumes of a commercially-available polymer monolithic column. After blocking the meso- and micropores a clear reduction in the column void time was observed. Using this approach, the internal porosity (defined as the sum of the meso- and micropores with respect to the volume of the monolithic material) was determined at 12.5%. Peak-dispersion measurements were conducted by applying reversed-phase (RP) conditions. The high plate-height values for small-molecule separations are mainly attributed to the large eddy-diffusion and mobile-phase mass-transfer contributions to band broadening, related to the inhomogeneous structure and presence of parabolic profiles in the macropores. The C-term contribution of early eluting (retained) compounds was higher than that of the late eluting compounds. This could be attributed to the low zone-retention factors of early-eluting compounds and consequently a large stationary-phase mass-transfer contribution. However, peak-dispersion measurements with blocked meso- and micropores carried out at RP conditions indicated that the Cs-contribution alone is likely not be the main cause of peak broadening. Finally, (1)H spin-spin (T2) relaxometry NMR measurements were conducted with water and ACN in the monolithic material. Copyright © 2013 Elsevier B.V. All rights reserved.

  19. Temperature control in large-internal-diameter scaffolded monolithic columns operated at ultra-high pressures.

    Science.gov (United States)

    Vonk, Rudy J; Aalbers, Tom; Eeltink, Sebastiaan; Schoenmakers, Peter J

    2015-07-03

    Scaffolding makes it feasible to create organic-polymer monoliths in large confinements, such as wide-bore columns. By creating the scaffold from a metal good heat conductivity inside the column is obtained, which renders the relatively large columns (comparable with 4.6 mm i.d.) suitable for application under ultra-high-pressure LC conditions. It was anticipated that the metal scaffold would allow accurate control of the temperature within the columns, but the temperature profiles within the columns could not be characterized using the previously available small-internal-diameter scaffolded columns. In the current study the internal diameter of the scaffolded columns was increased up to square conduits of 4×4 mm. Prior to the formation of the stationary phase the heating efficiency in the empty scaffolded conduits was addressed. The performance of stationary phases created in the large scaffolds was investigated using the kinetic performance approach and the results were compared to those of the previous studies. Finally, scaffolded columns were tested under ultra-high-pressure LC conditions, where good temperature control is essential. Copyright © 2015 Elsevier B.V. All rights reserved.

  20. Mass transfer kinetic mechanism in monolithic columns and application to the characterization of new research monolithic samples with different average pore sizes.

    Science.gov (United States)

    Gritti, Fabrice; Guiochon, Georges

    2009-06-05

    A general reduced HETP (height equivalent to a theoretical plate) equation is proposed that accounts for the mass transfer of a wide range of molecular weight compounds in monolithic columns. The detailed derivatization of each one of the individual and independent mass transfer contributions (longitudinal diffusion, eddy dispersion, film mass transfer resistance, and trans-skeleton mass transfer resistance) is discussed. The reduced HETPs of a series of small molecules (phenol, toluene, acenaphthene, and amylbenzene) and of a larger molecule, insulin, were measured on three research grade monolithic columns (M150, M225, M350) having different average pore size (approximately 150, 225, and 350 A, respectively) but the same dimension (100 mm x 4.6 mm). The first and second central moments of 2 muL samples were measured and corrected for the extra-column contributions. The h data were fitted to the new HETP equation in order to identify which contribution controls the band broadening in monolithic columns. The contribution of the B-term was found to be negligible compared to that of the A-term, even at very low reduced velocities (nu5), the C-term of the monolithic columns is controlled by film mass transfer resistance between the eluent circulating in the large throughpores and the eluent stagnant inside the thin porous skeleton. The experimental Sherwood number measured on the monolith columns increases from 0.05 to 0.22 while the adsorption energy increases by nearly 6 kJ/mol. Stronger adsorption leads to an increase in the value of the estimated film mass transfer coefficient when a first order film mass transfer rate is assumed (j proportional, variantk(f)DeltaC). The average pore size and the trans-skeleton mass transfer have no (<0.5%, small molecules) or little (<10%, insulin) effect on the overall C-term.

  1. Hydrophilic interaction chromatography using a meter-scale monolithic silica capillary column for proteomics LC-MS.

    Science.gov (United States)

    Horie, Kanta; Kamakura, Takeo; Ikegami, Tohru; Wakabayashi, Masaki; Kato, Takashi; Tanaka, Nobuo; Ishihama, Yasushi

    2014-04-15

    A meter-scale monolithic silica capillary column modified with urea-functional groups for hydrophilic interaction liquid chromatography (HILIC) was developed for highly efficient separation of biological compounds. We prepared a ureidopropylsilylated monolithic silica capillary column with a minimum plate height of 12 μm for nucleosides and a permeability of 2.1 × 10(-13) m(2), which is comparable with the parameters of monolithic silica-C18 capillary columns. Over 300,000 theoretical plates were experimentally obtained in HILIC with a 4 m long column at 8 MPa; this is the best result yet reported for HILIC. A 2 m long ureidopropylsilylated monolithic silica capillary column was utilized to develop a HILIC mode LC-MS system for proteomics applications. Using tryptic peptides from human HeLa cell lysate proteins, we identified the comparable numbers of peptides and proteins in HILIC with those in reversed-phase liquid chromatography (RPLC) using a C18-modified monolithic silica column when shallow gradients were applied. In addition, approximately 5-fold increase in the peak response on average was observed in HILIC for commonly identified tryptic peptides due to the high acetonitrile concentration in the HILIC mobile phase. Since HILIC mode LC-MS shows orthogonal selectivity to RPLC mode LC-MS, it is useful as a complementary tool to increase proteome coverage in proteomics studies.

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

    Science.gov (United States)

    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.

  3. Iron oxide nanoparticle coating of organic polymer-based monolithic columns for phosphopeptide enrichment

    Czech Academy of Sciences Publication Activity Database

    Křenková, Jana; Foret, František

    2011-01-01

    Roč. 34, 16-17 (2011), s. 2106-2112 ISSN 1615-9306 R&D Projects: GA ČR(CZ) GAP301/11/2055; GA ČR(CZ) GPP206/11/P004 Grant - others:Jihomoravský kraj(CZ) 2SGA2721 Program:2SGA Institutional research plan: CEZ:AV0Z40310501 Keywords : iron oxide nanoparticles * monolithic column * phosphopeptide enrichment Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 2.733, year: 2011

  4. Preparation and evaluation of 400μm I.D. polymer-based hydrophilic interaction chromatography monolithic columns with high column efficiency.

    Science.gov (United States)

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

    2017-08-04

    The quest for higher column efficiency is one of the major research areas in polymer-based monolithic column fabrication. In this research, two novel polymer-based HILIC monolithic columns with 400μm I.D.×800μm O.D. were prepared based on the thermally initiated co-polymerization of N,N-dimethyl-N-(3-methacrylamidopropyl)-N-(3-sulfopropyl) ammonium betaine (SPP) and ethylene glycol dimethacrylate (EDMA) or N,N'-methylenebisacrylamide (MBA). In order to obtain a satisfactory performance in terms of column permeability, mechanical stability, efficiency and selectivity, the polymerization parameters were systematically optimized. Column efficiencies as high as 142, 000 plates/m and 120, 000 plates/m were observed for the analysis of neutral compounds at 0.6mm/s on the poly(SPP-co-MBA) and poly(SPP-co-EDMA) monoliths, respectively. Furthermore, the Van Deemter plots for thiourea on the two monoliths were compared with that on a commercial silica based ZIC-HILIC column (3.5μm, 200Å, 150mm×300μm I.D.) using ACN/H 2 O (90/10, v/v) as the mobile phase at room temperature. It was noticeable that the Van Deemter curves for both monoliths, particularly the poly(SPP-co-MBA) monolith, are significantly flatter than that obtained for the ZIC-HILIC column, which indicates that in spite of their larger internal diameters, they yield better overall efficiency, with less peak dispersion, across a much wider range of usable linear velocities. A clearly better separation performance was also observed for nucleobases, nucleosides, nucleotides and small peptides on the poly(SPP-co-MBA) monolith compared to the ZIC-HILIC column. It is particularly worth mentioning that these 400μm I.D. polymer-based HILIC monolithic columns exhibit enhanced mechanical strength owing to the thicker capillary wall of the fused-silica capillaries. Copyright © 2017 Elsevier B.V. All rights reserved.

  5. New hydroxyapatite monolithic column for DNA extraction and its application in the purification of Bacillus subtilis crude lysate.

    Science.gov (United States)

    Yu, Shengbing; Geng, Jing; Zhou, Ping; Wang, Jing; Chen, Xiangdong; Hu, Jiming

    2008-03-07

    A hydroxyapatite (Hap) monolithic column with micrometer macropores skeleton structure was prepared by sol-gel technique for efficient DNA extraction. The main extraction mechanism of this monolithic column was attributed to the electrostatic interaction between the phosphate groups of DNA and the calcium ions (C site) of Hap. DNA extraction conditions, such as pH, ion concentration, ion type and loading capacity, on the monolithic column were optimized online by capillary electrophoresis with laser-induced fluorescence detection. Under the optimal condition, a 6 cm length monolithic column provided a capacity of 40 ng DNA with an extraction efficiency of 64+/-6.2% (X+/-RSD). As low concentration of salts were used in the extraction procedure, the purified PBE2 plasmid from the Bacillus subtilis crude lysate could be amplified by polymerase chain reaction. This result illustrated that Hap was a potential matrix for DNA purification from complex biological samples which was compatible with the subsequent genetic analysis in miniature format. Since the preparation of this monolithic column was very simple, it was possible to integrate this novel matrix with chip to allow rapid and efficient DNA purification in microscale. This study provided a new attractive solid-phase support for DNA extraction to meet the miniaturized and automated trends of genetic analysis.

  6. Advances in the development of organic polymer monolithic columns and their applications in food analysis--a review.

    Science.gov (United States)

    Jandera, Pavel

    2013-10-25

    Monolithic continuous separation media are gradually finding their way to sample pre-treatment, isolation, enrichment and final analytical separations of a plethora of compounds, occurring as food components, additives or contaminants, including pharmaceuticals, pesticides and toxins, which have traditionally been the domain of particulate chromatographic materials. In the present review, recent advances in the technology of monolithic columns and the applications in food analysis are addressed. Silica-based monoliths are excellent substitutes to conventional particle-packed columns, improving the speed of analysis for low-molecular weight compounds, due to their excellent efficiency and high permeability. These properties have been recently appreciated in two-dimensional HPLC, where the performance in the second dimension is of crucial importance. Organic-polymer monoliths in various formats provide excellent separations of biopolymers. Thin monolithic disks or rod columns are widely employed in isolation, purification and pre-treatment of sample containing proteins, peptides or nucleic acid fragments. Monolithic capillaries were originally intended for use in electrochromatography, but are becoming more frequently used for capillary and micro-HPLC. Monoliths are ideal highly porous support media for immobilization or imprinting template molecules, to provide sorbents for shape-selective isolation of target molecules from various matrices occurring in food analysis. The separation efficiency of organic polymer monoliths for small molecules can be significantly improved by optimization of polymerization approach, or by post-polymerization modification. This will enable full utilization of a large variety of available monomers to prepare monoliths with chemistry matching the needs of selectivity of separations of various food samples containing even very polar or ionized compounds. Copyright © 2013 Elsevier B.V. All rights reserved.

  7. [Preparation of a reversed-phase capillary monolithic column and its application in the separation of polypeptide mixtures].

    Science.gov (United States)

    Xie, Jingxin; Bi, Kaishun; Qian, Xiaohong; Zuang, Yangiun

    2009-03-01

    Capillary monolithic columns (75 microm i.d.) were prepared by the copolymerization of lauryl methacrylate as the basic monomer, ethylene dimethacrylate as the cross-linking agent and 1-dodecyl alcohol, 1,4-butanediol and dimethyl sulfoxide as the porogenic mixture. The synthetic stationary phases had better mechanical properties and chemical stabilities. A series of characterization and evaluations were performed on the capillary monolithic columns including the scanning electron microscope (SEM) images, the influences of pressure and the effects on the separation of peptide mixtures by changing the proportions of the porogen solution and cross-linking agent. The final prescription ciontained 15% (w/w) monomer, 15% (w/ w) cross-linking agent, and 70% (w/w) porogenic agent. Then the solution was heated at 70 1C for 24 h. The test of relationship between column length and back pressure showed that the capillary monolithic columns prepared have superior permeability, so a longer column can be used to improve the effects of separation. The prepared capillary monolithic columns are fitted on the nano-scale high performance liquid chromatography for the separation of tryptic digests of bovine serum albumin (BSA) and human plasma samples, and better results have been obtained.

  8. Ring-opening metathesis polymerization for the preparation of norbornene-based weak cation-exchange monolithic capillary columns.

    Science.gov (United States)

    Gatschelhofer, Christina; Mautner, Agnes; Reiter, Franz; Pieber, Thomas R; Buchmeiser, Michael R; Sinner, Frank M

    2009-03-27

    Functionalized monolithic columns were prepared via ring-opening metathesis polymerization (ROMP) within silanized fused silica capillaries with an internal diameter of 200 microm by in situ grafting. This procedure is conducted in two steps, the first of which is the formation of the basic monolithic structure by polymerization of norborn-2-ene (NBE) and 1,4,4a,5,8,8a-hexahydro-1,4,5,8-exo,endo-dimethanonaphthalene (DMN-H6) in a porogenic system (toluene and 2-propanol) using RuCl(2)(PCy(3))(2)(CHPh) as ROMP initiator. In the second step the still active initiator sites located on the surface of the structure-forming microglobules were used as receptor groups for the attachment ("grafting") of functional groups onto the monolithic backbone by flushing the monolith with 7-oxanorborn-2-ene-5,6-carboxylic anhydride (ONDCA). Functionalization conditions were first defined that did not damage the backbone of low polymer content (20%) monoliths allowing high-throughput chromatographic separations. Variation of the functionalization conditions was then shown to provide a means of controlling the degree of functionalization and resulting ion-exchange capacity. The maximum level of in situ ONDCA grafting was obtained by a 3h polymerization in toluene at 40 degrees C. The weak cation-exchange monoliths obtained provided good separation of a standard peptide mixture comprising four synthetic peptides designed specifically for the evaluation of cation-exchange columns. An equivalent separation was also achieved using the lowest capacity column studied, indicative of a high degree of robustness of the functionalization procedure. As well as demonstrably bearing ionic functional groups enabling analyte separation in the cation-exchange mode, the columns exhibited additional hydrophobic characteristics which influenced the separation process. The functionalized monoliths thus represent useful tools for mixed-mode separations.

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

    Science.gov (United States)

    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.

  10. Selection of column dimensions and gradient conditions to maximize the peak-production rate in comprehensive off-line two-dimensional liquid chromatography using monolithic columns

    NARCIS (Netherlands)

    Eeltink, S.; Dolman, S.; Vivo-Truyols, G.; Schoenmakers, P.; Swart, R.; Ursem, M.; Desmet, G.

    2010-01-01

    The peak-production rate (peak capacity per unit time) in comprehensive off-line two-dimensional liquid chromatography (LC/x/LC) was optimized for the separation of peptides using poly(styrene-co-divinylbenzene) monolithic columns in the reversed-phase (RP) mode. A first-dimension (D-1) separation

  11. [Preparation of new hydrophilic monolithic columns and their applications in capillary liquid chromatography and pressurized capillary electrochromatography].

    Science.gov (United States)

    Gao, Ye; Wang, Yan; Wang, Chaoran; Gu, Xue; Yan, Chao

    2012-05-01

    New hydrophilic monolithic columns were prepared with {[3-(methacryloylamino) propyl] dimethyl(3-sulfopropyl)ammonium hydroxide inner salt (SPP)} as monomer, pentaerythritol triacrylate (PETA) as crosslinking agent, azobisisobutyronitrile (AIBN) as initiator with two different porogens consisting of ethanol/ethylene glycol and methanol/1 ,4-butanediol, separately. In order to obtain monolithic columns with satisfactory efficiency, electroosmotic flow (EOF) velocity and permeability, the contents of the polymerization mixture were investigated and optimized. The performances of the two columns were compared in the permeability and separation performance. It was found that the monolithic column prepared with ethanol/ ethylene glycol had a better column efficiency and selectivity than that with methanol/1,4-butanediol, but was inferior to the latter in permeability. The effect of salt concentration (from 10 to 70 mmol/L ammonium formate) on the retention of nucleosides was investigated. It was observed that the retention factors of these nucleosides increased at first and then decreased. The columns were used in capillary liquid chromatography (cLC) and pressurized capillary electrochromatography (pCEC) for the separation of a test mixture of amines, phenols and nucleosides separately, and satisfactory separations for these samples were achieved. The column used in pCEC system showed better separation and higher speed of the mixture consisted of phenols and nucleosides compared to those used in cLC system.

  12. Chromatographic selectivity of poly(alkyl methacrylate-co-divinylbenzene) monolithic columns for polar aromatic compounds by pressure-driven capillary liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Lin, Shu-Ling; Wang, Chih-Chieh; Fuh, Ming-Ren, E-mail: msfuh@scu.edu.tw

    2016-10-05

    In this study, divinylbenzene (DVB) was used as the cross-linker to prepare alkyl methacrylate (AlMA) monoliths for incorporating π-π interactions between the aromatic analytes and AlMA-DVB monolithic stationary phases in capillary LC analysis. Various AlMA/DVB ratios were investigated to prepare a series of 30% AlMA-DVB monolithic stationary phases in fused-silica capillaries (250-μm i.d.). The physical properties (such as porosity, permeability, and column efficiency) of the synthesized AlMA-DVB monolithic columns were investigated for characterization. Isocratic elution of phenol derivatives was first employed to evaluate the suitability of the prepared AlMA-DVB columns for small molecule separation. The run-to-run (0.16–1.20%, RSD; n = 3) and column-to-column (0.26–2.95%, RSD; n = 3) repeatabilities on retention times were also examined using the selected AlMA-DVB monolithic columns. The π-π interactions between the aromatic ring and the DVB-based stationary phase offered better recognition on polar analytes with aromatic moieties, which resulted in better separation resolution of aromatic analytes on the AlMA-DVB monolithic columns. In order to demonstrate the capability of potential environmental and/or food safety applications, eight phenylurea herbicides with single benzene ring and seven sulfonamide antibiotics with polyaromatic moieties were analyzed using the selected AlMA-DVB monolithic columns. - Highlights: • First investigation on chromatographic selectivity of AlMA-DVB monolithic columns. • Good run-to-run/column-to-column repeatability (<3%) on AlMA-DVB monolithic columns. • Efficient separation of phenylurea herbicides and sulfonamides on AlMA-DVB columns.

  13. Molecularly imprinted macroporous monoliths for solid-phase extraction: Effect of pore size and column length on recognition properties.

    Science.gov (United States)

    Vlakh, E G; Stepanova, M A; Korneeva, Yu M; Tennikova, T B

    2016-09-01

    The series of macroporous monolithic molecularly imprinted monoliths differed by pore size, column length (volume) and amount of template used for imprinting was synthesized using methacrylic acid and glycerol dimethacrylate as co-monomers and antibiotic ciprofloxacin as a template. The prepared monoliths were characterized regarding to their permeability, pore size, porosity, and resistance to the flow of a mobile phase. The surface morphology was also analyzed. The slight dependence of imprinting factor on flow rate, as well as its independence on pore size of macroporous molecularly imprinted monolithic media was observed. The column obtained at different conditions exhibited different affinity of ciprofloxacin to the imprinted sites that was characterized with Kdiss values in the range of 10(-5)-10(-4)M. The solid-phase extraction of ciprofloxacin from such biological liquids as human blood serum, human urine and cow milk serum was performed using the developed monolithic columns. In all cases, the extraction was found to be 95.0-98.6%. Additionally, the comparison of extraction of three fluoroqinolone analogues, e.g. ciprofloxacin, levofloxacin and moxifloxacin, from human blood plasma was carried out. Contrary to ciprofloxacin extracted with more than 95%, this parameter did not exceed 40% for its analogues. Copyright © 2016 Elsevier B.V. All rights reserved.

  14. Photografted methacrylate-based monolithic columns coated with cellulose tris(3,5-dimethylphenylcarbamate) for chiral separation in CEC.

    Science.gov (United States)

    Noel Echevarria, Romina; Carrasco-Correa, Enrique Javier; Keunchkarian, Sonia; Reta, Mario; Herrero-Martinez, José Manuel

    2018-03-01

    A chiral capillary monolithic column for enantiomer separation in capillary electrochromatography was prepared by coating cellulose tris(3,5-dimethylphenylcarbamate) on porous glycidyl methacrylate-co-ethylene dimethacrylate monolith in capillary format grafted with chains of [2(methacryloyloxy)ethyl] trimethylammonium chloride. The surface modification of the monolith by the photografting of [2(methacryloyloxy)ethyl] trimethylammonium chloride monomer as well as the coating conditions of cellulose tris(3,5-dimethylphenylcarbamate) onto the grafted monolithic scaffold were optimized to obtain a stable and reproducible chiral stationary phase for capillary electrochromatography. The effect of organic modifier (acetonitrile) in aqueous mobile phase for the enantiomer separation by capillary electrochromatography was also investigated. Several pairs of enantiomers including acidic, neutral, and basic analytes were tested and most of them were partially or completely resolved under aqueous mobile phases. The prepared monolithic chiral stationary phases exhibited a good stability, repeatability, and column-to-column reproducibility, with relative standard deviations below 11% in the studied electrochromatographic parameters. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Measurement of the eddy dispersion term in chromatographic columns: III. Application to new prototypes of 4.6 mm I.D. monolithic columns.

    Science.gov (United States)

    Gritti, Fabrice; Guiochon, Georges

    2012-02-17

    We investigated the mass transfer mechanism in four research prototypes of silica monolithic columns of the second generation provided by their manufacturer (Merck KGaA, Darmstadt, Germany). The heights equivalent to a theoretical plate (HETP) of these columns were measured. The different contributions to the total HETP (longitudinal diffusion term B/u(S), skeleton/eluent mass transfer resistance term Cu(S), and eddy diffusion term A) were determined experimentally for a non-retained (uracil) and for a retained (naphthalene) compound. We used the peak parking method to determine the longitudinal diffusion term, a recently developed accurate model of effective diffusion in silica monolithic structures to determine the skeleton/eluent mass transfer resistance term, and an accurate method of measurement of the total column HETP to determine the eddy diffusion term. The results show that the minimum plate heights of these monolithic column prototypes range between 6 and 7 μm for retained analytes, three times lower than those observed for monolithic columns of the first generation. A detailed analysis of the eddy diffusion term demonstrates that the improvement observed in the column efficiency is explained in part by the 40% reduction of the domain size (which provides thinner half-height peak width) but mostly by a two-fold decrease of the radial velocity bias across the silica rods (which provides more symmetrical peaks). Yet, the rods in these columns exhibit a residual radial heterogeneity leading to a minimum HETP of only 10 μm for non-retained compounds. Copyright © 2011 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

    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.

  17. Preparation, characterization and application of molecularly imprinted monolithic column for hesperetin.

    Science.gov (United States)

    Shao, Huikai; Zhao, Lingguo; Chen, Jian; Zhou, Haitao; Huang, Shuting; Li, Kang

    2015-01-01

    The molecularly imprinted solid-phase extraction (MISPE) monolithic column coupled with high-performance liquid chromatography (HPLC) was firstly developed for the extraction of hesperetin in the flesh of Citrus reticulata cv. Chachiensis, which is a traditional Chinese medicine (TCM). The molecularly imprinted polymers (MIPs) have been prepared by a thermal polymerization method using hesperetin as the template, acrylamide (AM) as functional monomer and ethylene glycol dimethacrylamide (EGDMA) as cross-linker in the mixed porogen of methanol, toluene and dodecanol. The prepared MIPs were characterized in detail by SEM and FTIR. The results confirmed the uniform and open structure of network skeleton with large flow-through pores. The influence of synthesis conditions on the specific recognition properties of hesperetin MIPs were also investigated systematically. The results showed that high adsorption capacity and good selectivity of MIPs were achieved when using non-imprinted polymer monolith (NIP) and structure similarly compound rutin as references. Furthermore, several parameters of the MISPE method have been optimized, and then it was successfully applied to the extraction of hesperetin from the flesh of Citrus reticulata cv. Chachiensis. Good gathering and impurity removing ability of prepared MIP were demonstrated. The MISPE method was proven to be a potentially competitive technique for separation and cleanup of hesperetin in complex TCM with satisfied recovery (90.8 ± 3.2%) and good precision (RSD = 6.48%). Copyright © 2015 Elsevier B.V. All rights reserved.

  18. Preparation and evaluation of poly(alkyl methacrylate-co-methacrylic acid-co-ethylene dimethacrylate) monolithic columns for separating polar small molecules by capillary liquid chromatography.

    Science.gov (United States)

    Lin, Shu-Ling; Wu, Yu-Ru; Lin, Tzuen-Yeuan; Fuh, Ming-Ren

    2015-04-29

    In this study, methacrylic acid (MAA) was incorporated with alkyl methacrylates to increase the hydrophilicity of the synthesized ethylene dimethacrylate-based (EDMA-based) monoliths for separating polar small molecules by capillary LC analysis. Different alkyl methacrylate-MAA ratios were investigated to prepare a series of 30% alkyl methacrylate-MAA-EDMA monoliths in fused-silica capillaries (250-μm i.d.). The porosity, permeability, and column efficiency of the synthesized MAA-incorporated monolithic columns were characterized. A mixture of phenol derivatives is employed to evaluate the applicability of using the prepared monolithic columns for separating small molecules. Fast separation of six phenol derivatives was achieved in 5 min with gradient elution using the selected poly(lauryl methacrylate-co-MAA-co-EDMA) monolithic column. In addition, the effect of acetonitrile content in mobile phase on retention factor and plate height as well as the plate height-flow velocity curves were also investigated to further examine the performance of the selected poly(lauryl methacrylate-co-MAA-co-EDMA) monolithic column. Moreover, the applicability of prepared polymer-based monolithic column for potential food safety applications was also demonstrated by analyzing five aflatoxins and three phenicol antibiotics using the selected poly(lauryl methacrylate-co-MAA-co-EDMA) monolithic column. Copyright © 2015 Elsevier B.V. All rights reserved.

  19. Silica-based monolithic capillary columns modified by liposomes for characterization of analyte–liposome interactions by capillary liquid chromatography

    Czech Academy of Sciences Publication Activity Database

    Moravcová, Dana; Planeta, Josef; Wiedmer, S. K.

    2013-01-01

    Roč. 1317, SI (2013), s. 159-166 ISSN 0021-9673 R&D Projects: GA MV VG20112015021; GA ČR(CZ) GAP206/11/0138 Institutional support: RVO:68081715 Keywords : monolithic silica capillary column * immobilized liposomes * biomimicking stationary phase Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 4.258, year: 2013

  20. Selective Depletion of Neuropathy-Related Antibodies from Human Serum by Monolithic Affinity Columns Containing Ganglioside Mimics

    NARCIS (Netherlands)

    Tetala, Kishore K. R.; Heikema, Astrid P.; Pukin, Aliaksei V.; Weijers, Carel A. G. M.; Tio-Gillen, Anne P.; Gilbert, Michel; Endtz, Hubert P.; van Belkum, Alex; Zuilhof, Han; Visser, Gerben M.; Jacobs, Bart C.; van Beek, Teris A.

    2011-01-01

    Monolithic columns containing ganglioside GM2 and GM3 mimics were prepared for selective removal of serum anti-ganglioside antibodies from patients with acute and chronic immune-mediated neuropathies. ELISA results demonstrated that anti-GM2 IgM antibodies in human sera and a mouse monoclonal

  1. Characterization of polymer-based monolithic capillary columns by inverse size-exclusion chromatography and mercury-intrusion porosimetry

    NARCIS (Netherlands)

    Urban, J.; Eeltink, S.; Jandera, P.; Schoenmakers, P.J.

    2008-01-01

    Organic-polymer monolithic capillary columns were prepared in fused-silica capillaries by a radical copolymerization reaction of butyl methacrylate and ethylene dimethacrylate monomers in the presence of 1,4-butanediol and 1-propanol as porogen solvents and azobisisobutyronitrile as the initiator.

  2. Determination of phthalate esters in physiological saline solution by monolithic silica spin column extraction method

    Directory of Open Access Journals (Sweden)

    Lu Lu

    2011-05-01

    Full Text Available Monolithic silica spin column extraction (MonoSpin-SPE was developed as a simple, sensitive, and eco-friendly pretreatment method which combined with ultra-fast liquid chromatography-mass spectrometry (UFLC-MS to determine the levels of six phthalate esters, dimethyl-(DMP, diethyl-(DEP, dipropyl- [DPrP], butyl-benzyl-(BBP, dicyclohexyl(DcHP, and di- n-octyl-(DOP phthalate in physiological saline samples. Under optimized experimental conditions, the method was linear in the following ranges: 0.2- 50 μ/L for DMP, DEP, DPrP, DcHP and DOP; 5 – 100 μ/L for BBP. The correlation coefficients (R2 were in the range of O. 9951 – O. 9995 for all the analytes and the limits of detection (LODs and limits of quantification (LOQs were in the ranges of 0.02 – 0.9 μ/L and 0.08 – 2.7 μ/L, respectively. The pretreatment process showed good reproducibility with inter-day and intra-day relative standard deviations (RSDs below 8.5% and 11.2%, respectively. This method was used to determine the levels of six phthalate esters in physiological saline samples and the recoveries ranged from 71.2% to 107. 3%. DMP and DEP were found in actual physical saline samples (brand A and brand B. Keywords: Monolithic silica spin column, Phthalate esters, Physiological saline samples, Ultra fast liquid chromatographymass spectrometry (UFLC-MS

  3. Selection of column dimensions and gradient conditions to maximize the peak-production rate in comprehensive off-line two-dimensional liquid chromatography using monolithic columns.

    Science.gov (United States)

    Eeltink, Sebastiaan; Dolman, Sebastiaan; Vivo-Truyols, Gabriel; Schoenmakers, Peter; Swart, Remco; Ursem, Mario; Desmet, Gert

    2010-08-15

    The peak-production rate (peak capacity per unit time) in comprehensive off-line two-dimensional liquid chromatography (LC/x/LC) was optimized for the separation of peptides using poly(styrene-co-divinylbenzene) monolithic columns in the reversed-phase (RP) mode. A first-dimension ((1)D) separation was performed on a monolithic column operating at a pH of 8, followed by sequential analysis of all the (1)D fractions on a monolithic column operating at a pH of 2. To obtain the highest peak-production rate, effects of column length, gradient duration, and sampling time were examined. RP/x/RP was performed at undersampling conditions using a short 10 min (1)D gradient. The peak-production rate was highest using a 50 mm long (2)D column applying an 8-10 min (2)D gradient time and was almost a factor of two higher than when a 250 mm monolithic column was used. The best way to obtain a higher peak-production rate in off-line LC/x/LC proved to be an increase in the number of (1)D fractions collected. Increasing the (2)D gradient time was less effective. The potential of the optimized RP/x/RP method is demonstrated by analyzing proteomics samples of various complexities. Finally, the trade-off between peak capacity and analysis time is discussed in quantitative terms for both one-dimensional RP gradient-elution chromatography and the off-line two-dimensional (RP/x/RP) approach. At the conditions applied, the RP/x/RP approach provided a higher peak-production rate than the (1)D-LC approach when collecting three (1)D fractions, which corresponds to a total analysis time of 60 min.

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

    Energy Technology Data Exchange (ETDEWEB)

    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 the 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

  5. Experimental study of the operation of the bolt joint of a bearerwith a column in precast-monolithic ceiling

    Directory of Open Access Journals (Sweden)

    Koyankin Aleksandr Aleksandrovich

    2015-05-01

    Full Text Available Precast-monolithic construction is becoming an increasingly popular form of housing. The wide distribution of this type of construction is explained by the possibility to successfully combine the advantages of precast and monolithic construction, at the same time reducing their disadvantages. Though there is a significant lack of data, including experimental data, for objective assessment of the stress-strain state of precast-monolithic floor structures. In order to investigate the structural reliability of the bolt joint of a bearer with a column in a precast-monolithic building a series of experimental investigations were carried out in the laboratory of testing the building structures of the Siberian Federal University.One of the main conclusions is that the bolt joint of a bearer with a column is characterized by sufficient rigidity, crack resistance and bearing capacity. The results of the given work have proved the data obtained in previously conducted investigations on a fragment of a precast-monolithic ceiling.

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

    Science.gov (United States)

    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.

  7. Preparation and evaluation of poly(alkyl methacrylate-co-methacrylic acid-co-ethylene dimethacrylate) monolithic columns for separating polar small molecules by capillary liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Lin, Shu-Ling; Wu, Yu-Ru; Lin, Tzuen-Yeuan; Fuh, Ming-Ren, E-mail: msfuh@scu.edu.tw

    2015-04-29

    Highlights: • Methacrylic acid (MAA) was used to increase hydrophilicity of polymeric monoliths. • Fast separation of phenol derivatives was achieved in 5 min using MAA-incorporated column. • Separations of aflatoxins and phenicol antibiotics were achieved using MAA-incorporated column. - Abstract: In this study, methacrylic acid (MAA) was incorporated with alkyl methacrylates to increase the hydrophilicity of the synthesized ethylene dimethacrylate-based (EDMA-based) monoliths for separating polar small molecules by capillary LC analysis. Different alkyl methacrylate–MAA ratios were investigated to prepare a series of 30% alkyl methacrylate–MAA–EDMA monoliths in fused-silica capillaries (250-μm i.d.). The porosity, permeability, and column efficiency of the synthesized MAA-incorporated monolithic columns were characterized. A mixture of phenol derivatives is employed to evaluate the applicability of using the prepared monolithic columns for separating small molecules. Fast separation of six phenol derivatives was achieved in 5 min with gradient elution using the selected poly(lauryl methacrylate-co-MAA-co-EDMA) monolithic column. In addition, the effect of acetonitrile content in mobile phase on retention factor and plate height as well as the plate height-flow velocity curves were also investigated to further examine the performance of the selected poly(lauryl methacrylate-co-MAA-co-EDMA) monolithic column. Moreover, the applicability of prepared polymer-based monolithic column for potential food safety applications was also demonstrated by analyzing five aflatoxins and three phenicol antibiotics using the selected poly(lauryl methacrylate-co-MAA-co-EDMA) monolithic column.

  8. [Preparation of weak cation exchange monolithic column and its applications for on-line determination of nifedipine in human plasma].

    Science.gov (United States)

    Yang, Xinru; Yang, Gengliang; Zhu, Tao; Feng, Xiaojuan; Yang, Guanqun

    2009-03-01

    A cation exchange monolithic column was prepared with methylacrylic acid (MAA) as the functional monomer and ethylene dimethacrylate (EDMA) as the cross linker. This column was applied to remove the matrix compounds and enrich the ionic medicines in human plasma with water as the mobile phase. As a result, the human plasma samples can be directly injected into chromatographic system. The relationship between the mobile phase flow rate and back pressure was studied. The results showed that the monolithic column had good performances in lower pressure and higher permeability. In addition, the maximum adsorption of nifedipine on this monolithic column was investigated. The on-line clean-up and enrichment of samples were carried out using this column as the solid-phase extraction material and the C18 column as the analytical column. The chromatography was performed on a C18 reversed-phase high performance liquid chromatographic column with ultraviolet detection at 235 nm. The mobile phase was a mixture of methanol-water (70:30, v/v), and the flow rate was 1.0 mL/min. The linear range of nifedipine in human plasma was 5.0-75.0 microg/L. The intra- and inter-day relative standard deviations (RSDs) were both less than 5.0%. The limit of detection (LOD) was 1 microg/L and the limit of quantification (LOQ) was 4 microg/L. In this method tedious pretreatment procedure is not necessary. It is a fast, economical, reproducible and efficient method for assaying trace nifedipine in human plasma.

  9. A novel application of methacrylate based short monolithic columns: concentrating Potato spindle tuber viroid from water samples.

    Science.gov (United States)

    Ruščić, Jelena; Gutiérrez-Aguirre, Ion; Urbas, Lidija; Kramberger, Petra; Mehle, Nataša; Škorić, Dijana; Barut, Miloš; Ravnikar, Maja; Krajačić, Mladen

    2013-01-25

    Potato spindle tuber viroid (PSTVd) is the causal agent of a number of agriculturally important diseases. It is a single-stranded, circular and unencapsidated RNA molecule with only 356-360 nucleotides and no coding capacity. Because of its peculiar structural features, it is very stable ex vivo and it is easily transmitted mechanically by contaminated hands, tools, machinery, etc. In this work, we describe the development and optimization of a method for concentrating PSTVd using Convective Interaction Media (CIM) monolithic columns. The ion-exchange chromatography on diethylamine (DEAE) monolithic analytical column (CIMac DEAE-0.1 mL) resulted in up to 30% PSTVd recovery whilst the hydrophobic interaction chromatography on C4 monolithic analytical column (CIMac C4-0.1 mL) improved it up to 60%. This was due to the fact that the binding of the viroid to the C4 matrix was less strong than to the highly charged anion-exchange matrix and could be easier and more completely eluted under the applied chromatographic conditions. Based on these preliminary results, a C4 HLD-1 (High Ligand Density) 1 mL monolithic tube column was selected for further experiments. One-litre-water samples were mixed with different viroid quantities and loaded onto the column. By using reverse transcription quantitative polymerase chain reaction (RT-qPCR), the viroid RNA was quantified in the elution fraction (≈5 mL) indicating that 70% of the viroid was recovered and concentrated by at least two orders of magnitude. This approach will be helpful in screening irrigation waters and/or hydroponic systems' nutrient solutions for the presence of even extremely low concentrations of PSTVd. Copyright © 2012 Elsevier B.V. All rights reserved.

  10. Polystyrene-co-Divinylbenzene PolyHIPE Monoliths in 1.0 mm Column Formats for Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    Sidratul Choudhury

    2016-03-01

    Full Text Available The reversed phase liquid chromatographic (RP-HPLC separation of small molecules using a polystyrene-co-divinylbenzene (PS-co-DVB polyHIPE stationary phases housed within 1.0 mm i.d. silcosteel columns is presented within this study. A 90% PS-co-DVB polyHIPE was covalently attached to the walls of the column housing by prior wall modification with 3-(trimethoxysilyl propyl methacrylate and could withstand operating backpressures in excess of 200 bar at a flow rate of 1.2 mL/min. Permeability studies revealed that the monolith swelled slightly in 100% acetonitrile relative to 100% water but could nevertheless be used to separate five alkylbenzenes using a flow rate of 40 µL/min (linear velocity: 0.57 mm/s. Remarkable column-to-column reproducibility is shown with retention factor variation between 2.6% and 6.1% for two separately prepared columns.

  11. Controlled ultraviolet (UV) photoinitiated fabrication of monolithic porous layer open tubular (monoPLOT) capillary columns for chromatographic applications.

    Science.gov (United States)

    Collins, David A; Nesterenko, Ekaterina P; Brabazon, Dermot; Paull, Brett

    2012-04-03

    An automated column fabrication technique that is based on a ultraviolet (UV) light-emitting diode (LED) array oven, and provides precisely controlled "in-capillary" ultraviolet (UV) initiated polymerization at 365 nm, is presented for the production of open tubular monolithic porous polymer layer capillary (monoPLOT) columns of varying length, inner diameter (ID), and porous layer thickness. The developed approach allows the preparation of columns of varying length, because of an automated capillary delivery approach, with precisely controlled and uniform layer thickness and monolith morphology, from controlled UV power and exposure time. The relationships between direct exposure times, intensity, and layer thickness were determined, as were the effects of capillary delivery rate (indirect exposure rate), and multiple exposures on the layer thickness and axial distribution. Layer thickness measurements were taken by scanning electron microscopy (SEM), with the longitudinal homogeneity of the stationary phase confirmed using scanning capacitively coupled contactless conductivity detection (sC(4)D). The new automated UV polymerization technique presented in this work allows the fabrication of monoPLOT columns with a very high column-to-column production reproducibility, displaying a longitudinal phase thickness variation within ±0.8% RSD (relative standard deviation).

  12. Sodium hyaluronate-functionalized urea-formaldehyde monolithic column for hydrophilic in-tube solid-phase microextraction of melamine.

    Science.gov (United States)

    Wang, Jiabin; Jiang, Nan; Cai, Zhengmiao; Li, Wenbang; Li, Jianhua; Lin, Xucong; Xie, Zenghong; You, Lijun; Zhang, Qiqing

    2017-09-15

    A novel sodium hyaluronate-functionalized urea-formaldehyde (UF) monolithic column has been developed by in-situ polycondensation of urea, formaldehyde and sodium hyaluronate (HA). HA plays both the roles of crosslinking and hydrophilic functionalization. The preparation factors including different molecular weights of HA and different amounts of HA were optimized, and then a uniform monolith with satisfactory permeability and hydrophilic binding capacity was obtained. Due to the excellent hydrophilicity of HA, HA-functionalized UF monolith showed higher hydrophilic extraction efficiency than UF monolith, and was applied for hydrophilic in-tube solid-phase microextraction (SPME) of melamine (MEL). Several factors for hydrophilic in-tube SPME, such as ACN percentage in the sampling solution, salt concentration and pH value of the sampling solution, elution volume, sampling and elution flow rate, were investigated with respect to the extraction efficiency of MEL. Under the optimized SPME conditions, the limit of detection (LOD) of MEL was found to be 0.2ng/mL in the milk formula samples, the recoveries of MEL spiked in milk formula samples ranged from 87.3% to 96.7% with relative standard deviations (RSDs) less than 5.1%. Owing to the excellent hydrophilic extraction ability, the novel HA-functionalized UF monolith could provide a promising tool for the sensitive analysis of polar analytes in complicated samples. Copyright © 2017 Elsevier B.V. All rights reserved.

  13. Rapid determination of Papaver somniferum alkaloids in process streams using monolithic column high-performance liquid chromatography with chemiluminescence detection

    Energy Technology Data Exchange (ETDEWEB)

    Costin, Jason W. [School of Life and Environmental Sciences, Deakin University, Geelong, Victoria 3217 (Australia); Lewis, Simon W. [Department of Applied Chemistry, Curtin University of Technology, Perth, WA 6845 (Australia); Purcell, Stuart D. [GlaxoSmithKline, Port Fairy, Victoria 3284 (Australia); Waddell, Lucy R. [GlaxoSmithKline, Port Fairy, Victoria 3284 (Australia); Francis, Paul S. [School of Life and Environmental Sciences, Deakin University, Geelong, Victoria 3217 (Australia); Barnett, Neil W. [School of Life and Environmental Sciences, Deakin University, Geelong, Victoria 3217 (Australia)]. E-mail: barnie@deakin.edu.au

    2007-07-30

    We have combined high-performance liquid chromatography (HPLC) separations using a monolithic column with acidic potassium permanganate and tris(2,2'-bipyridyl)ruthenium(II) chemiluminescence detection in a rapid and highly sensitive method to monitor the process of extracting opiate alkaloids from Papaver somniferum. Due to the high flow rates allowed with the monolithic column and the inherent selectivity of the chemiluminescence reactions, the four predominant alkaloids - morphine, codeine, oripavine and thebaine - were determined in less than 2 min. The results obtained with numerous process samples compared favourable with those of the standard HPLC methodology. Limits of detection were 1 x 10{sup -10} M, 5 x 10{sup -10} M, 5 x 10{sup -10} M and 1 x 10{sup -9} M, for morphine, codeine, oripavine and thebaine, respectively.

  14. SH2 Superbinder Modified Monolithic Capillary Column for the Sensitive Analysis of Protein Tyrosine Phosphorylation.

    Science.gov (United States)

    Yao, Yating; Bian, Yangyang; Dong, Mingming; Wang, Yan; Lv, Jiawen; Chen, Lianfang; Wang, Hongwei; Mao, Jiawei; Dong, Jing; Ye, Mingliang

    2018-01-05

    In this study, we present a method to specifically capture phosphotyrosine (pTyr) peptides from minute amount of sample for the sensitive analysis of protein tyrosine phosphorylation. We immobilized SH2 superbinder on a monolithic capillary column to construct a microreactor to enrich pTyr peptides. It was found that the synthetic pTyr peptide could be specifically enriched by the microreactor from the peptide mixture prepared by spiking of the synthetic pTyr peptide into the tryptic digests of α-casein and β-casein with molar ratios of 1:1000:1000. The microreactor was further applied to enrich pTyr peptides from pervanadate-treated HeLa cell digests for phosphoproteomics analysis, which resulted in the identification of 796 unique pTyr sites. In contrast, the conventional SH2 superbinder-based method identified 41 pTyr sites for the same sample, only 5.2% of the number achieved by the microreactor. Finally, this microreactor was also applied to analyze the pTyr in Shc1 complex, an immunopurified protein complex, which resulted in the identification of 15 pTyr sites. Together, this technique is best fitted to analyze the pTyr in minute amount of sample and will have broad application in fields where only a limited amount of sample is available.

  15. Separation of nucleobases, nucleosides, and nucleotides using two zwitterionic silica-based monolithic capillary columns coupled with tandem mass spectrometry

    Czech Academy of Sciences Publication Activity Database

    Moravcová, Dana; Haapala, M.; Planeta, Josef; Hyötyläinen, T.; Kostiainen, R.; Wiedmer, S. K.

    2014-01-01

    Roč. 1373, Dec (2014), s. 90-96 ISSN 0021-9673 R&D Projects: GA MV VG20112015021; GA ČR(CZ) GAP106/12/0522 Institutional support: RVO:68081715 Keywords : HILIC separation * ESI–MS * Monolithic silica column Subject RIV: CB - Analytical Chemistry , Separation Impact factor: 4.169, year: 2014 http://hdl.handle.net/11104/0242051

  16. Poly (methacrylic acid-co-diethenyl-benzene) monolithic microextraction column and its application to simultaneous enrichment and analysis of mycotoxins.

    Science.gov (United States)

    Wu, Fangling; Xu, Chongsheng; Jiang, Nan; Wang, Jiabin; Ding, Chuan-Fan

    2018-02-01

    A poly (methacrylic acid-co-divinyl-benzene) [poly (MAA-co-DVB)] monolithic column was specially prepared according to the chemical structures of the three mycotoxins of aflatoxin B1, zearalenone and sterigmatocystin, and used for in-tube solid-phase microextraction (in-tube SPME) of the selected mycotoxins. The poly (MAA-co-DVB) monolithic column was characterized in detail, and exhibited effective hydrophobic, π-π, and hydrogen bonding interactions towards the target analytes. By coupling the poly (MAA-co-DVB) monolithic column-based in-tube SPME with high-performance liquid chromatography, a simple, sensitive and matrix effect-free method for determination of mycotoxins was developed. Some important parameters related to extraction efficiency were optimized systematically. Under the optimal conditions, the enrichment factors for the three mycotoxins ranged from 71.9 to 98.7. Recoveries of mycotoxins in rice grains with three spiked concentration levels were in the range of 78.0-102.8%, with satisfactory relative standard deviations (n = 4) of 2.96-4.74%. Good linearity was obtained with correlation coefficients larger than 0.99, and the detection limits (S/N = 3) of the three mycotoxins were between 0.69 and 2.03μgkg -1 . The developed poly (MAA-co-DVB) monolithic column based in-tube SPME-HPLC method was successfully used to sensitively determine trace mycotoxins in practical samples of rice grain without interference peaks, indicating that it is promising for the detection of trace mycotoxins in complex grain samples. Copyright © 2017. Published by Elsevier B.V.

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

    Science.gov (United States)

    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.

  18. Preparation of organic-silica hybrid boronate affinity monolithic column for the specific capture and separation of cis-diol containing compounds.

    Science.gov (United States)

    Li, Qianjin; Lü, Chenchen; Li, Hengye; Liu, Yunchun; Wang, Heye; Wang, Xin; Liu, Zhen

    2012-09-21

    A new boronate-silica hybrid monolithic column was prepared using a one-pot approach with 3-acrylamidophenylboronic acid (AAPBA) as the boronate affinity ligand. The AAPBA-silica monolith exhibited several attractive advantages. First, it is highly hydrophilic, providing excellent specificity and avoiding the presence of organic solvent in the mobile phase. Second, due to its large surface area, it exhibited a high binding capacity, 49.5 μmol/mL, the highest among the boronate affinity monolithic columns appeared in the literature. Third, the monolith can bind with cis-diol containing compounds at pH as low as 6.5, which not only avoids the use of basic pH conditions at which the silica monolith may hydrolysis but also facilitates the applications to wider sample range. Finally, the hybrid monolithic column exhibited apparent secondary separation capability, which allows for two-dimensional (2D) separation of cis-diol compounds in a single column. Due to these merits, the AAPBA-silica hybrid monolithic column can be a promising separation medium for the analysis of cis-diol containing compounds. Copyright © 2012 Elsevier B.V. All rights reserved.

  19. Fabrication of a novel hemin-based monolithic column and its application in separation of protein from complex bio-matrix.

    Science.gov (United States)

    Jiang, Xiaoya; Zhang, Doudou; Li, Xueying; Wang, Xixi; Bai, Ligai; Liu, Haiyan; Yan, Hongyuan

    2017-05-10

    A novel polymer-based monolithic column was prepared via redox initiation system within the confines of a stainless steel column with 4.6mm i.d. In the processes, hemin and lauryl methacrylate were used as co-monomers; ethylene dimethacrylate as crosslinking agent; n-butyl alcohol, ethanediol, and N, N-dimethylformamide as tri-porogens; benzoyl peroxide and N, N-dimethyl aniline as redox initiation system. The resulting polymer-based monolithic columns were characterized by scanning electron microscopy, nitrogen adsorption-desorption instrument, and mercury intrusion porosimeter, respectively. The results illustrated that the improved monolith had relative uniform porous structure, good permeability, and low back pressure. Aromatic compounds were used to test the chromatographic behavior of the monolith, resulting in highest column efficiency of 19 880 plates per meter with reversed-phase mechanism. Furthermore, the homemade monolith was used as the stationary phase of high performance liquid chromatography to separate proteins from complex bio-matrix, including human plasma, egg white, and snailase. The results showed that the monolithic column occupied good separation ability with these complex bio-samples. Excellent specific character of the homemade hemin-based monolith was that it could simultaneously remove high-abundance proteins (including human serum albumin, immunoglobulin G, and human fibrinogen) from human plasma and separate other proteins to different fractions. Copyright © 2017 Elsevier B.V. All rights reserved.

  20. [Application of online two-dimensional separation system using monolithic columns for proteome analysis of human cartilage].

    Science.gov (United States)

    Xie, Shajie; Wang, Fangjun; Yan, Dan; Zhou, Guangdong; Ye, Mingliang; Zou, Hanfa

    2010-02-01

    In Shotgun proteome analysis, where nano-flow is adopted to increase the sensitivity as well as extremely complicated samples such as proteolytic digest are inevitably confronted, monolithic capillary columns are widely used to improve the liquid chromatography separation performance. It is known that cartilage contains extensive amounts of extracellular matrix (ECM), in which collagens and aggrecans being the most abundant macromolecules. It is obvious that the high content of ECM components causes a challenge in the comprehensive proteome analysis of cartilage. In this study, a 7 cm x 150 microm i. d. phosphate strong cation exchange (SCX) monolithic capillary column was coupled with an 85 cm x 75 microm i. d. C12 reversed-phase monolithic capillary column for online two-dimensional separation of 20 microg tryptic digest of proteins extracted from human cartilage. After 14 salt steps fractionation and following gradient separation coupled with tandem mass spectrometry detection, finally 7 434 unique peptides, corresponding to 1 901 distinct proteins were positively identified. Then, the identified proteins were analyzed by Gene Ontology (GO), and it was found that most of the identified proteins were come from articular chondrocytes with low abundance, which is important for the researches of articular diseases.

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

    Science.gov (United States)

    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.

  2. Multilayered particle-packed column: Evaluation and comparison with monolithic and core-shell particle columns for the determination of red azo dyes in Sequential Injection Chromatography.

    Science.gov (United States)

    Chocholouš, Petr; Gil, Renato; Acebal, Carolina C; Kubala, Viktor; Šatínský, Dalibor; Solich, Petr

    2017-03-01

    A recently presented new type of "multilayered" organic-inorganic hybrid silica particle packed column YMC-Triart C 18 (50 mm × 4.6 mm, 5 μm) was used for the development of a sequential injection chromatography method for determination of five azo dyes (Sudan I, Sudan II, Sudan III, Sudan orange G, and para red) in selected food seasonings. The use of a novel sorbent brings attractive features, reduced backpressure, and broader chemical stability together with high separation performance, which are discussed and compared with that of three types of columns typically used in medium-pressure flow chromatography techniques (classic monolithic, narrow monolithic, and core-shell particle columns). The separation was performed in gradient elution mode created by the zone mixing of two mobile phases (acetonitrile/water 90:10, 1.5 mL + acetonitrile/water 100:0, 2.3 mL) at a flow rate of 0.60 mL/min and time of analysis <9.5 min. The spectrophotometric detection wavelengths were set to 400, 480, and 500 nm. The high performance of the developed method with multilayered particle column was well documented and the results indicate a broad capability of sequential injection chromatography. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Preparation of quaternary amine monolithic column for strong anion-exchange chromatography and its application to the separation of Enterovirus 71.

    Science.gov (United States)

    Gu, Huimin; Yin, Dezhong; Ren, Jie; Zhang, Baoliang; Zhang, Qiuyu

    2016-10-15

    Large size virion is unable to diffuse into pores of conventional porous chromatography particles. Therefore, separation of virion by conventional column-packing materials is not quite efficient. To solve this problem, a monolithic column with large convective pores and quaternary amine groups was prepared and was applied to separate Enterovirus 71 (EV71, ≈5700-6000kDa). Cross-section, pore structure, hydrodynamic performance, adsorption property and dynamic binding capacity of prepared monolithic column were determined. Double-pore structures, macropore at 2472nm and mesopore at 5-60nm, were formed. The porosity was up to 63.3%, which enable higher permeability and lower back pressure of the monolithic column than commercial UNO™ Q1 column. Based on the breakthrough curves, the loading capacity of bovine serum albumin was calculated to be 42.0mg per column. In addition, prepared quaternary amine monolithic column was proved to be suitable for the separation of protein mixture by strong anion-exchange chromatography. As a practical application, prepared monolith column presents excellent performance to the separation of EV71 from virus-proteins mixture. Copyright © 2016 Elsevier B.V. All rights reserved.

  4. Effects of pressure and frictional heating on protein separation using monolithic columns in reversed-phase chromatography.

    Science.gov (United States)

    Mann, Benjamin F; Makarov, Alexey A; Wang, Heather; Welch, Christopher J

    2017-03-17

    Pressure is not typically controlled or adjusted independently of flow rate during method development in reversed-phase LC (RPLC). However, it has been shown that pressure has an effect on analyte molecular molar volume, and the magnitude of this effect is greater for proteins and ionizable compounds than neutral small molecules. This phenomenon has received attention recently in the context of porous sub-2-micron particle packed columns. The present study surveys the effect of pressure and frictional heating on RPLC separations using commercially-available monolithic columns at constant flow rate and with controlled external temperature. Because the current monoliths cannot be operated at high pressures, all experiments were conducted with pressures at or below 200bar. Nonetheless, substantial changes in retention were still observed; for example, an increase in pressure of 75bar shifted the retention factor for bovine insulin from 1.27 to 1.78, a 40% increase, while a similar experiment with the neutral small molecule, toluene, showed no change in retention. Results are presented from investigations of model peptides and proteins ranging in size from 1kDa to 30kDa, as well as experiments performed with a silica-based C18 monolith and a polystyrene divinylbenzene monolith functionalized with a phenyl stationary phase. This work indicates that protein separations in monoliths are highly pressure sensitive, and pressure should therefore be considered as an additional parameter in method development for optimizing retention and selectivity. Given these findings, and the ever-increasing importance of chromatographic separations of proteins in both industrial and academic laboratories, improved instrumentation and mechanisms for directly controlling system backpressure could be of great practical value. Copyright © 2017 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

    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.

  6. Comparison of commercial organic polymer-based and silica-based monolithic columns using mixtures of analytes differing in size and chemistry.

    Science.gov (United States)

    Vyviurska, Olga; Lv, Yongqin; Mann, Benjamin F; Svec, Frantisek

    2018-01-02

    Commercially available silica-based monolithic columns Chromolith RP-8e, Chromolith RP-18, and Chromolith HR RP-18, and polymer-based monolithic columns ProSwift RP-1S, ProSwift RP-2H, and ProSwift RP-3U varying in pore size and bonded phase have been tested for the fast separation of selected sets of analytes. These mixtures of analytes included small molecules (uracil, caffeine, 1-phenylethanol, butyl paraben, and anthracene), acylated insulins, and intact proteins (ribonuclease A, cytochrome C, transferrin, apomyoglobin, and thyroglobulin), and covered wide range of chemistries and sizes. Small molecules were well separated with a height equivalent to theoretical plate of 11-26 μm using silica-based monolithic columns, while organic polymer-based monoliths excelled in the fast sub 1 min baseline separations of large molecules. A peak capacity of 37 was found for separation of acylated insulins on Chromolith columns using a 3 min gradient at a flow rate of 3 ml/min. Poor recovery of proteins from Chromolith columns and significant peak tailing of small molecules using ProSwift columns were the major obstacles in using monolithic columns in those applications. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Preparation and Evaluation of Poly(N-isopropylacrylamide-co-hexanediol diacrylate-co-ethylene dimethacrylate) Monolithic Column and its Applications in the Separation of Small Molecules.

    Science.gov (United States)

    Ma, Yamin; Liu, Haiyan; Wei, Aile; Qin, Junxiao; Zhang, Shiqi; Zhang, Wen; Bai, Ligai

    2016-11-01

    Poly(N-isopropylacrylamide-co-hexanediol diacrylate-co-ethylene dimethacrylate) [poly(NIPAAm-co-HDDA-co-EDMA)] monolithic column was prepared via in situ polymerization reaction. In order to investigate the porous properties of the monoliths prepared, the morphology was characterized by the scanning electron microscopy; the chemical group of the monolithic column was confirmed by a Fourier transform infrared spectroscopy method. The surface area was 39.1 m 2 /g by the nitrogen adsorption-desorption experiment. With methanol as the mobile phase, the permeability of the monolithic column was calculated as 3.2330 × 10 -14 m 2 Then it was used as the stationary phase of high performance liquid chromatography. The results indicted that poly(NIPAAm-co-HDDA-co-EDMA) monolithic column was good to separate small molecules by controlling the temperature. Column efficiency for p-chloronitrobenzene was 4,680 plates/m. Repeatability was defined by determining run-to-run and column-to-column variation of the retention times of aromatic compounds, expressed as relative standard deviation (RSD = standard deviation/mean × 100%), and the values were <0.58% and 3.1%, respectively. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  8. Pressure-assisted CEC versus CEC using methacrylate-based monolithic columns: influence of the polymerization-mixture composition.

    Science.gov (United States)

    Tanret, Indiana; Mangelings, Debby; Vander Heyden, Yvan

    2008-11-01

    Pressure-assisted CEC (pCEC) can either be performed on a CE instrument by adding pressure at the column inlet, or by applying voltage on a capillary liquid chromatography system. This study investigates the pressure's added value in pCEC using an LC instrument as well as the influence of the polymerization-mixture composition on monolithic columns in such experimental circumstances. Two factors of the polymerization mixture, which is used to prepare the monolithic capillary columns, were varied according to an experimental design approach: the pore-forming solvent/total monomer ratio and the pore-forming solvents composition. Initially, the effect of the resulting stationary phase on the elution behavior of mainly pharmaceutical compounds was studied. Four responses were used to evaluate the effects on the chromatography: retention time, retention factor, peak asymmetry and number of theoretical plates. After processing the results, the stationary phase composition with the best chromatographic behavior was determined and tested. The advantageous properties of this stationary phase compared with the design center-point column were demonstrated. Secondly, the results of these pCEC experiments were compared with those generated in an identical experimental setup previously performed using CEC. Chromatographic conditions were chosen so that the center-point column showed similar retention in CEC and pCEC. The expected advantage (faster analysis) and drawback (decreased efficiency) of pCEC in the analysis of pharmaceuticals was evaluated. Analysis time and efficiency were both found to depend greatly on the porosity of the column. The conclusion of this comparison is that pCEC did not have a significant added value to CEC. However, this was mainly due to the instrument's limitation of the pressure-driven flow over the column. A clear benefit of the pCEC setup was apparatus-related, i.e. the presence of a loop injection system on the pCEC instrument, which avoids the

  9. Preparation of phosphorylcholine-based hydrophilic monolithic column and application for analysis of drug-related impurities with capillary electrochromatography.

    Science.gov (United States)

    Qiu, Danye; Li, Feng; Zhang, Mingyu; Kang, Jingwu

    2016-07-01

    A hydrophilic monolithic CEC column was prepared by thermal copolymerization of zwitterionic monomer 2-methacryloyloxyethyl phosphorylcholine (MPC), pentaerythritol triacrylate (PETA), either methacrylatoethyl trimethyl ammonium chloride (META) or sodium 2-methylpropene-1-sulfonate (MPS) in a polar binary porogen consisting of methanol and THF. A typical hydrophilic interaction LC retention mechanism was observed for low-molecular weight polar compounds including amides, nucleotides, and nucleosides in the separation mode of hydrophilic interaction CEC, when high content of ACN (>60%) was used as the mobile phase. The effect of the electrostatic interaction between the analytes and the stationary phase was found to be negligible. The poly(MPC-co-PETA-co-META or MPS) monolithic columns have an average column efficiency of 40 000 plates/m and displayed with a satisfactory repeatability in terms of migration time and peak areas. Finally, the column was successfully applied to determine the impurities of a positively charged drug pramipexole which are often separated by ion pair RP chromatography due to their high hydrophilicity. All four components can be baseline separated within 5 min with BGE consisting of ACN/20 mM ammonium formate buffer (pH 3.0; 80/20). © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. Fast determination of prominent carotenoids in tomato fruits by CEC using methacrylate ester-based monolithic columns.

    Science.gov (United States)

    Adalid, Ana Maria; Herrero-Martínez, José Manuel; Roselló, Salvador; Maquieira, Angel; Nuez, Fernando

    2007-11-01

    In this study, the major carotenoids (beta-carotene and lycopene) present in tomato fruits were analyzed by CEC with a methacrylate ester-based monolithic column. The effects of the porogenic solvent ratio, and the hydrophobicity of bulk monomer employed were examined on carotenoids separations. A fast separation of these analytes was achieved in less than 5.0 min in a mobile phase containing 35% THF, 30% ACN, 30% methanol, and 5% of a 5 mM Tris aqueous buffer, pH 8, with lauryl methacrylate-based monoliths. The CEC method was evaluated in terms of detection limit and reproducibility (retention time, area, and column preparation) with values below 1.6 microg/mL and 7.2%, respectively. The proposed procedure was successfully applied to the determination of both carotenoids in fruits of several tomato-related species and its usefulness to analyze large series of samples for nutritional quality screening trials in tomato breeding programs is demonstrated. To our knowledge, this is the first work that exploits the powerful and user-friendly monolithic technology for quality breeding and germplasm evaluation program purposes.

  11. The preparation of a poly (pentaerythritol tetraglycidyl ether-co-poly ethylene imine) organic monolithic capillary column and its application in hydrophilic interaction chromatography for polar molecules.

    Science.gov (United States)

    Chen, Ye; Shu, Yan; Yang, Zihui; Lv, Xumei; Tan, Wangming; Chen, Yingzhuang; Ma, Ming; Chen, Bo

    2017-10-02

    An easy single-step thermal treatment "one-pot" approach for the preparation of poly (pentaerythritol tetraglycidyl ether-co-poly ethylene imine) organic monolithic capillary columns was developed successfully. The column was prepared by the epoxy-amine ring-opening polymerization of pentaerythritol tetraglycidyl ether (PTE) with poly (ethylene imine) (PEI) using acetonitrile (ACN) and polyethylene glycol 600 (PEG 600) as the porogenic system at 60 °C for 12 h. The obtained monolith was homogeneous and permeable. It achieved the high-efficiency separation of polar molecules including amides, nucleosides, bases, phenols, and benzoic acids in capillary liquid chromatography (cLC). The highest column efficiency reached ca. 101,000 plates/m (for guanine) on monolith poly(PTE-co-PEI) at 0.64 mm/s, and satisfactory chromatographic performance with column efficiencies ranged from 45,500 to 97,000 plates/m was achieved for the four amides. A typical hydrophilic interaction liquid chromatography (HILIC) retention mechanism was observed with high organic solvent contents (>60% ACN). Also, the polymer-based monolithic column was successfully applied to separate the tumor markers. Furthermore, the poly(PTE-co-PEI) monolith could be easily modified with 1, 2-epoxydodecane, which reacted with the amino groups presented on the surface of the poly(PTE-co-PEI) monolith. Hydrophobic interactions were observed during the separation of alkylbenzenes and anilines on the post-modified poly(PTE-co-PEI) monolith. Together, these results confirm the feasibility of the epoxy-amine ring-opening polymerization reaction during the fabrication of a monolithic column with high efficiency for cLC applications. Copyright © 2017 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

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

    2011-03-15

    Poly(glycidyl methacrylate) cation exchange monolithic column was prepared in fused-silica capillaries of 320 μm i.d. by thermally initiated radical polymerization and utilized in capillary ion chromatography. With 15 mM methanesulfonic acid as the mobile phase, the separations of a mixture of inorganic cations (Li(+), Na(+), NH(4)(+), K(+)) was tested by using a capacitively coupled contactless conductivity detector (C(4)D) and a low impedance C(4)D (LIC(4)D). The LIC(4)D is the series combination of a C(4)D and a quartz crystal resonator. At the resonant frequency of the series combination, the capacitor impedance from capillary wall was offset by the inductance impedance from the quartz crystal resonator. A minimum impedance was obtained in the impedance-frequency curve of the combination. The responses of the C(4)D and LIC(4)D were analyzed based on an equivalent circuit model. It was shown that the sensitivity of the C(4)D to the change in analyte concentration is rather poor due to the high ratio of the impedance from the capillary wall capacitor to the solution impedance. The LIC(4)D has the similar sensitivity as a contact conductivity detector but a much smaller cell volume. The on-column detection model was realized by LiC(4)D without preparation of optical detection window in monolithic column. Copyright © 2010 Elsevier B.V. All rights reserved.

  13. [Preparation of strong cation-exchange monolithic column and its application in polypeptide separation by capillary electrochromatography].

    Science.gov (United States)

    Qi, Nan; Cui, Ruihong; You, Huiyan

    2011-09-01

    A strong cation-exchange monolithic column was prepared by polymerization inside the fused-silica capillary. The solution consisted of acrylic acid and 2-acrylamido-2-methyl-1-propanesulfonic acid as functional monomers, N,N'-methylenebisacrylamide as a cross-linking agent, dimethyl suiphoxide and dodecanol, 1 , 4-butanediol as organic porogenic solvents and azobisisobutyronitrile as a suitable initiator. The effects of the applied voltage, concentrations of organic modifier and salt solution, pH value on the electroosmotic flow were investigated. The experimental results showed that there existed a good linear relationship between the applied voltage and electroosmotic flow with a correlation coefficient of 0.9981; When the concentration of organic modifier (acetonitrile, ACN) was less than 70%, the swelling degree of stationary phase played a main role and the electroosmotic flow was decreased abnormally with the increase of ACN concentration; The electroosmotic flow was decreased with the increase of the concentration of phosphate. When the pH value was in the range of 3-9, it did not exert a significant change in electroosmotic flow. These results were consistent with the theoretical role. At the same time, five peptides were separated successfully under the optimal experimental conditions on the monolithic column for capillary electrochromatography. The column has obvious advantages in polypeptide separation and will be favorable for the protein investigation.

  14. Preparation and evaluation of a hydrophilic poly(2-hydroxyethyl methacrylate-co-N,N'-methylene bisacrylamide) monolithic column for pressurized capillary electrochromatography.

    Science.gov (United States)

    Cheng, Jintian; Chen, Xiadi; Cai, Yimin; He, Yu; Chen, Zongbao; Lin, Zian; Zhang, Lan

    2013-04-01

    A polar polymethacrylate-based monolithic column was introduced and evaluated as a hydrophilic interaction CEC stationary phase. The monolithic stationary phase was prepared by in situ copolymerization of a neutral monomer 2-hydroxyethyl methacrylate and a polar cross-linker N,N'-methylene bisacrylamide in a binary porogenic solvent consisting of dodecyl alcohol and toluene. The hydroxyl and amino groups at the surface of the monolithic stationary phase provided polar sites which were responsible for hydrophilic interactions. The composition and proportion of the polymerization mixture was investigated in detail. The mechanical stability and reproducibility of the obtained monolithic column preformed was satisfied. The effects of pH and organic solvent content on the EOF and the separation of amines, nucleosides, and narcotics on the optimized monolithic column were investigated. A typical hydrophilic interaction CEC was observed on the neutral polar stationary phase. The optimized monolithic column can obtain high-column efficiencies with 62,000-126,000 theoretical plates/m and the RSDs of column-to-column (n = 9), run-to-run (n = 5), and day-to-day (n = 3) reproducibility were less than 6.3%. The calibration curves of these five narcotics exhibited good linearity with R in the range of 0.9959-0.9970 and linear ranges of 1.0-200.0 μg/mL. The detection limits at S/N = 3 were between 0.2 and 1.2 μg/mL. The recoveries of the separation of narcotics on the column were in the range of 84.0-108.6%. The good mechanical stability, reproducibility, and quantitation capacity was suitable for pressure-assisted CEC applications. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. 3D printed titanium micro-bore columns containing polymer monoliths for reversed-phase liquid chromatography.

    Science.gov (United States)

    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.

  16. Preparation of monolithic polymer columns with homogeneous structure via photoinitiated thiol-yne click polymerization and their application in separation of small molecules.

    Science.gov (United States)

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

    2014-12-16

    Two monolithic polymer columns were directly prepared in the UV-transparent fused-silica capillaries via photoinitiated thiol-yne click polymerization of 1,7-octadiyne (ODY) with a dithiol (1,6-hexanedithiol, 2SH) or a tetrathiol (pentaerythriol tetrakis(3-mercaptopropionate), 4SH) within 15 min. The rapid polymerization provided a time-saving approach to optimize preparation conditions. Then, two porogenic systems of diethylene glycol diethyl ether (DEGDE)/tetrahydrofuran (THF) and DEGDE/poly(ethylene glycol) (PEG, Mn = 200) were found to effectively control the porous structure of two kinds of polymeric monoliths (O2SH and O4SH), respectively. The almost disappearance of thiol and alkynyl vibrations (2560 and 2115 cm(-1), respectively) in infrared spectra and Raman spectra indicated a high conversion of the thiol-yne polymerization reaction. The thiol-yne polymerization was further proved by analyzing the energy-dispersive X-ray spectrum (EDS), MALDI-TOF mass spectrum, and elemental data. Scanning electron microscopy (SEM) images showed the monolithic polymer columns with homogeneous porous structure and macropore size of 0.5-1.0 μm, which facilitated the minimum plate heights of 10.0-12.0 μm for alkylbenzenes in reversed-phase liquid chromatography (RPLC). The low values of the A and C terms (monolithic silica columns. The BSA tryptic digest was also separated on the monolithic polymer column by cLC-MS/MS. The result with 85% protein coverage was better than those given by some hybrid monolithic columns. The monolithic polymer columns were further applied for separation of phenols, natural products, and standard proteins and demonstrated satisfactory separation ability.

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

    Science.gov (United States)

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

    2018-01-24

    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.

  18. Measurement of the eddy dispersion term in chromatographic columns. II. Application to new prototypes of 2.3 and 3.2 mm I.D. monolithic silica columns.

    Science.gov (United States)

    Gritti, Fabrice; Guiochon, Georges

    2012-03-02

    The mass transfer mechanisms in silica monolithic columns of the second generation were investigated, using four research samples (two 2.3 mm × 50 mm and two 3.2 mm × 50 mm silica rods) provided by their manufacturer. The heights equivalent to a theoretical plate (HETP) of these columns were measured in a range of mobile phase velocities, following a meticulous experimental protocol. The coefficients of the van Deemter equation (longitudinal diffusion term B/u(S), skeleton/eluent mass transfer resistance term Cu(S), and eddy diffusion term A) were determined. The protocol includes using the peak parking method (to determine the longitudinal diffusion term), an accurate model of effective diffusion in silica monolithic structures (to determine the skeleton/eluent mass transfer resistance term), and an accurate method to measure the column HETP and determine the eddy diffusion term. The results show that the minimum plate heights of these new monolithic columns ranges between 4 and 5 μm, three to four times lower than those observed for monolithic columns of the first generation. A detailed analysis of the eddy diffusion term demonstrates that this improvement in column efficiency is partly explained by the reduction of the domain size (the sum of the skeleton and throughpore sizes, -40%) but mostly by an increase of the radial homogeneity of the monolithic rods. The columns of this second generation exhibit residual trans-column relative velocity biases as low a 1.4% (instead of 3% for previous columns), a value which is comparable to those observed in 4.6mm I.D. columns packed with sub-3 μm core-shell particles, with which they might become competitive. Copyright © 2011 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

    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.

  20. The synthesis of surface-glycosylated porous monolithic column via aqueous two-phase graft copolymerization and its application in capillary-liquid chromatography.

    Science.gov (United States)

    Xiong, Xiyue; He, Haiqin; Shu, Yan; Li, Yuxin; Yang, Zihui; Chen, Yingzhuang; Ma, Ming; Chen, Bo

    2016-12-01

    A facile, flexible process was developed for the preparation of surface-glycosylated porous monolithic columns via aqueous two-phase graft copolymerization of polyethylene glycol diacrylate (PEGDA) and water-soluble dextran (dextran sulfate). The formation of poly(PEGDA) porous skeletons and surface glycosylation were achieved via a one-step process without pre-modification of the dextran. The synthesis conditions were thoroughly optimized. The optimal monolithic column exhibited a large dry state surface area (greater than 400m 2 /g), and it was evaluated as a hydrophilic liquid chromatography (HILIC) stationary phase. A typical HILIC mechanism was observed at high organic solvent content (≥65% acetonitrile). In addition, the resulting monolithic column demonstrated the potential use in analysis of complex biological sample and enviroment water. Copyright © 2016 Elsevier B.V. All rights reserved.

  1. Synthesis and application of a macroporous boronate affinity monolithic column using a metal-organic gel as a porogenic template for the specific capture of glycoproteins.

    Science.gov (United States)

    Yang, Fan; Lin, Zian; He, Xiwen; Chen, Langxing; Zhang, Yukui

    2011-12-23

    A macroporous boronate affinity monolithic column was prepared and applied to specifically capture glycoproteins using metal-organic gels (MOGs) as a porogenic template. This newly explored application of MOGs has proven to be a more convenient method for the formation of macropores in contrast to traditional porogenic methods. The poly (3-acrylamidophenylboronic acid-co-ethylene dimethacrylate) monolithic columns were synthesized in stainless columns by in situ polymerization. To fabricate the macroporous formation with a uniformed open-channel network, the preparation conditions, such as reaction temperature, the concentration of the MOGs and the ratio of monomers were systematically investigated. The prepared macroporous monoliths were characterized by scanning electron microscope (SEM) and mercury intrusion porosimetry. Furthermore, horseradish peroxidase (HRP) and transferrin (TF) were chosen as test glycoproteins, and the chromatographic analysis demonstrated that the macroporous boronate affinity monoliths exhibited a higher selectivity and better dynamic binding capacity toward glycoproteins compared with non-glycoproteins. The resulted affinity monolithic column was successfully employed to specifically capture TF from a bovine serum sample. Copyright © 2011 Elsevier B.V. All rights reserved.

  2. 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.

    Science.gov (United States)

    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.

  3. Rapid determination of 18 glucocorticoids in serum using reusable on-line SPE polymeric monolithic column coupled with LC-quadrupole/orbitrap high-resolution mass spectrometer.

    Science.gov (United States)

    Li, Hui; Ai, Lianfeng; Fan, Sufang; Wang, Yan; Sun, Dianxing

    2017-10-15

    A simple, rapid and sensitive method for the simultaneous determination of 18 glucocorticoids in serum was developed by coupling on-line solid-phase extraction (SPE) polymeric monolithic column to a liquid chromatography-quadrupole/orbitrap high-resolution mass spectrometer. A simple poly(ethylene glycol dimethacrylate) monolith column (10mm×2.1mm i.d.) was fabricated, and the morphology, surface area and extraction performance of the monolithic column were characterized. Serum samples were extracted by acetonitrile (ACN). Then, online SPE was achieved on the synthesized monolithic column using a 10mmol/L ammonium acetate solution as the loading solvent. After the transfer from the monolith into analytical column (Capcell Pak ADME column) using ACN, the adsorbed analytes were separated on the analytical column and detected with a high-resolution hybrid quadrupole/orbitrap mass spectrometer with full scan/ddMS 2 scan mode Under optimized conditions, the method was linear with target linear correlation coefficient (R 2 ) higher than 0.995. Detection limits were in range of 0.1-0.6ng/mL, and the quantification limits were 0.3-1.5ng/mL. The recovery was between 71.9% and 89.2% in three spike levels with precision (n=5) of 5.40-12.1%. The serum sample was directly analyzed after a simple extraction procedure, and the on-line SPE and determination were achieved within only 16min. The method was used to analyze the dynamic contents variation of cortisone and hydrocortisone in serum before and after the surgery. Copyright © 2017 Elsevier B.V. All rights reserved.

  4. Enantioseparation of 2-aryloxypropionic acids on chiral porous monolithic columns by capillary electrochromatography Evaluation of column performance and enantioselectivity

    Czech Academy of Sciences Publication Activity Database

    Messina, A.; Flieger, Miroslav; Bachechi, F.; Sinibaldi, M.

    2006-01-01

    Roč. 1120, - (2006), s. 69-74 ISSN 0021-9673 Institutional research plan: CEZ:AV0Z50200510 Keywords : cec enantioseparations * chiral monolythic columns * polymethacrylates Subject RIV: EE - Microbiology, Virology Impact factor: 3.554, year: 2006

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

    Science.gov (United States)

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

    2015-06-01

    A novel organic-silica hybrid monolith was prepared through the binding of histidine onto the surface of monolithic matrix for mixed-mode per aqueous and ion-exchange capillary electrochromatography. The imidazolium and amino groups on the surface of the monolithic stationary phase were used to generate an anodic electro-osmotic flow as well as to provide electrostatic interaction sites for the charged compounds at low pH. Typical per aqueous chromatographic behavior was observed in water-rich mobile phases. Various polar and hydrophilic analytes were selected to evaluate the characteristics and chromatographic performance of the obtained monolith. Under per aqueous conditions, the mixed-mode mechanism of hydrophobic and ion-exchange interactions was observed and the resultant monolithic column proved to be very versatile for the efficient separations of these polar and hydrophilic compounds (including amides, nucleosides and nucleotide bases, benzoic acid derivatives, and amino acids) in highly aqueous mobile phases. The successful applications suggested that the histidine-modified organic-silica hybrid monolithic column could offer a wide range of retention behaviors and flexible selectivities toward polar and hydrophilic compounds. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

    Science.gov (United States)

    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.

  7. A Design of a New Column-Parallel Analog-to-Digital Converter Flash for Monolithic Active Pixel Sensor.

    Science.gov (United States)

    Chakir, Mostafa; Akhamal, Hicham; Qjidaa, Hassan

    2017-01-01

    The CMOS Monolithic Active Pixel Sensor (MAPS) for the International Linear Collider (ILC) vertex detector (VXD) expresses stringent requirements on their analog readout electronics, specifically on the analog-to-digital converter (ADC). This paper concerns designing and optimizing a new architecture of a low power, high speed, and small-area 4-bit column-parallel ADC Flash. Later in this study, we propose to interpose an S/H block in the converter. This integration of S/H block increases the sensitiveness of the converter to the very small amplitude of the input signal from the sensor and provides a sufficient time to the converter to be able to code the input signal. This ADC is developed in 0.18  μ m CMOS process with a pixel pitch of 35  μ m. The proposed ADC responds to the constraints of power dissipation, size, and speed for the MAPS composed of a matrix of 64 rows and 48 columns where each column ADC covers a small area of 35 × 336.76  μ m 2 . The proposed ADC consumes low power at a 1.8 V supply and 100 MS/s sampling rate with dynamic range of 125 mV. Its DNL and INL are 0.0812/-0.0787 LSB and 0.0811/-0.0787 LSB, respectively. Furthermore, this ADC achieves a high speed more than 5 GHz.

  8. Preparation of a long-alkyl-chain-based hybrid monolithic column with mixed-mode interactions using a "one-pot" process for pressurized capillary electrochromatography.

    Science.gov (United States)

    Lyu, Haixia; Zhao, Heqing; Qin, Wenfei; Xie, Zenghong

    2017-12-01

    A simple "one-pot" approach for the preparation of a new vinyl-functionalized organic-inorganic hybrid monolithic column is described. In this improved method, the hydrolyzed alkoxysilanes of tetramethoxysilane and triethoxyvinylsilane were used as precursors for the synthesis of a silica-based monolith, while 1-hexadecene and sodium ethylenesulfonate were used as vinyl functional monomers along with azobisisobutyronitrile as an initiator. The effects of reaction temperature, urea content, and composition of organic monomers on the column properties (e.g. morphology, mechanical stability, and chromatographic performance) were investigated. The monolithic column was used for the separation of neutral solutes by reversed-phase pressurized capillary. Furthermore, the monolith can separate various aromatic amines, which indicated its excellent cation-exchange capability and hydrophobic interactions. The baseline separation of the aromatic amines was obtained with a column efficiency of up to 78 000 plates/m. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. LC-MS/MS analysis of lipidized analogs of prolactin-releasing peptide utilizing a monolithic column and simple sample preparation

    Czech Academy of Sciences Publication Activity Database

    Zemenová, Jana; Sýkora, D.; Freislebenová, A.; Maletínská, Lenka

    2017-01-01

    Roč. 9, č. 17 (2017), s. 1319-1328 ISSN 1757-6180 R&D Projects: GA ČR(CZ) GA15-08679S Institutional support: RVO:61388963 Keywords : LC-MS * lipopeptides * monolithic column * prolactin-releasing peptide * stability Subject RIV: CE - Biochemistry OBOR OECD: Biochemical research methods Impact factor: 2.673, year: 2016

  10. Online micro-solid-phase extraction based on boronate affinity monolithic column coupled with high-performance liquid chromatography for the determination of monoamine neurotransmitters in human urine.

    Science.gov (United States)

    Yang, Xiaoting; Hu, Yufei; Li, Gongke

    2014-05-16

    Quantification of monoamine neurotransmitters is very important in diagnosing and monitoring of patients with neurological disorders. We developed an online analytical method to selectively determine urinary monoamine neurotransmitters, which coupled the boronate affinity monolithic column micro-solid-phase extraction with high-performance liquid chromatography (HPLC). The boronate affinity monolithic column was prepared by in situ polymerization of vinylphenylboronic acid (VPBA) and N,N'-methylenebisacrylamide (MBAA) in a stainless capillary column. The prepared monolithic column showed good permeability, high extraction selectivity and capacity. The column-to-column reproducibility was satisfactory and the enrichment factors were 17-243 for four monoamine neurotransmitters. Parameters that influence the online extraction efficiency, including pH of sample solution, flow rate of extraction and desorption, extraction volume and desorption volume were investigated. Under the optimized conditions, the developed method exhibited low limit of detection (0.06-0.80μg/L), good linearity (with R(2) between 0.9979 and 0.9993). The recoveries in urine samples were 81.0-105.5% for four monoamine neurotransmitters with intra- and inter-day RSDs of 2.1-8.2% and 3.7-10.6%, respectively. The online analytical method was sensitive, accurate, selective, reliable and applicable to analysis of trace monoamine neurotransmitters in human urine sample. Copyright © 2014 Elsevier B.V. All rights reserved.

  11. Automated dual two-dimensional liquid chromatography approach for fast acquisition of three-dimensional data using combinations of zwitterionic polymethacrylate and silica-based monolithic columns.

    Science.gov (United States)

    Hájek, Tomáš; Jandera, Pavel; Staňková, Magda; Česla, Petr

    2016-05-13

    A monolithic sulfobetaine polymethacrylate micro-column BIGDMA-MEDSA designed in our laboratory, shows dual retention mechanism: In acetonitrile-rich mobile phase, hydrophilic interactions control the retention (HILIC system), whereas in more aqueous mobile phases the column shows essentially reversed-phase behavior with major role of hydrophobic interactions. The zwitterionic polymethacrylate micro-column can be used in the first dimension of two-dimensional LC in alternating reversed-phase (RP) and HILIC modes, coupled with an alkyl-bonded core-shell or silica-based monolithic column in the second dimension, for HILIC×RP and RP×RP comprehensive two-dimensional separations. During the HILIC×RP period, a gradient of decreasing acetonitrile gradient is used for separation in the first dimension, so that at the end of the gradient the polymeric monolithic micro-column is equilibrated with a highly aqueous mobile phase and is ready for repeated sample injection, this time for separation under reversed-phase gradient conditions with increasing concentration of acetonitrile in the first dimension. The fast repeating reversed-phase gradients on a short silica-monolithic or core-shell column in the second dimension can be optimized independently of the actual running first-dimension gradient program. As the alternating HILIC and RP separations on the first-dimension zwitterionic methacrylate column are based on complementary retention mechanisms, the instrumental setup essentially represents two coupled two-dimensional systems. It is first time that such an automated dual LCxLC approach is reported. The novel system allows obtaining three-dimensional data in a relatively short time and can be applied not only to multidimensional gradient separations of flavones and related polyphenolic compounds. Copyright © 2016 Elsevier B.V. All rights reserved.

  12. Dipentaerythritol penta-/hexa-acrylate based-highly cross-linked hybrid monolithic column: Preparation and its applications for ultrahigh efficiency separation of proteins.

    Science.gov (United States)

    Ma, Junqian; Dai, Qian; Li, Xueyun; Zhu, Xianghui; Ma, Teng; Qiao, Xiaoqiang; Shen, Shigang; Liu, Xiuhua

    2017-04-22

    In this study, multi-acrylate based dipentaerythritol penta-/hexa-acrylate (DPEPA) was exploited for fabrication of highly cross-linked hybrid monolithic column by copolymerization with polyhedral oligomeric silsesquioxane methacryl substituted (POSS-MA) via a "one-pot" method. The new DPEPA-POSS hybrid monolithic column was respectively characterized by Fourier transform infrared spectrometry, thermogravimetric analysis, scanning electron microscopy and nitrogen adsorption/desorption measurement. When it was used for the separation of amides, thioureas and positional isomers of phenols, ultrahigh column efficiency separation (up to 511,000 N m -1 ) was achieved with excellent selectivity. Moreover, intact protein standards could be efficiently separated with minimum tailing peaks, outperforming the commercially available silica-based C8 column. Furthermore, successful separation of complex egg white proteins and expressed BARD1 BRCT domains protein sample was also achieved with good chromatographic performance. In the future work, the DPEPA-POSS hybrid monolithic column will be further exploited and applied in capillary electrochromatography as well as the top-down based proteome research. Copyright © 2017 Elsevier B.V. All rights reserved.

  13. Analysis of aflatoxin b1 in Iranian foods using HPLC and a monolithic column and estimation of its dietary intake.

    Science.gov (United States)

    Yazdanpanah, Hassan; Zarghi, Afshin; Shafaati, Ali Reza; Foroutan, Seyed Mohsen; Aboul-Fathi, Farshid; Khoddam, Arash; Nazari, Firoozeh; Shaki, Fatemeh

    2013-01-01

    A high performance liquid chromatographic method was developed for determination of aflatoxin B1 (AFB1) in foods using a monolithic column with sample clean up on an immunoaffinity column. The method was validated for analysis of AFB1 in rice, bread, puffed corn snack, wheat flour and peanut samples. The average recoveries for AFB1 in different foods ranged from 94.4 to 102.5% with the coefficient of variation lower than 10% for all foods. Limit of detection was 0.01 ng/g. A survey of AFB1 was performed on 90 samples collected from Tehran retail market in June 2005. The results showed that none of the bread and wheat flour samples were contaminated with AFB1. The mean AFB1 levels in rice, puffed corn snack and peanut samples were 4.17, 0.11, and 1.97 ng/g, respectively. The level of contamination of 3 samples (one rice sample and two peanuts samples) to AFB1 was found to be higher than 5 ng/g. Although all food samples had mean concentration of AFB1 below the maximum tolerated level in Iran, the mean intake of AFB1 from rice was estimated 3.49 times higher than the guidance value of 1 ng AFB1/Kg body weight/day. Therefore, it is strongly recommended to monitor AFB1 in foods, especially in rice, in Iran. This is the first study on exposure assessment of Iranian population to AFB1.

  14. [Fast determination of active components in Angelica dahurica extract using capillary electrochromatography with methacrylate ester-based monolithic columns].

    Science.gov (United States)

    Wang, Jiajing; Chen, Zhao; Wu, Yutian; Fan, Guorong

    2010-03-01

    The separation and determination of four important active components (imperatorin, isoimperatorin, phelloptorin and falcarindiol) from Angelica dahurica extract has been performed using capillary electrochromatography (CEC) with a methacrylate ester-based monolithic column. The effect of the porogen ratio on the column preparation was studied. The mobile phase composition, such as the concentration of organic solvent, the ionic strength and the pH of the buffer were also optimized. Under the optimized conditions (50% acetonitrile and 50% of a 20 mmol/L sodium dihydrogen phosphate electrolyte at pH 4.95, - 25 kV), a fast and baseline separation of the four analytes was achieved. The calibration curves showed a good linearity (r2 > 0.997) and the limits of detection were lower than 0.34 mg/L. The mean recoveries of the studied components ranged between 95.18% and 98.44%. The method developed is sensitive, reliable and suitable for the quality control. With this CEC system, the quality of Angelica dahurica extracts from 18 various regions was evaluated.

  15. Synthesis of boronate-functionalized organic-inorganic hybrid monolithic column for the separation of cis-diol containing compounds at low pH.

    Science.gov (United States)

    Zhao, Heqing; Lyu, Haixia; Qin, Wenfei; Xie, Zenghong

    2018-04-01

    In this work, an organic-inorganic hybrid boronate affinity monolithic column was prepared via "one-pot" process using 4-vinylphenylboronic acid as organic monomer and divinylbenzene as cross-linker. The effects of reaction temperature, solvents and composition of organic monomers on the column properties (e.g. morphology, permeability, and mechanical stability) were investigated. A series of test compounds including small neutral molecules, aromatic amines, and cis-diol compounds were used to evaluate the retention behaviors of the prepared hybrid monolithic column. The results demonstrated that the prepared hybrid monolith exhibited mixed-interactions including hydrophilicity, cation exchange, and boronate affinity interaction. The run-to-run, day-to-day and batch-to-batch reproducibilities of the prepared hybrid monolith for thiourea's retention time were satisfactory with the relative standard deviations (RSDs) less than 0.09, 1.45 and 4.05% (n = 3), respectively, indicating the effectiveness and practicability of the proposed method. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

    Energy Technology Data Exchange (ETDEWEB)

    Zhai, Haiyun, E-mail: zhaihaiyun@126.com [College of Pharmacy, Guangdong Pharmaceutical University, Guangzhou 510006 (China); Su, Zihao [College of Pharmacy, Guangdong Pharmaceutical University, Guangzhou 510006 (China); Chen, Zuanguang, E-mail: chenzg@mail.sysu.edu.cn [School of Pharmaceutical Science, Sun Yat-sen University, Guangzhou 510006 (China); Liu, Zhenping; Yuan, Kaisong; Huang, Lu [College of Pharmacy, Guangdong Pharmaceutical University, Guangzhou 510006 (China)

    2015-03-20

    Highlights: • A new GO-MISPE monolithic capillary column was prepared. • The column showed ability of impurities removal and excellent selectivity. • Phloxine B existed in real sample was enriched more than 90 times. • The GO-MISPE column presented good recovery and high stability. • The method was prospered to analyze phloxine B and LOD achieved 0.3 ng g{sup −1}. - Abstract: 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{sup −1} (r = 0.9995) with the detection limit (S/N = 3) of 0.075 ng mL{sup −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.

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

    International Nuclear Information System (INIS)

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

    2015-01-01

    Highlights: • A new GO-MISPE monolithic capillary column was prepared. • The column showed ability of impurities removal and excellent selectivity. • Phloxine B existed in real sample was enriched more than 90 times. • The GO-MISPE column presented good recovery and high stability. • The method was prospered to analyze phloxine B and LOD achieved 0.3 ng g −1 . - Abstract: 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

  18. Preparation of a hyper-cross-linked polymer monolithic column and its application to the sensitive determination of genomic DNA methylation.

    Science.gov (United States)

    Chen, Ming-Luan; Liu, Yu-Li; Xing, Xi-Wen; Zhou, Xiang; Feng, Yu-Qi; Yuan, Bi-Feng

    2013-01-14

    A hyper-cross-linked polymer monolithic column, poly(methacrylatoethyl trimethyl ammonium-co-vinylbenzene chloride-co-divinylbenzene) (MATE-co-VBC-co-DVB) with phenyl and quaternary ammonium groups was successfully prepared in the current study. The prepared monolith possesses large specific surface area, narrow mesopore size distribution and high column efficiency. The poly(MATE-co-VBC-co-DVB) monolithic column was demonstrated to have strong anion exchange/reversed-phase (SAX/RP) mixed-mode retention for analytes on capillary liquid chromatography (cLC). By using this monolithic column, we developed a rapid and sensitive method for the detection of DNA methylation. Our results showed that six nucleobases (adenine, guanine, cytosine, thymine, uracil, and 5-methylcytosine (5-mC)) can be baseline separated within 15 min by electrostatic repulsion and hydrophobic interactions between nucleobases and the monolithic stationary phase. The limit of detection (LOD, signal/noise = 3) of 5-mC is 0.014 pmol and endogenous 5-mC can be distinctly detected by using only 10 ng genomic DNA, which is comparable to that obtained by mass spectrometry analysis. Furthermore, by using the method developed here, we found that DNA methylation inhibitor 5-azacytidine (5-aza-C) and 5-aza-2'-deoxycytidine (5-aza-CdR) could induce a significant decrease of genome-wide DNA methylation in human lung carcinoma cells (A549) and cervical carcinoma cells (HeLa). Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. A Design of a New Column-Parallel Analog-to-Digital Converter Flash for Monolithic Active Pixel Sensor

    Directory of Open Access Journals (Sweden)

    Mostafa Chakir

    2017-01-01

    Full Text Available The CMOS Monolithic Active Pixel Sensor (MAPS for the International Linear Collider (ILC vertex detector (VXD expresses stringent requirements on their analog readout electronics, specifically on the analog-to-digital converter (ADC. This paper concerns designing and optimizing a new architecture of a low power, high speed, and small-area 4-bit column-parallel ADC Flash. Later in this study, we propose to interpose an S/H block in the converter. This integration of S/H block increases the sensitiveness of the converter to the very small amplitude of the input signal from the sensor and provides a sufficient time to the converter to be able to code the input signal. This ADC is developed in 0.18 μm CMOS process with a pixel pitch of 35 μm. The proposed ADC responds to the constraints of power dissipation, size, and speed for the MAPS composed of a matrix of 64 rows and 48 columns where each column ADC covers a small area of 35 × 336.76 μm2. The proposed ADC consumes low power at a 1.8 V supply and 100 MS/s sampling rate with dynamic range of 125 mV. Its DNL and INL are 0.0812/−0.0787 LSB and 0.0811/−0.0787 LSB, respectively. Furthermore, this ADC achieves a high speed more than 5 GHz.

  20. [Preparation of hydrophilic interaction monolithic column and its application in the analysis of melamine in dairy products using pressurized capillary electrochromatography].

    Science.gov (United States)

    Li, Xinyan; Wang, Yan; Gu, Xue; Chen, Yan; Yan, Chao

    2010-03-01

    The hydrophilic monolithic column was prepared in 100 microm i. d. capillary in situ using ethylene dimethacrylate as crosslinker, butyl methacrylate and 3-[dimethyl-[2-(2-methyl-prop-2-enoyloxy) ethyl] azaniumyl] propane-1-sulfonate as monomers. In the study, the hydrophilic interaction behavior of the monolithic column was demonstrated. The application of the column in pressurized capillary electrochromatography (pCEC) for the separation of melamine with ultraviolet detection has been studied. The effects of the composition of mobile phase, pH value, the concentration of the buffer, the flow rate of pump and voltage were investigated. The optimum separation for melamine was achieved with the mobile phase of 10 mmol/L phosphate buffer (pH 3.0) and acetonitrile (20: 80, v/v), voltage at 3 kV and UV detection at 215 nm. The limits of detection (LODs) (S/N = 3) for melamine standard was 0.05 mg/L. The method is simple, accurate and works well without using the ion-pairing agent. The powdered milk and liquid milk were analyzed quantitatively by pCEC using the hydrophilic interaction monolithic column. It is shown that this method is promising in the routine analysis of melamine in dairy products.

  1. Preparation of poly(butyl methacrylate-co-ethyleneglyceldimethacrylate) monolithic column modified with β-cyclodextrin and nano-cuprous oxide and its application in polymer monolithic microextraction of polychlorinated biphenyls.

    Science.gov (United States)

    Zheng, Haijiao; Liu, Qingwen; Jia, Qiong

    2014-05-23

    A poly(butyl methacrylate-co-ethyleneglyceldimethacrylate) (poly(BMA-EDMA)) monolithic column was prepared with in situ polymerization method and modified with allylamine-β-cyclodextrin (ALA-β-CD) and nano-cuprous oxide (Cu2O). A polymer monolith microextraction method was developed with the modified monolithic column for the preconcentration of polychlorinated biphenyls combined with gas chromatography-electron capture detector. 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. Because of the hydrophobic properties of β-CD and the porous nano structure of Cu2O, the enrichment capacity of the poly(BMA-EDMA) monolithic column was significantly improved. The extraction efficiency followed the order: poly(BMA-EDMA-ALA-β-CD-Cu2O)>poly(BMA-EDMA-ALA-β-CD)>poly(BMA-EDMA)>direct GC analysis. When applied to the determination of polychlorinated biphenyls in wine samples, low limits of detection (0.09ngmL(-1)) were obtained under the preoptimized conditions (sample volume 1.0mL, sample flow rate 0.1mLmin(-1), eluent volume 0.1mL, and eluent flow rate 0.05mLmin(-1)). In addition, the present method was employed to determine polychlorinated biphenyls in red wine samples and the accuracy was assessed through recovery experiments. The obtained recovery values were in the range of 78.8-104.1% with relative standard deviations less than 9.0%. Copyright © 2014 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

    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.

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

    Science.gov (United States)

    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.

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

    Science.gov (United States)

    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.

  5. 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.

    Science.gov (United States)

    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.

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

    Science.gov (United States)

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

    2015-10-16

    A newly improved one-pot method, based on "thiol-ene" click chemistry and sol-gel approach in microemulsion system, was developed for the preparation of C8/PO(OH)2-silica hybrid monolithic capillary column. The prepared monolith possesses large specific surface area, narrow mesopore size distribution and high column efficiency. The monolithic column was demonstrated to have cation exchange/reversed-phase (CX/RP) mixed-mode retention for analytes on nano-liquid chromatography (nano-LC). On the basis of the developed nano-LC system with MS detector coupled to pipette tip solid phase extraction (PT-SPE) and derivatization process, we then realized simultaneous determination of 10 gibberellins (GAs) with low limits of detection (LODs, 0.003-0.025 ng/mL). Furthermore, 6 endogenous GAs in only 5mg rice leaves (fresh weight) were successfully detected and quantified. The developed PT-SPE-nano-LC-MS strategy may offer promising applications in the determination of low abundant bioactive molecules from complex matrix. Copyright © 2015 Elsevier B.V. All rights reserved.

  7. HPLC determination of betamethasone and prednisolone in urine samples using monolithic column

    International Nuclear Information System (INIS)

    Abro, K.; Memon, N.; Bhanger, M.I.

    2011-01-01

    A fast and reliable HPLC method is reported for the separation and quantification of betamethasone and prednisolone in urine samples using Chromolith at the rate of Performance RP-l8e (100 mm x 4.6 mm) column. The separation and detection was achieved using an isocratic mobile phase composed of methanol:water (44:56 v/v) at 2.0 mL/min and wavelength of 254 nm. After successful optimisation of method parameters, it was applied to the urine samples. Solid phase extraction technique was used to clean the sample before analysis. The developed method was validated for the system suitability, precision and accuracy. The limits of defection for the prednisolone and betamethasone are 0.11 ng and 0.075 ng/10 macro L injection, respectively allowing their determination in human urine samples. Recovery for spiked urine samples was in the range of 97-103 %. The method offers a valuable alternative to the methodologies currently employed for separation and quantification of prednisolone and betamethasone in urine samples. A fast and reliable HPLC method is reported for the separation and quantification of betamethasone and prednisolone in urine samples using Chromolith at the rate of Performance RP-l8e (100 mm x 4.6 mm) column. The separation and detection was achieved using an isocratic mobile phase composed of methanol:water (44:56 v/v) at 2.0 mL/min and wavelength of 254 nm. After successful optimisation of method parameters, it was applied to the urine samples. Solid phase extraction technique was used to clean the sample before analysis. The developed method was validated for the system suitability, precision and accuracy. The limits of defection for the prednisolone and betamethasone are 0.11 ng and 0.075 ng/10 macro L injection, respectively allowing their determination in human urine samples. Recovery for spiked urine samples was in the range of 97-103 %. The method offers a valuable alternative to the methodologies currently employed for separation and quantification

  8. Effects of functional monomers on retention behavior of small and large molecules in monolithic capillary columns at isocratic and gradient conditions.

    Science.gov (United States)

    Urban, Jiří; Jandera, Pavel; Langmaier, Pavel

    2011-08-01

    The polarity of (poly)methacrylate monolithic capillary columns was varied by using alkylmethacrylate monomers with butyl, cyclohexyl, 2-ethylhexyl, lauryl, and stearyl functional groups in the polymerization mixture. The hydrodynamic properties, as well as the retention characteristics in RP-LC of small molecules (alkylbenzenes) and of proteins under gradient elution conditions were studied. The RP selectivity depends on the type of alkyl chain in methacrylate monomer; however, there was no direct correlation between the size of the monomer molecule and methylene or aromatic selectivity of the monlithic column. The lowest selectivity was found for column based on lauryl methacrylate monomer. On the other hand, butyl methacrylate column shows high phenyl selectivity and the column with stearyl methacrylate possesses the highest methylene selectivity for small molecules. The retention increases with longer alkyl chain in methacrylate monomer, especially for high molar mass proteins on all prepared columns and showed gradient elution behavior of proteins in agreement with the linear solvent strength gradient model. The poly(laurylmethacrylate) column showed lowest hydrophobicity but best efficiency for proteins of all columns tested. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. The fabrication of monolithic capillary column based on poly (bisphenol A epoxy vinyl ester resin-co-ethylene glycol dimethacrylate) and its applications for the separation of small molecules in high performance liquid chromatography.

    Science.gov (United States)

    Niu, Wenjing; Wang, Lijuan; Bai, Ligai; Yang, Gengliang

    2013-07-05

    A new polymeric monolith was synthesized in fused-silica capillary by in situ polymerization technique. In the polymerization, bisphenol A epoxy vinyl ester resin (VER) was used as the functional monomer, ethylene glycol dimethacrylate (EDMA) as the crosslinking monomer, 1,4-butanediol, 1-propanol and water as the co-porogens, and azobisisobutyronitrile (AIBN) as the initiator. The conditions of polymerization have been optimized. Morphology of the prepared poly (VER-co-EDMA) monolith was investigated by the scanning electron microscopy (SEM); pore properties were assayed by mercury porosimetry and nitrogen adsorption. The optimized poly (VER-co-EDMA) monolith showed a uniform structure, good permeability and mechanical stability. Then, the column was used as the stationary phase of high performance liquid chromatography (HPLC) to separate the mixture of benzene derivatives. The best column efficiency achieved for phenol was 235790 theoretical plates per meter. Baseline separations of benzene derivatives and halogenated benzene compounds under optimized isocratic mode conditions were achieved with high column efficiency. The column showed good reproducibility: the relative standard deviation (RSD) values based on the retention times (n=3) for run-to-run, column-to-column and batch-to-batch were less than 0.98, 1.68, 5.48%, respectively. Compared with poly (BMA-co-EDMA) monolithic column, the proposed monolith exhibited more efficiency in the separation of small molecules. Copyright © 2013 Elsevier B.V. All rights reserved.

  10. Band broadening in fast gradient high-performance liquid chromatography: application to the second generation of 4.6 mm I.D. silica monolithic columns.

    Science.gov (United States)

    Gritti, Fabrice; Guiochon, Georges

    2012-05-18

    The sources of band broadening in fast gradient elution chromatography include the contributions of the tubings placed upstream the column, the isocratic migration of the sample that takes place in the column until the moment when the front of the gradient catches up with it, dispersion and mass transfer resistance during band migration under gradient elution to the column outlet, and dispersion in the tubings downstream the column to the detector. The measurements of all these contributions is meticulously described, analyzed, and applied to assess the kinetic performance of monolithic columns of the second generation (KGaA Merck) in gradient elution, at the highest possible speed at which they can be operated (t(0)=25s at P=200 bar). These results are compared to those provided by several 4.6mm × 100mm columns packed with sub-3 μm core-shell particles (Kinetex, Phenomenex and Halo, Advanced Material Technologies) and by a 2.1mm × 100mm column packed with fully porous 1.7 μm BEH particles (Waters). A RPLC checkout sample (Agilent) containing nine alkanophenones (molecular weights between 120 and 204 g/mol) was used for this purpose. The mobile phase was a mixture of acetonitrile and water and the instrument, an optimized version of the 1290 Infinity HPLC system (Agilent). The results show that the overall peak capacity provided by this second generation of monolithic columns is nearly 30% smaller than that provided by commercial columns packed with sub-3 μm core-shell particles and 20% smaller than that provided by a narrow-bore column packed with sub-2 μm fully porous particles. After isolating the sole band broadening contribution due to the gradient migration of the analytes along the columns, the BEH column proved to provide the highest resolution power (apparent average plate height, of 2 μm), followed by the 2.6 μm Kinetex particles (3.0 μm), the Halo particles (3.2 μm), and the second generation of 4.6mm I.D. monolithic columns (6.5 μm). This

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

    OpenAIRE

    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.

    2017-01-01

    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. Depleted fully monolithic CMOS pixels with fast readout architectures are currently being developed as promising candidates for the outer pixel layers of the future ATLAS Inner Tracker, which w...

  12. High-performance liquid chromatography analysis of polyacetylenes and polyenes in Echinacea pallida by using a monolithic reversed-phase silica column.

    Science.gov (United States)

    Pellati, Federica; Calò, Samuele; Benvenuti, Stefania

    2007-05-11

    In this study, a RP-HPLC method for the analysis of polyacetylenes and polyenes in Echinacea pallida roots and phytopharmaceuticals was developed. The reference compounds used for quantification were isolated from the plant material and their structures were determined on the basis of the analysis of UV, IR, NMR and MS data. The complete structure elucidation of three compounds, namely 8-hydroxy-tetradec-(9E)-ene-11,13-diyn-2-one (1), tetradec-(8Z)-ene-11,13-diyn-2-one (6) and pentadec-(8Z)-en-2-one (9) is described. In the analysis of the n-hexane extracts of E. pallida roots, the comparison between conventional and monolithic columns showed that the elution order in both cases is identical and the selectivity is equivalent. However, the retention times achieved by the monolithic column are shorter, resulting in a faster separation (20 min). Therefore, the analyses were carried out on a Chromolith Performance RP-18e (100 mm x 4.6 mm i.d.), with a gradient mobile phase composed by H(2)O and ACN at the flow rate of 2 mL/min. The column was thermostatted at 20 degrees C. The photodiode array detector monitored the eluent at 210 nm. The validation procedure confirmed that this technique affords reliable analysis of these components and is appropriate for the quality control of complex matrices, such as E. pallida roots and phytopharmaceuticals.

  13. Rapid determination of telmisartan in human plasma by HPLC using a monolithic column with fluorescence detection and its application to a bioequivalence study.

    Science.gov (United States)

    Zhang, He; Jiang, Yunyun; Wen, Jun; Zhou, Tingting; Fan, Guorong; Wu, Yutian

    2009-11-01

    A rapid HPLC method using a monolithic column with fluorescence detection has been developed for determination of telmisartan in human plasma. Sample preparation was done by protein precipitation with acetonitrile and naproxen was used as IS. The compounds were detected by fluorescence detection, using an excitation wavelength of 300 nm and emission wavelength of 385 nm. Calibration curves of telmisartan were linear in the range of 1-200 ng/mL. The assay was high throughput, sensitive and precise, and it was successfully applied to a bioequivalence study of two formulations of telmisartan.

  14. Charge heterogeneity profiling of monoclonal antibodies using low ionic strength ion-exchange chromatography and well-controlled pH gradients on monolithic columns.

    Science.gov (United States)

    Talebi, Mohammad; Nordborg, Anna; Gaspar, Andras; Lacher, Nathan A; Wang, Qian; He, Xiaoping Z; Haddad, Paul R; Hilder, Emily F

    2013-11-22

    In this work, the suitability of employing shallow pH gradients generated using single component buffer systems as eluents through cation-exchange (CEX) monolithic columns is demonstrated for the high-resolution separation of monoclonal antibody (mAb) charge variants in three different biopharmaceuticals. A useful selection of small molecule buffer species is described that can be used within very narrow pH ranges (typically 1 pH unit) defined by their buffer capacity for producing controlled and smooth pH profiles when used together with porous polymer monoliths. Using very low ionic strength eluents also enabled direct coupling with electrospray ionisation mass spectrometry. The results obtained by the developed pH gradient approach for the separation of closely related antibody species appear to be consistent with those obtained by imaged capillary isoelectric focusing (iCE) in terms of both resolution and separation profile. Both determinants of resolution, i.e., peak compression and peak separation contribute to the gains in resolution, evidently through the Donnan potential effect, which is increased by decreasing the eluent concentration, and also through the way electrostatic charges are distributed on the protein surface. Retention mechanisms based on the trends observed in retention of proteins at pH values higher than the electrophoretic pI are also discussed using applicable theories. Employing monolithic ion-exchangers is shown to enable fast method development, short analysis time, and high sample throughput owing to the accelerated mass transport of the monolithic media. The possibility of short analysis time, typically less than 15 min, and high sample throughput is extremely useful in the assessment of charge-based changes to the mAb products, such as during manufacturing or storage. Copyright © 2013 Elsevier B.V. All rights reserved.

  15. [Determination of five avermectins in bovine liver by on-line solid-phase extraction with hydrophobic monolithic column coupled with high performance liquid chromatography-tandem mass spectrometry].

    Science.gov (United States)

    Li, Xin; Zhang, Yaoqin; Ai, Lianfeng; Wang, Xuesheng; Wang, Manman; Xu, Houjun; Hao, Yulan

    2015-06-01

    A method based on on-line solid-phase extraction (SPE) with hydrophobic monolithic column coupled with high performance liquid chromatography-tandem mass spectrometry was developed for the simultaneous determination of five avermectins in bovine liver. A poly(butyl methacrylate-co-ethylene dimethacrylate) monolithic column was used as the sorbent. The parameters influenced on on-line SPE and separation process such as the loading mobile phase, the eluting flow rate and the solvent for the separation were investigated in detail. Blank samples, spiked samples, matrix effect and recovery experiments were investigated to evaluate the extraction efficiency and potential interfering compounds originating from the matrix. Under the optimized conditions, the method showed a linear range of 1-100 µg/L and the quantification limit of 5 µg/kg for each analyte. The presented method gave recoveries of 77.4%-98.4%. The relative standard deviations of intra-day and inter-day were 4.46%-8.03% and 4.79%-8.68%, respectively. Moreover, no significant changes were found in the extraction performance after more than 400 usages on one monolithic column, and even on the monoliths with various batches. The feasibility of the developed poly (butyl methacrylate-coethylene dimethacrylate) monolithic column based on the on-line SPE method for the determination of avermectins was further demonstrated by the analysis of real samples.

  16. Monolithic columns based on a poly(styrene-divinylbenzene-methacrylic acid) copolymer for capillary liquid chromatography of small organic molecules

    Czech Academy of Sciences Publication Activity Database

    Svobodová, A.; Křížek, T.; Širc, Jakub; Šálek, Petr; Tesařová, E.; Coufal, P.; Štulík, K.

    2011-01-01

    Roč. 1218, č. 11 (2011), s. 1544-1547 ISSN 0021-9673 R&D Projects: GA AV ČR KAN200520804 Institutional research plan: CEZ:AV0Z40500505 Keywords : capillary liquid chromatography * methacrylic acid * polystyrene-based monolithic stationary phase Subject RIV: EI - Biotechnology ; Bionics Impact factor: 4.531, year: 2011

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

    Energy Technology Data Exchange (ETDEWEB)

    Nakamoto, Akihiro [Scientific Investigation Laboratory, Hiroshima Prefectural Police Headquarters, Kohnan 2-26-3, Naka-ku, Hiroshima 730-0825 (Japan); Nishida, Manami [Hiroshima University Technical Center, Kasumi 1-2-3, Minami-ku, Hiroshima 734-8551 (Japan); Saito, Takeshi [Department of Emergency and Critical Care Medicine, Tokai University School of Medicine, Shimokasuya 143, Isehara, Kanagawa 259-1143 (Japan); Kishiyama, Izumi; Miyazaki, Shota [GL Sciences Inc., Sayamagahara 237-2, Iruma, Saitama 358-0032 (Japan); Murakami, Katsunori [Scientific Investigation Laboratory, Hiroshima Prefectural Police Headquarters, Kohnan 2-26-3, Naka-ku, Hiroshima 730-0825 (Japan); Nagao, Masataka [Department of Forensic Medicine, Graduate School of Biomedical Sciences, Hiroshima University, Kasumi 1-2-3, Minami-ku, Hiroshima 734-8551 (Japan); Namura, Akira, E-mail: namera@hiroshima-u.ac.jp [Department of Forensic Medicine, Graduate School of Biomedical Sciences, Hiroshima University, Kasumi 1-2-3, Minami-ku, Hiroshima 734-8551 (Japan)

    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{sub 5} was used as an internal standard. The linear ranges were 0.01-5.0 {mu}g mL{sup -1} for methamphetamine (MA) and 3,4-methylenedioxymethamphetamine (MDMA) and 0.02-5.0 {mu}g mL{sup -1} for amphetamine (AP) and 3,4-methylenedioxyamphetamine (MDA) (coefficient of correlation {>=}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 {mu}g mL{sup -1} of APs and MDAs ranged from 1.4% to 13.6%. The lowest detection limit (signal-to-noise ratio {>=} 3) in urine was 5 ng mL{sup -1} for MA and MDMA and 10 ng mL{sup -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.

  18. Purification of monoclonal antibodies, IgG1, from cell culture supernatant by use of metal chelate convective interaction media monolithic columns.

    Science.gov (United States)

    Rajak, Poonam; Vijayalakshmi, M A; Jayaprakash, N S

    2012-12-01

    Monoclonal antibodies (MAbs) have diverse applications in diagnostics and therapeutics. The recent advancement in hybridoma technology for large-scale production of MAbs in bioreactors demands rapid and efficient purification methods. Conventional affinity purification systems have drawbacks of low flow rates and denaturation of antibodies owing to harsh elution conditions. Here, we attempted purification of MAbs by use of a high-throughput metal-chelate methacrylate monolithic system. Monolithic macroporous convective interaction media-iminodiacetate (CIM-IDA) disks immobilized with four different metal ions (Cu²⁺, Ni²⁺, Zn²⁺ and Co²⁺) were used and evaluated for purification of anti-human serum albumin IgG1 mouse MAbs from cell culture supernatant after precipitation with 50% ammonium sulfate. Elution with 10 mM imidazole in the equilibration buffer (25 mM MMA = MOPS (Morpholino propane sulfonic acid) + MES (Morpholino ethane sulfonic acid) + Acetate + 0.5 M NaCl, pH 7.4) resulted in a purification of 25.7 ± 2.9-fold and 32.5 ± 2.6-fold in experiments done using Zn²⁺ and Co²⁺ metal ions, respectively. The highest recovery of 85.4 ± 1.0% was obtained with a CIM-IDA-Zn(II) column. SDS-PAGE, ELISA and immuno-blot showed that the antibodies recovered were pure, with high antigen-binding efficiency. Thus, metal chelate CIM monoliths could be a potential alternative to conventional systems for fast and efficient purification of MAbs from the complex cell culture supernatant. Copyright © 2012 John Wiley & Sons, Ltd.

  19. Evaluation of monolithic and sub 2 microm particle packed columns for the rapid screening for illicit drugs--application to the determination of drug contamination on Irish euro banknotes.

    Science.gov (United States)

    Bones, Jonathan; Macka, Mirek; Paull, Brett

    2007-03-01

    A study comparing recently available 100 x 3 mm id, 200 x 3 mm id monolithic reversed-phase columns with a 50 x 2.1 mm id, 1.8 microm particle packed reversed-phase columns was carried out to determine the most efficient approach (using traditional van Deemter analysis and a modern kinetic plot approach) for the rapid screening of samples for 16 illicit drugs and associated metabolites. A plot of column backpressure versus plate number (N) showed a significant advantage of using the monolithic phases, with the 20 cm monolithic column exhibiting a maximum 15,000 plates at a column backpressure of approximately 70 bar, compared to approximately 7000 plates at 150 bar for the 5 cm 1.8 microm particle packed column. Optimum linear velocities were found to be 0.40 mm s(-1), 0.52 mm s(-1) and 0.98 mm s(-1) for the three above columns, respectively. The 20 cm monolithic column was subsequently applied to the separation and determination of illicit drug contamination on Irish euro banknotes, using methanol extraction followed by LC-MS/MS. Method performance data showed that the new LC-MS/MS method was significantly more sensitive than previous GC-MS/MS based methods for this application, with detection limits in the pg note(-1) region, based upon a 20 microL standard injection. All of the notes examined tested positive for trace quantities of cocaine, with benzoylecgonine detected on 12 of the 45 notes sampled. Traces of heroin were also detected on three of the 45 notes.

  20. A sensitive and robust lc-ms/ms method with monolithic column and electrospray ionization for the quantitation of efavirenz in human plasma: application to a bioequivalence study

    Directory of Open Access Journals (Sweden)

    Danilo Cesar Galindo Bedor

    2011-01-01

    Full Text Available An LC-MS/MS method has been developed for the determination of efavirenz (EFZ in human plasma using hydrochlorothiazide as internal standard (I.S.. An ESI negative mode with multiple reaction-monitoring was used monitoring the transitions m/z 313.88→69.24 (EFZ and 296.02→204.76 (I.S.. Samples were extracted using liquid-liquid extraction. The total run time was 2.0 min. The separation was achieved with HPLC-RP using a monolithic column. The assay was linear in the concentration range of 100 - 5000 ng mL-1. The mean recovery was 83%. Intra- and inter-day precision were < 9.5% and < 8.9%, respectively and accuracy was in the range ± 8.33%. The method was successfully applied to a bioequivalence study.

  1. Purification of recombinant adenovirus type 3 dodecahedric virus-like particles for biomedical applications using short monolithic columns.

    Science.gov (United States)

    Urbas, Lidija; Jarc, Barbara Lah; Barut, Miloš; Zochowska, Monika; Chroboczek, Jadwiga; Pihlar, Boris; Szolajska, Ewa

    2011-04-29

    Adenovirus type 3 dodecahedric virus-like particles (Ad3 VLP) are an interesting delivery vector. They penetrate animal cells in culture very efficiently and up to 300,000 Ad3 VLP can be observed in one cell. The purification of such particles usually consists of several steps. In these work we describe the method development and optimization for the purification of Ad3 VLP using the Convective Interaction Media analytical columns (CIMac). Results obtained with the CIMac were compared to the already established two-step purification protocol for Ad3 VLP based on sucrose density gradient ultracentifugation and the Q-Sepharose ion-exchange column. Pure, concentrated and bioactive VLP were obtained and characterized by several analytical methods. The recovery of the Ad3 VLP was more than 50% and the purified fraction was almost completely depleted of DNA; less than 1% of DNA was present. The purification protocol was shortened from five days to one day and remarkably high penetration efficacy of the CIMac-purified vector was retained. Additionally, CIMac QA analytical column has proven to be applicable for the final and in-process control of various Ad3 VLP samples. Copyright © 2011 Elsevier B.V. All rights reserved.

  2. A fast and accurate method for the pharmacokinetic research of four coumarin analogs in Fructus cnidii using capillary electro-chromatography with a methacrylate ester-based monolithic column.

    Science.gov (United States)

    Chen, Zhao; Xu, Aili; Bi, Xiaoli; Luo, Wenhui; Li, Ji; Fan, Guorong; Sun, Dongmei

    2017-11-01

    In the present study, a monolithic capillary column with higher permeability was developed for the in vivo discrimination of four coumarin analogs (bergapten, 2'-acetylangelicin, imperatorin, and osthole) that typically require long separation times in HPLC. Instead of conventional methacrylate ester monolith (containing 19.5% porogen) with insufficient permeability (K = 1.52 - 1.66 × 10 -14 M 2 ) for plasma sample, the proposed column (20.5% porogen) had better permeability (around 3.80 × 10 -14 M 2 ) while properties such as pore distribution, stability, and resolution changed slightly. As a result, due to the negatively charged electro-dynamic flow of the methacrylate ester groups in the monolith, the migration of targeted analytes was achieved within 6 min (compared with 30 min in HPLC) with acceptable resolution and improved sensitivity (0.005-0.02 μg/mL vs. 0.04 μg/mL). The proposed method was also applied to pharmacokinetic research: accelerated solvent extraction (ASE) was used to improve the extraction efficiency, which prepared extract much faster and more pure than conventional methods. As the pharmacokinetic parameters indicated, the monolithic capillary electro-chromatography method was efficient, sensitive, specific, and durable, guaranteeing its utility for the determination of multiple structure-related compounds in rat plasma. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Evaluation of fused-core and monolithic versus porous silica-based C18 columns and porous graphitic carbon for ion-pairing liquid chromatography analysis of catecholamines and related compounds.

    Science.gov (United States)

    Chirita, Raluca-Ioana; Finaru, Adriana-Luminita; Elfakir, Claire

    2011-03-15

    This paper evaluates the performances of reversed-phase (RPLC) and ion-pairing chromatography (IPLC) coupled with UV detection for the analysis of a set of 12 catecholamines and related compounds. Different chromatographic columns (porous C18-silica, perfluorinated C18-silica, porous graphitic carbon, monolithic and fused-core silica-based C18 columns) were tested using semi-long perfluorinated carboxylic acids as volatile ion-pairing reagents. Much more promising results were obtained by IPLC than by RPLC and important improvements in analytes peak symmetry and separation resolution were observed when using the "fast chromatography" columns (monolithic and fused-core C18) under IPLC conditions. For UV detection, a satisfactory separation of the 12 selected analytes was achieved in less than 20 min by using a fused-core particles column (Halo C18) and a mobile phase composed of a 1.25 mM nonafluoropentanoic acid aqueous solution and methanol under gradient elution mode. The chromatographic method developed can be directly coupled with electrospray ionization tandem mass spectrometry (ESI-MS/MS) in positive ionization mode and 10 solutes among those selected can be observed. The presence of the acidic ion-pairing reagent in the mobile phase makes this system incompatible with negative ionization mode and thus unable to detect the two acidic compounds that only responded in negative mode. In terms of MS detection, Monolithic C18 column proved to be the best one to reach the lowest detection limits (LODs) (from 0.5 ngmL(-1) to 10 ngmL(-1) depending on the neurotransmitter). The applicability of the optimized LC-MS/MS method to a "real world" sample was finally evaluated. The presence of the matrix leads to signal suppression for several solutes and thus to higher LODs. Copyright © 2011 Elsevier B.V. All rights reserved.

  4. Monolithic bed structure for capillary liquid chromatography.

    Science.gov (United States)

    Aggarwal, Pankaj; Tolley, H Dennis; Lee, Milton L

    2012-01-06

    Monolithic stationary phases show promise for LC as a result of their good permeability, ease of preparation and broad selectivity. Inorganic silica monoliths have been extensively studied and applied for separation of small molecules. The presence of a large number of through pores and small skeletal structure allows the chromatographic efficiencies of silica monoliths to be comparable to columns packed with 5 μm silica particles, at much lower back pressure. In comparison, organic polymeric monoliths have been mostly used for separation of bio-molecules; however, recently, applications are expanding to small molecules as well. Organic monoliths with high surface areas and fused morphology rather than conventional globular morphology have shown good performance for small molecule separations. Factors such as domain size, through-pore size and mesopore size of the monolithic structures have been found to govern the efficiency of monolithic columns. The structure and performance of monolithic columns are reviewed in comparison to particle packed columns. Studying and characterizing the bed structures of organic monolithic columns can provide great insights into their performance, and aid in structure-directed synthesis of new and improved monoliths. Copyright © 2011 Elsevier B.V. All rights reserved.

  5. Applications of monolithic materials for sample preparation.

    Science.gov (United States)

    Nema, Tarang; Chan, Eric C Y; Ho, Paul C

    2014-01-01

    Recent advances in monolithic columns have made them an alternative to traditional packed columns used in liquid chromatography as well as capillary electrochromatography (CEC). The monolithic columns have been extensively studied and shown to possess several advantages that make them a promising and potential substitute for the particle packed columns. A large number of papers relating to monolithic columns have been published every year, focusing on different preparation techniques, characteristic evaluations as well as applications. This review highlighted the latest development of monoliths for other modes of analytical chemistry. In particular, this review will highlight the application of monoliths for sample preparation which is an important step of the entire analysis. Copyright © 2013 Elsevier B.V. All rights reserved.

  6. A novel dilute and shoot HPLC assay method for quantification of irbesartan and hydrochlorothiazide in combination tablets and urine using second generation C18-bonded monolithic silica column with double gradient elution.

    Science.gov (United States)

    Koyuturk, Sema; Can, Nafiz Oncu; Atkosar, Zeki; Arli, Goksel

    2014-08-01

    Irbesartan (IRB) and hydrochlorothiazide (HCT) are angiotensin-II receptor antagonist and thiazide-class diuretic compounds, respectively, which are in use in the treatment of hypertension. A novel dilute-and-shoot HPLC assay method for simultaneous quantification of IRB and HCT in fixed-dose combination tablets and urine samples was described. The separation of IRB, HCT and agomelatine (internal standard) was carried out using a second generation C18-bonded monolithic silica column (Chromolith(®) High Resolution RP-18e, 100×4.6mm, Merck KGaA), utilizing both mobile phase and flow rate gradient elution programs. The analytes were detected at 230 nm wavelength using photodiode array detector within 24 minutes with high resolution, observing about 50 percent more peak capacity when using second generation C18-bonded monolithic silica column. Urine samples were introduced into the system effortlessly, with only filtration and subsequent dilution. Validation studies were performed according to the official recommendations of USP and ICH, and the developed method was successfully applied to pharmaceutical tablets and urine samples. Copyright © 2014 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

    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.

  8. 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.

    Science.gov (United States)

    Nasr, Jenny Jeehan; Shalan, Shereen; Belal, Fathalla

    2014-01-01

    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. 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. 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.

  9. Monolithic spectrometer

    Science.gov (United States)

    Rajic, Slobodan; Egert, Charles M.; Kahl, William K.; Snyder, Jr., William B.; Evans, III, Boyd M.; Marlar, Troy A.; Cunningham, Joseph P.

    1998-01-01

    A monolithic spectrometer is disclosed for use in spectroscopy. The spectrometer is a single body of translucent material with positioned surfaces for the transmission, reflection and spectral analysis of light rays.

  10. Development and application of a new in-line coupling of a miniaturized boronate affinity monolithic column with capillary zone electrophoresis for the selective enrichment and analysis of cis-diol-containing compounds.

    Science.gov (United States)

    Espina-Benitez, Maria Betzabeth; Randon, Jérôme; Demesmay, Claire; Dugas, Vincent

    2017-04-21

    An integrated, miniaturized and fully automated system was developed for the analysis (preconcentration/purification, separation and detection) of cis-diol containing molecules in complex matrices. This innovative in-line coupling system was achieved via the in-situ and localized synthesis of a short segment of silica-based monolith at the inlet of a 75-μm inner diameter fused silica capillary. The monolithic segment was locally functionalized with an acrylamide derivative of phenylboronic acid by free radical photopolymerization within 10min of irradiation time. Efficiency of the photopolymerization reaction was followed by frontal affinity chromatography of 1,2-dihydroxybenzene (catechol) as cis-diol model solute. An active-site amount of 0.43nmolcm -1 (9.8nmolμL -1 ) of phenylboronic acid moieties was obtained, with a K d value of about 290μM close to reported value for the phenyl boronate-catechol complex. The optimal conditions of use of the miniaturized boronate affinity monolithic column (μBAMC) were determined and adapted to the in-line coupling with capillary electrophoresis. Catechol was specifically preconcentrated in a pH 8.5 phosphate buffer/MeOH (80/20, v/v) mixture. A volume up to 20 times the monolith volume can be percolated with a quantitative recovery yield. Three catecholamines were purified, preconcentrated and in-line separated. Elution from the μBAMC was performed with a small plug of acidic solution, allowing field amplified sample stacking of solutes within the plug before their in-line electrophoretic separation at pH 8.75. This unique in-line coupling was successfully used for the fully automated analysis of catecholamines neurotransmitters in urine samples, highlighting the purification efficiency of the μBAMC and the potential of such a fully integrated approach. In addition to the low sample volume required (less than 2μL), the limits of detection (LOD) accomplished with this coupling were estimated at 9.0, 9.5 and 4.8ngmL -1

  11. A novel application of Onyxtrade mark monolithic column for simultaneous determination of salicylic acid and triamcinolone acetonide by sequential injection chromatography.

    Science.gov (United States)

    Chocholous, Petr; Holík, Pavel; Satínský, Dalibor; Solich, Petr

    2007-04-30

    A novel and fast simultaneous determination of triamcinolone acetonide (TCA) and salicylic acid (SA) in topical pharmaceutical formulations by sequential injection chromatography (SIC) as an alternative to classical high performance liquid chromatography (HPLC) has been developed. A recently introduced Onyxtrade mark monolithic C18 (50mmx4.6mm, Phenomenex((R))) with 5mm monolithic precolumn were used for the first time for creating sequential injection chromatography system based on a FIAlab((R)) 3000 with a six-port selection valve and 5.0mL syringe pump in study. The mobile phase used was acetonitrile/water (35:65, v/v), pH 3.3 adjusted with acetic acid at flow rate 0.9mLmin(-1). UV detection provided by fibre-optic DAD detector was set up at 240nm. Propylparaben was chosen as suitable internal standard (IS). There is only simple pre-adjustment of the sample of topical solution (dilution with mobile phase) so the analysis is not uselessly elongated. Parameters of the method showed good linearity in wide range, correlation coefficient >0.999; system precision (relative standard deviation, R.S.D.) in the range 0.45-1.95% at three different concentration levels, detection limits (3sigma) 1.00mugmL(-1) (salicylic acid), 0.66mugmL(-1) (triamcinolone acetonide) and 0.33mugmL(-1) (propylparaben) and recovery from the pharmaceutical preparations in the range 97.50-98.94%. The chromatographic resolution between peaks of compounds was more than 4.5 and analysis time was 5.1min under the optimal conditions. The advantages of sequential injection chromatography against classical HPLC are discussed and showing that SIC can be a method of option in many cases.

  12. Porous polymer monolithic col

    Directory of Open Access Journals (Sweden)

    Lydia Terborg

    2015-05-01

    Full Text Available 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 of surface coverage with the alkanethiol and mercaptoalkanoic acid ligands. Interestingly, alkanethiols coverage in a range of 4.46–4.51 molecules/nm2 significantly exceeded that of mercaptoalkanoic acids with 2.39–2.45 molecules/nm2. 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.

  13. Monolithic ceramics

    Science.gov (United States)

    Herbell, Thomas P.; Sanders, William A.

    1992-01-01

    A development history and current development status evaluation are presented for SiC and Si3N4 monolithic ceramics. In the absence of widely sought improvements in these materials' toughness, and associated reliability in structural applications, uses will remain restricted to components in noncritical, nonman-rated aerospace applications such as cruise missile and drone gas turbine engine components. In such high temperature engine-section components, projected costs lie below those associated with superalloy-based short-life/expendable engines. Advancements are required in processing technology for the sake of fewer and smaller microstructural flaws.

  14. Electrochromatographic performance of conventional and polar-embedded C16 silica monolithic stationary phases.

    Science.gov (United States)

    Ye, Fanggui; Huang, Baojun; Wang, Shun; Zhao, Shulin

    2010-11-01

    A novel monolithic silica column that has a polar-embedded amide-secondary amine group linking with C16 functionality for RP-CEC is described. The amide-secondary aminealkyloxysilane was synthesized by the reaction of 3-(2-aminoethylamino) propyltrimethoxysilane with hexadecanoyl chloride. Then, the silylant agent was bonded to the silica monolith matrix to produce hexadecanamide-secondary amine bonded silica (HDAIS) monolithic column. The electrochromatographic performance of HDAIS monolithic column for the separation of neutral, basic and polar solutes was studied, which was compared to that using the hexadecyl bonded silica monolithic column. The HDAIS monolithic column displayed reduced hydrophobic retention characteristics in the separation of five hydrophobic n-alkylbenzenes and four polar phenols when compared to the hexadecyl bonded silica monolithic column. A very much reduced silanol activity of HDAIS monolithic column was observed in the separation of test basic mixture including four aromatic amines, atenolol and metoprolol with 10 mM borate buffer (pH 7.5) containing 30% v/v ACN as the mobile phase. The comparison results indicate good performance for both polar and basic mixtures on HDAIS monolithic column in RP-CEC, and also show promising results for further applications.

  15. Immobilized monolithic enzyme reactors for application in proteomics and pharmaceutics.

    Science.gov (United States)

    Spross, Jens; Sinz, Andrea

    2009-11-01

    The use of monolithic supports for a wide variety of applications has rapidly expanded during the past few years. The examples for applications of monoliths presented herein show that the chromatographic performance of bioreactors and affinity media prepared from monolithic media is superior to that of conventional particle-based systems. The ease of fabrication and modification combined with the long lifetime of the monolithic columns and their potential to be used in fully automated analytical systems make them attractive tools for an increasing number of applications.

  16. Development of double chain phosphatidylcholine functionalized polymeric monoliths for immobilized artificial membrane chromatography.

    Science.gov (United States)

    Wang, Qiqin; Peng, Kun; Chen, Weijia; Cao, Zhen; Zhu, Peijie; Zhao, Yumei; Wang, Yuqiang; Zhou, Haibo; Jiang, Zhengjin

    2017-01-06

    This study described a simple synthetic methodology for preparing biomembrane mimicking monolithic column. The suggested approach not only simplifies the preparation procedure but also improves the stability of double chain phosphatidylcholine (PC) functionalized monolithic column. The physicochemical properties of the optimized monolithic column were characterized by scanning electron microscopy, energy-dispersive X-ray spectrometry, and nano-LC. Satisfactory column permeability, efficiency, stability and reproducibility were obtained on this double chain PC functionalized monolithic column. It is worth noting that the resulting polymeric monolith exhibits great potential as a useful alternative of commercial immobilized artificial membrane (IAM) columns for in vitro predication of drug-membrane interactions. Furthermore, the comparative study of both double chain and single chain PC functionalized monoliths indicates that the presence or absence of glycerol backbone and the number of acyl chains are not decisive for the predictive ability of IAM monoliths on drug-membrane interactions. This novel PC functionalized monolithic column also exhibited good selectivity for a protein mixture and a set of pharmaceutical compounds. Copyright © 2016 Elsevier B.V. All rights reserved.

  17. Preparation and evaluation of zirconia-coated silica monolith for capillary electrochromatography.

    Science.gov (United States)

    Shi, Z-G; Feng, Y-Q; Xu, L; Zhang, M; Da, S-L

    2004-06-17

    Silica monoliths were fabricated inside fused-silica capillaries. Then the monolithic columns were coated with membrane-like zirconia. The zirconia-coated silica monoliths exhibited different EOF behavior comparing with that of bare silica monoliths. The magnitude and direction could be manipulated by changing the running buffers. Due to the amphoteric characteristic of zirconia, the silica monoliths with zirconia surface facilitate the separation of basic compounds. Aromatic amines and alkaloids were separated without obvious peak tailing. The zirconia surface was easily modified with octadecylphosphonic acid for the separation of neutral compounds. Column efficiency as high as 90,000 and 80,000m(-1) was obtained for beberine and naphthalene, respectively. Furthermore, the zirconia coating increased the stability of the monolithic columns. Even after being exposed to severe condition, there was no apparently efficiency decrease for the test samples.

  18. Characterization of polymer monolithic stationary phases for capillary HPLC

    Czech Academy of Sciences Publication Activity Database

    Moravcová, D.; Jandera, P.; Urban, J.; Planeta, Josef

    2003-01-01

    Roč. 26, č. 11 (2003), s. 1005-1016 ISSN 1615-9306 R&D Projects: GA ČR GA203/02/0023 Institutional research plan: CEZ:AV0Z4031919; CEZ:MSM 253100002 Keywords : monolithic column s * capillary HPLC * column testing Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 2.108, year: 2003

  19. Applications of methacrylate-based monolithic supports for speciation analysis.

    Science.gov (United States)

    Scancar, Janez; Milacic, Radmila

    2009-08-01

    Liquid chromatography combined with element specific detection is commonly applied in speciation analysis. In these analyses, to obtain reliable data chemical species should not be transformed. To preserve chemical species during the separation step, fast chromatographic procedures and mild separation conditions are required. Monolithic supports that enable rapid chromatographic separations have rarely been used in speciation analysis. Methacrylate-based anion- and cation-exchange monolithic supports offer separation of charged chemical species of elements and can be used as a complementary tool to particle-packed liquid chromatographic columns. The present paper presents an overview of successful applications of methacrylate-based monolithic supports in speciation of zinc (Zn), chromium (Cr), and aluminium (Al) in environmental, occupational health, and biological samples. Measures of analytical performance of convective interaction media (CIM) monolithic chromatographic supports, namely selectivity, sensitivity, and time of analysis, are compared to those of particle-packed columns. The potential of CIM monolithic chromatography in speciation analysis is critically discussed. Direct comparison of the experimental data in speciation of elements by ion-exchange monolithic and fast protein liquid chromatography is reported for the first time. Finally, some recommendations are given for further investigations of the potential of monolithic chromatography and its implementations in different fields of element speciation analysis.

  20. Monolithic exploding foil initiator

    Science.gov (United States)

    Welle, Eric J; Vianco, Paul T; Headley, Paul S; Jarrell, Jason A; Garrity, J. Emmett; Shelton, Keegan P; Marley, Stephen K

    2012-10-23

    A monolithic exploding foil initiator (EFI) or slapper detonator and the method for making the monolithic EFI wherein the exploding bridge and the dielectric from which the flyer will be generated are integrated directly onto the header. In some embodiments, the barrel is directly integrated directly onto the header.

  1. Comparison of perfusion media and monoliths for protein and virus-like particle chromatography.

    Science.gov (United States)

    Wu, Yige; Abraham, Dicky; Carta, Giorgio

    2016-05-20

    Structural and performance characteristics of perfusion chromatography media (POROS HS 20 and 50) and those of a polymethacrylate monolith (CIM SO3-1 tube monolith column) are compared for protein and virus-like particle chromatography using 1mL columns. Axial flow columns are used for POROS while the monolith has a radial flow configuration, which provides comparable operating pressures. The POROS beads contain a bimodal distribution of pore sizes, some as large as 0.5μm, which allow a small fraction of the mobile phase to flow within the particles, while the monolith contains 1-2μm flow channels. For proteins (lysozyme and IgG), the dynamic binding capacity of the POROS columns is more than twice that of the monolith at longer residence times. While the DBC of the POROS HS 50 column decreases at shorter residence times, the DBC of the POROS HS 20 column for IgG remains nearly twice that of the monolith at residence times at least as low as 0.2min as a result of intraparticle convection. Protein recoveries are comparable for all three columns. For VLPs, however, the eluted peaks are broader and recovery is lower for the monolith than for the POROS columns and is dependent on the direction of flow in the monolith, which is attributed to denser layer observed by SEM at the inlet surface of the monolith that appears to trap VLPs when loading in the normal flow direction. Copyright © 2016 Elsevier B.V. All rights reserved.

  2. Large volume monolithic stationary phases: preparation, properties, and applications.

    Science.gov (United States)

    Podgornik, Aleš; Jančar, Janez; Mihelič, Igor; Barut, Miloš; Strancar, Aleš

    2010-03-01

    Monoliths represents the 4th generation of chromatographic supports. They consist of a single piece of highly porous material with interconnected flow through pores. Because of that transport is based on convection what results in a flow unaffected separation and dynamic binding capacity. This is especially important when large molecular weight molecules such as proteins, DNA or viruses have to be purified. For this purpose large volume monolithic columns are needed. In this article preparation of such columns is described together with their main applications. The article is dedicated to Prof. Tine Koloini who substantially contributed to this topic.

  3. A monolithic white laser.

    Science.gov (United States)

    Fan, Fan; Turkdogan, Sunay; Liu, Zhicheng; Shelhammer, David; Ning, C Z

    2015-09-01

    Monolithic semiconductor lasers capable of emitting over the full visible-colour spectrum have a wide range of important applications, such as solid-state lighting, full-colour displays, visible colour communications and multi-colour fluorescence sensing. The ultimate form of such a light source would be a monolithic white laser. However, realizing such a device has been challenging because of intrinsic difficulties in achieving epitaxial growth of the mismatched materials required for different colour emission. Here, we demonstrate a monolithic multi-segment semiconductor nanosheet based on a quaternary alloy of ZnCdSSe that simultaneously lases in the red, green and blue. This is made possible by a novel nanomaterial growth strategy that enables separate control of the composition, morphology and therefore bandgaps of the segments. Our nanolaser can be dynamically tuned to emit over the full visible-colour range, covering 70% more perceptible colours than the most commonly used illuminants.

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

    Science.gov (United States)

    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.

  5. Embedded-monolith armor

    Science.gov (United States)

    McElfresh, Michael W.; Groves, Scott E; Moffet, Mitchell L.; Martin, Louis P.

    2016-07-19

    A lightweight armor system utilizing a face section having a multiplicity of monoliths embedded in a matrix supported on low density foam. The face section is supported with a strong stiff backing plate. The backing plate is mounted on a spall plate.

  6. Rapid recovery of DNA from agarose gel slices by coupling electroelution with monolithic SPE.

    Science.gov (United States)

    Yu, Shengbing; Yang, Shuixian; Zhou, Ping; Zhou, Ke; Wang, Jing; Chen, Xiangdong

    2009-06-01

    An amino silica monolithic column prepared by in situ polymerization of tetraethoxysilane and N-(beta-aminoethyl)-gamma-aminopropyltriethoxysilane was firstly applied to recover DNA from agarose gel slices by coupling electroelution with monolithic SPE. DNA was electroeluted from the agarose gel slices onto the amino silica monolithic column. The DNA adsorbed on this monolithic column was then recovered using sodium phosphate solution at pH 10. The whole recovery procedure could be completed within 10 min because the use of amino silica monolithic column accelerated the DNA capture and facilitated the DNA release. Electroelution conditions, such as buffer pH, buffer concentration and applied voltage, were online optimized. The average yield for herring sperm DNA, pBR 322 DNA and lambda DNA recovered from 1.0% w/v agarose gel slices were 55+/-4, 50+/-6 and 42+/-7% (n=3), respectively. The polymerase chain reaction performance of pGM plasmid recovered from agarose gel slices demonstrated that the method could provide high-quality DNA for downstream processes. The combination of electroelution with monolithic SPE allows a rapid, simple and efficient DNA recovery method. This technique is especially useful for applications that need to purify small starting amounts of DNA.

  7. Intact-protein trapping columns for proteomic analysis in capillary high-performance liquid chromatography.

    Science.gov (United States)

    Guan, Xia; Yan, Guoquan; Gao, Mingxia; Hong, Guangfeng; Deng, Chunhui; Zhang, Xiangmin

    2010-10-29

    A new type of monolithic trapping columns with high mechanical strength was prepared by thin-layer sol-gel coating method and applied to trapping intact proteins for on-line capillary liquid chromatography. Monolithic trapping columns were fabricated by entrapping C8 reversed-phase particles into the capillary columns through a sol-gel network, which was formed by hydrolysis and polycondensation of methyltriethoxysilane. Hundreds times of trapping/untrapping for intact proteins were carried out. The trapping columns showed long-term stability up to 300 bar. Recovery, loading capacity and reproducibility of trapping columns were evaluated using four proteins. The recovery of four protein mixtures for the C8 monolithic trapping columns was 99.3% on average. The loading capacity of 5 mm × 320 μm i.d. C8 trapping columns for the protein mixtures was 30 μg. Day-to-day relative standard deviation (RSD) values for recoveries of protein mixtures on the same C8 trapping column ranged from 2.34 to 5.87%, column-to-column RSD values were from 3.01 to 6.81%. The C8 trapping columns were used to trap normal mouse liver intact proteins in a capillary liquid chromatography system. Results demonstrated high efficiency of the monolithic trapping columns for trapping intact proteins for proteomic analysis in on-line capillary liquid chromatography system. Copyright © 2010 Elsevier B.V. All rights reserved.

  8. Bioaffinity chromatography on monolithic supports

    NARCIS (Netherlands)

    Tetala, K.K.R.; Beek, van T.A.

    2010-01-01

    Affinity chromatography on monolithic supports is a powerful analytical chemical platform because it allows for fast analyses, small sample volumes, strong enrichment of trace biomarkers and applications in microchips. In this review, the recent research using monolithic materials in the field of

  9. Monoliths from poly(ethylene glycol) diacrylate and dimethacrylate for capillary hydrophobic interaction chromatography of proteins.

    Science.gov (United States)

    Li, Yuanyuan; Tolley, H Dennis; Lee, Milton L

    2010-07-23

    Rigid monoliths were synthesized solely from poly(ethylene glycol) diacrylates (PEGDA) or poly(ethylene glycol) dimethacrylates (PEGDMA) containing different ethylene glycol chain lengths by one-step UV-initiated polymerization. Methanol/ethyl ether and cyclohexanol/decanol were used as bi-porogen mixtures for the PEGDA and PEGDMA monoliths, respectively. Effects of PEG chain length, bi-porogen ratio and reaction temperature on monolith morphology and back pressure were investigated. For tri- and tetra-ethylene glycol diacrylates (i.e., PEGDA 258 and PEGDA 302), most combinations of methanol and ethyl ether were effective in forming monoliths, while for diacrylates containing longer chain lengths (i.e., PEGDA 575 and PEGDA 700), polymerization became more sensitive to the bi-porogen ratio. A similar tendency was also observed for PEGDMA monomers. Polymerization of monoliths was conducted at approximately 0 degrees C and room temperature, which produced significant differences in monolith morphology and permeability. Monoliths prepared from PEGDA 258 were found to provide the best chromatographic performance with respect to peak capacity and resolution in hydrophobic interaction chromatography (HIC). Detailed study of these monoliths demonstrated that chromatographic performance was not affected by changing the ratios of the two porogens, but resulted in almost identical retention times and comparable peak capacities. An optimized PEGDA 258 monolithic column was able to separate proteins using a 20-min elution gradient with a peak capacity of 62. Mass recoveries for test proteins were found to be greater than 90, indicating its excellent biocompatibility. All monoliths demonstrated nearly no swelling or shrinking in different polarity solvents, and most of them could be stored dry, indicating excellent stability due to their highly crosslinked networks. The preparation of these in situ polymerized single-monomer monolithic columns was highly reproducible. The

  10. Preparation and characterization of poly-(methacrylatoethyl trimethylammonium chloride-co-vinylbenzyl chloride-co-ethylene dimethacrylate monolith

    Directory of Open Access Journals (Sweden)

    Eko Malis

    2015-05-01

    Full Text Available A polymer monolithic column, poly-(methacrylatoethyltrimethylammonium chloride-co-vinylbenzyl chloride-co-ethylene dimethacrylate or poly-(MATE-co-VBC-co-EDMA was successfully prepared in the current study by one-step thermally initiated in situ polymerization, confined in a steel tubing of 0.5 mm i.d. and 1/16” o.d. The monoliths were prepared from methacrylatoethyltrimethylammonium chloride (MATE and vinylbenzyl chloride (VBC as monomer and ethylene dimethacrylate (EDMA as crosslinker using a binary porogen system of 1-propanol and 1,4-butanediol. The inner wall of steel tubing was pretreated with 3-methacryloxypropyl-trimethoxysilane (MAPS. In order to obtain monolith with adequate column efficiency and low flow resistance, some parameters such as total monomer concentration (%T and crosslinker concentration (%C were optimized. The morphology of this monolith was assessed by scanning electron microscopy (SEM. The properties of the monolithic column, such as permeability, binding capacity, and pore size distribution were also characterized in detail. From the results of the characterization of all monolith variation, monolith with %T 30 %C 50 and %T 35 %C 50 give the best characteristic. These monoliths have high permeability, adequate molecular recognition sites (represented with binding capacity value of over 20 mg/mL, and have over 80% flow through pores in their pore structure contribute to low flow resistance. The resulted monolithic columns have promising potential for dual mode liquid chromatography. MATE may contribute for anion-exchange while VBC may responsible for reversed-phase liquid chromatography.

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

    NARCIS (Netherlands)

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

    2003-01-01

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

  12. Silver-coated monolithic columns for separation in radiopharmaceutical applications

    Czech Academy of Sciences Publication Activity Database

    Sedláček, Ondřej; Kučka, Jan; Švec, F.; Hrubý, Martin

    2014-01-01

    Roč. 37, č. 7 (2014), s. 798-802 ISSN 1615-9306 R&D Projects: GA ČR GA202/09/2078; GA MPO FR-TI4/625 Grant - others:AV ČR(CZ) M200501201 Program:M Institutional support: RVO:61389013 Keywords : capture * Iodide * Iodine Subject RIV: BO - Biophysics Impact factor: 2.737, year: 2014

  13. High efficiency polyethylene glycol diacrylate monoliths for reversed-phase capillary liquid chromatography of small molecules.

    Science.gov (United States)

    Aggarwal, Pankaj; Lawson, John S; Tolley, H Dennis; Lee, Milton L

    2014-10-17

    Highly cross-linked monolithic networks (i.e., polyethylene glycol diacrylate, PEGDA) synthesized from monomers containing varying ethylene oxide chain lengths were fabricated inside fused silica capillary columns for use in liquid chromatography (LC) of small molecules. Tergitol was used as a surfactant porogen in combination with other typical organic liquid porogens. Column performance was correlated with quantitative descriptors of the physical/chemical properties of the monomers and porogens using a statistical model. Solubility and viscosity values of the components were identified as important predictors of monolith morphology and efficiency. The chromatographic retention mechanism was determined to be principally reversed-phase (RP) with additional hydrogen bonding between the polar groups of the analytes and the ethylene oxide groups embedded in the monolith structure. The fabricated monolithic columns were evaluated under RPLC conditions using phenols, hydroxy benzoic acids, and alkyl parabens as test compounds. Isocratic elution of hydroxy benzoic acids at a linear velocity of 0.04 cm/s using a PEGDA-700 monolith gave chromatographic peaks with little tailing (i.e., tailing factorcolumn was 186,000 plates/m when corrected for injector dead volume. High resolution gradient separations of selected pharmaceutical compounds and phenylurea herbicides were achieved in less than 18 min. Optimized monoliths synthesized from all four crosslinking monomers exhibited high permeability and demonstrated little swelling or shrinking in different polarity solvents. Column preparation was highly reproducible, with relative standard deviation (RSD) values less than 2.1%, based on retention times of the phenol standards (3 different columns). Copyright © 2014 Elsevier B.V. All rights reserved.

  14. A Monolithically-Integrated μGC Chemical Sensor System

    Directory of Open Access Journals (Sweden)

    Davor Copic

    2011-06-01

    Full Text Available Gas chromatography (GC is used for organic and inorganic gas detection with a range of applications including screening for chemical warfare agents (CWA, breath analysis for diagnostics or law enforcement purposes, and air pollutants/indoor air quality monitoring of homes and commercial buildings. A field-portable, light weight, low power, rapid response, micro-gas chromatography (μGC system is essential for such applications. We describe the design, fabrication and packaging of mGC on monolithically-integrated Si dies, comprised of a preconcentrator (PC, μGC column, detector and coatings for each of these components. An important feature of our system is that the same mechanical micro resonator design is used for the PC and detector. We demonstrate system performance by detecting four different CWA simulants within 2 min. We present theoretical analyses for cost/power comparisons of monolithic versus hybrid μGC systems. We discuss thermal isolation in monolithic systems to improve overall performance. Our monolithically-integrated μGC, relative to its hybrid cousin, will afford equal or slightly lower cost, a footprint that is 1/2 to 1/3 the size and an improved resolution of 4 to 25%.

  15. A monolithically-integrated μGC chemical sensor system.

    Science.gov (United States)

    Manginell, Ronald P; Bauer, Joseph M; Moorman, Matthew W; Sanchez, Lawrence J; Anderson, John M; Whiting, Joshua J; Porter, Daniel A; Copic, Davor; Achyuthan, Komandoor E

    2011-01-01

    Gas chromatography (GC) is used for organic and inorganic gas detection with a range of applications including screening for chemical warfare agents (CWA), breath analysis for diagnostics or law enforcement purposes, and air pollutants/indoor air quality monitoring of homes and commercial buildings. A field-portable, light weight, low power, rapid response, micro-gas chromatography (μGC) system is essential for such applications. We describe the design, fabrication and packaging of μGC on monolithically-integrated Si dies, comprised of a preconcentrator (PC), μGC column, detector and coatings for each of these components. An important feature of our system is that the same mechanical micro resonator design is used for the PC and detector. We demonstrate system performance by detecting four different CWA simulants within 2 min. We present theoretical analyses for cost/power comparisons of monolithic versus hybrid μGC systems. We discuss thermal isolation in monolithic systems to improve overall performance. Our monolithically-integrated μGC, relative to its hybrid cousin, will afford equal or slightly lower cost, a footprint that is 1/2 to 1/3 the size and an improved resolution of 4 to 25%.

  16. PULSE COLUMN

    Science.gov (United States)

    Grimmett, E.S.

    1964-01-01

    This patent covers a continuous countercurrent liquidsolids contactor column having a number of contactor states each comprising a perforated plate, a layer of balls, and a downcomer tube; a liquid-pulsing piston; and a solids discharger formed of a conical section at the bottom of the column, and a tubular extension on the lowest downcomer terminating in the conical section. Between the conical section and the downcomer extension is formed a small annular opening, through which solids fall coming through the perforated plate of the lowest contactor stage. This annular opening is small enough that the pressure drop thereacross is greater than the pressure drop upward through the lowest contactor stage. (AEC)

  17. Assessment of the Grouted IXC Monolith in Support of K East Basin Hazard Categorization

    Energy Technology Data Exchange (ETDEWEB)

    Short, Steven M.; Dodson, Michael G.; Alzheimer, James M.; Meyer, Perry A.

    2007-10-12

    Addendum to original report updating the structural analysis of the I-beam accident to reflect a smaller I-beam than originally assumed (addendum is 2 pages). The K East Basin currently contains six ion exchange columns (IXCs) that were removed from service over 10 years ago. Fluor Hanford plans to immobilize the six ion exchange columns (IXCs) in place in a concrete monolith. PNNL performed a structural assessment of the concrete monolith to determine its capability to absorb the forces imposed by postulated accidents and protect the IXCs from damage and thus prevent a release of radioactive material. From this assessment, design specifications for the concrete monolith were identified that would prevent a release of radioactive material for any of the postulated hazardous conditions.

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

    Science.gov (United States)

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

    2013-04-05

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

  19. Monolithic metal oxide transistors.

    Science.gov (United States)

    Choi, Yongsuk; Park, Won-Yeong; Kang, Moon Sung; Yi, Gi-Ra; Lee, Jun-Young; Kim, Yong-Hoon; Cho, Jeong Ho

    2015-04-28

    We devised a simple transparent metal oxide thin film transistor architecture composed of only two component materials, an amorphous metal oxide and ion gel gate dielectric, which could be entirely assembled using room-temperature processes on a plastic substrate. The geometry cleverly takes advantage of the unique characteristics of the two components. An oxide layer is metallized upon exposure to plasma, leading to the formation of a monolithic source-channel-drain oxide layer, and the ion gel gate dielectric is used to gate the transistor channel effectively at low voltages through a coplanar gate. We confirmed that the method is generally applicable to a variety of sol-gel-processed amorphous metal oxides, including indium oxide, indium zinc oxide, and indium gallium zinc oxide. An inverter NOT logic device was assembled using the resulting devices as a proof of concept demonstration of the applicability of the devices to logic circuits. The favorable characteristics of these devices, including (i) the simplicity of the device structure with only two components, (ii) the benign fabrication processes at room temperature, (iii) the low-voltage operation under 2 V, and (iv) the excellent and stable electrical performances, together support the application of these devices to low-cost portable gadgets, i.e., cheap electronics.

  20. Monoliths in capillary electrochromatography and capillary liquid chromatography in conjunction with mass spectrometry

    Czech Academy of Sciences Publication Activity Database

    Moravcová, Dana; Rantamäki, A. H.; Duša, Filip; Wiedmer, S. K.

    2016-01-01

    Roč. 37, 7-8 (2016), s. 880-912 ISSN 0173-0835 Institutional support: RVO:68081715 Keywords : capillary electrochromatography * capillary liquid chromatography * mass spec- trometry * monolithic columns Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 2.744, year: 2016

  1. Fabrication and chromatographic performance of porous-shell pillar-arry columns

    NARCIS (Netherlands)

    Detobel, Frederik; De Bruyne, Selm; de Bruyne, S.; Vangelooven, Joris; de Malsche, Wim; Aerts, Tim; Terryn, Herman; Gardeniers, Johannes G.E.; Eeltink, Sebastiaan; Desmet, Gert

    2010-01-01

    We report on a new approach to obtain highly homogeneous silica-monolithic columns, applying a sol−gel fabrication process inside a rectangular pillar-array column (1 mm in width, 29 μm in height and 33.75 mm in length) having a cross-sectional area comparable to that of a 200 μm diameter circular

  2. Use of monolithic supports for high-throughput protein and peptide separation in proteomics.

    Science.gov (United States)

    Andjelković, Uroš; Tufegdžić, Srdjan; Popović, Milica

    2017-11-01

    The exclusive properties of monolithic supports enable fast mass transfer, high porosity, low back pressure, easy preparation process and miniaturisation, and the availability of different chemistries make them particularly suitable materials for high-throughput (HTP) protein and peptide separation. In this review recent advances in monolith-based chromatographic supports for HTP screening of protein and peptide samples are presented and their application in HTP sample preparation (separation, enrichment, depletion, proteolytic digestion) for HTP proteomics is discussed. Development and applications of different monolithic capillary columns in HTP MS-based bottom-up and top-down proteomics are overviewed. By discussing the chromatographic conditions and the mass spectrometric data acquisition conditions an attempt is made to present currently demonstrated capacities of monolithic capillary columns for HTP identification and quantification of proteins and peptides from complex biological samples by MS-based proteomics. Some recent advances in basic monolith technology of importance for proteomics are also discussed. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Acoustic of monolithic dome structures

    Directory of Open Access Journals (Sweden)

    Mostafa Refat Ismail

    2018-03-01

    The interior of monolithic domes have perfect, concave shapes to ensure that sound travels through the dome and perfectly collected at different vocal points. These dome structures are utilized for domestic use because the scale allows the focal points to be positioned across daily life activities, thereby affecting the sonic comfort of the internal space. This study examines the various acoustic treatments and parametric configurations of monolithic dome sizes. A geometric relationship of acoustic treatment and dome radius is established to provide architects guidelines on the correct selection of absorption needed to maintain the acoustic comfort of these special spaces.

  4. Preparation of porous polymer monoliths featuring enhanced surface coverage with gold nanoparticles

    KAUST Repository

    Lv, Yongqin

    2012-10-01

    A new approach to the preparation of porous polymer monoliths with enhanced coverage of pore surface with gold nanoparticles has been developed. First, a generic poly(glycidyl methacrylate-co-ethylene dimethacrylate) monolith was reacted with cystamine followed by the cleavage of its disulfide bonds with tris(2-carboxylethyl)phosphine, which liberated the desired thiol groups. Dispersions of gold nanoparticles with sizes varying from 5 to 40. nm were then pumped through the functionalized monoliths. The materials were then analyzed using both energy dispersive X-ray spectroscopy and thermogravimetric analysis. We found that the quantity of attached gold was dependent on the size of nanoparticles, with the maximum attachment of more than 60. wt% being achieved with 40. nm nanoparticles. Scanning electron micrographs of the cross sections of all the monoliths revealed the formation of a non-aggregated, homogenous monolayer of nanoparticles. The surface of the bound gold was functionalized with 1-octanethiol and 1-octadecanethiol, and these monolithic columns were used successfully for the separations of proteins in reversed phase mode. The best separations were obtained using monoliths modified with 15, 20, and 30. nm nanoparticles since these sizes produced the most dense coverage of pore surface with gold. © 2012 Elsevier B.V.

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

    Science.gov (United States)

    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.

  6. THE PECULIARITIES OF DESIGNING OF MONOLITHIC FOUNDATION SLABS IN BANGLADESH

    Directory of Open Access Journals (Sweden)

    Анна Николаевна Малахова

    2017-05-01

    Full Text Available The climatic and engineering-geological conditions of the construction sites for civil buildings in the People's Republic of Bangladesh are considered. There are described the features of the constructive solution of load-bearing structures of buildings of mass urban development. Monolithic reinforced concrete buildings of medium height of column and wall construction systems are considered, and the average ground pressure is determined. There are shown the slabs foundations of such buildings, the features of their design and reinforcement, including under the conditions of seismic influences.

  7. Monolithic fiber optic sensor assembly

    Science.gov (United States)

    Sanders, Scott

    2015-02-10

    A remote sensor element for spectrographic measurements employs a monolithic assembly of one or two fiber optics to two optical elements separated by a supporting structure to allow the flow of gases or particulates therebetween. In a preferred embodiment, the sensor element components are fused ceramic to resist high temperatures and failure from large temperature changes.

  8. UV-LED photopolymerised monoliths

    Czech Academy of Sciences Publication Activity Database

    Abele, S.; Nie, F.; Foret, František; Paull, B.; Macka, M.

    2008-01-01

    Roč. 133, č. 7 (2008), s. 864-866 ISSN 0003-2654 R&D Projects: GA AV ČR KAN400310651 Institutional research plan: CEZ:AV0Z40310501 Keywords : photopolymerisation * UV-LED * polymethacrylate monolith Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.761, year: 2008

  9. Porous polymer monoliths functionalized through copolymerization of a C60 fullerene-containing methacrylate monomer for highly efficient separations of small molecules

    KAUST Repository

    Chambers, Stuart D.

    2011-12-15

    Monolithic poly(glycidyl methacrylate-co-ethylene dimethacrylate) and poly(butyl methacrylate-co-ethylene dimethacrylate) capillary columns, which incorporate the new monomer [6,6]-phenyl-C 61-butyric acid 2-hydroxyethyl methacrylate ester, have been prepared and their chromatographic performance have been tested for the separation of small molecules in the reversed phase. While addition of the C60-fullerene monomer to the glycidyl methacrylate-based monolith enhanced column efficiency 18-fold, to 85 000 plates/m at a linear velocity of 0.46 mm/s and a retention factor of 2.6, when compared to the parent monolith, the use of butyl methacrylate together with the carbon nanostructured monomer afforded monolithic columns with an efficiency for benzene exceeding 110 000 plates/m at a linear velocity of 0.32 mm/s and a retention factor of 4.2. This high efficiency is unprecedented for separations using porous polymer monoliths operating in an isocratic mode. Optimization of the chromatographic parameters affords near baseline separation of 6 alkylbenzenes in 3 min with an efficiency of 64 000 plates/m. The presence of 1 wt % or more of water in the polymerization mixture has a large effect on both the formation and reproducibility of the monoliths. Other factors such as nitrogen exposure, polymerization conditions, capillary filling method, and sonication parameters were all found to be important in producing highly efficient and reproducible monoliths. © 2011 American Chemical Society.

  10. Behavior of reinforced concrete columns strenghtened by partial jacketing

    Directory of Open Access Journals (Sweden)

    D. B. FERREIRA

    Full Text Available This article presents the study of reinforced concrete columns strengthened using a partial jacket consisting of a 35mm self-compacting concrete layer added to its most compressed face and tested in combined compression and uniaxial bending until rupture. Wedge bolt connectors were used to increase bond at the interface between the two concrete layers of different ages. Seven 2000 mm long columns were tested. Two columns were cast monolithically and named PO (original column e PR (reference column. The other five columns were strengthened using a new 35 mm thick self-compacting concrete layer attached to the column face subjected to highest compressive stresses. Column PO had a 120mm by 250 mm rectangular cross section and other columns had a 155 mm by 250mm cross section after the strengthening procedure. Results show that the ultimate resistance of the strengthened columns was more than three times the ultimate resistance of the original column PO, indicating the effectiveness of the strengthening procedure. Detachment of the new concrete layer with concrete crushing and steel yielding occurred in the strengthened columns.

  11. Review on recent and advanced applications of monoliths and related porous polymer gels in micro-fluidic devices.

    Science.gov (United States)

    Vázquez, Mercedes; Paull, Brett

    2010-06-04

    This review critically summarises recent novel and advanced achievements in the application of monolithic materials and related porous polymer gels in micro-fluidic devices appearing within the literature over the period of the last 5 years (2005-2010). The range of monolithic materials has developed rapidly over the past decade, with a diverse and highly versatile class of materials now available, with each exhibiting distinct porosities, pore sizes, and a wide variety of surface functionalities. A major advantage of these materials is their ease of preparation in micro-fluidic channels by in situ polymerisation, leading to monolithic materials being increasingly utilised for a larger variety of purposes in micro-fluidic platforms. Applications of porous polymer monoliths, silica-based monoliths and related homogeneous porous polymer gels in the preparation of separation columns, ion-permeable membranes, preconcentrators, extractors, electrospray emitters, micro-valves, electrokinetic pumps, micro-reactors and micro-mixers in micro-fluidic devices are discussed herein. Procedures used in the preparation of monolithic materials in micro-channels, as well as some practical aspects of the micro-fluidic chip fabrication are addressed. Recent analytical/bioanalytical and catalytic applications of the final micro-fluidic devices incorporating monolithic materials are also reviewed. Copyright 2010 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

    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 ions). The monolithic chelating ion-exchanger was applied to the separation of alkaline earth and transition metal ions spiked in natural and potable waters.

  13. Peptide immobilized monolith containing tentacle-type functionalized polymer chains for high-capacity binding of immunoglobulin G.

    Science.gov (United States)

    Du, Kaifeng

    2014-12-29

    A peptide immobilized tentacle-type monolith is developed here for high-performance IgG purification. In this work, the glucose-anchored GMA molecules serve as monomers to be grafted into the tentacle-type chains on highly porous monolith by a series of chemical reactions. While maintaining high column permeability, the tentacle grafting endows the monolith with lots of reactive handles to anchor more peptides. With that, the grafted monolith shows high peptide density of about 155μmolmL(-1), up to approximately 4.7 times higher over the ungrafted one (33μmolmL(-1)). As a result, the static adsorbing capacity and dynamic adsorption capacity at 50% breakthrough point reach 101.8 and 83.3mgmL(-1) for IgG adsorption, respectively. Regeneration, recycle and reuse of grafted monolith are highly successful for 25 runs without obvious capacity loss. By taking these advantages of high capacity and excellent structure stability, the affinity grafted monolith is evaluated by using cleared human blood supernatant. And the result shows the peptide immobilized tentacle type monolith displays excellent specificity and high effectiveness for IgG purification. Copyright © 2014 Elsevier B.V. All rights reserved.

  14. Experimental characterization of the transport phenomena, adsorption, and elution in a protein A affinity monolithic medium.

    Science.gov (United States)

    Herigstad, M Omon; Dimartino, Simone; Boi, Cristiana; Sarti, Giulio C

    2015-08-14

    A commercially available convective interaction media (CIM) Protein A monolithic column was fully characterized in view of its application for the affinity capture of IgG in monoclonal antibody production processes. By means of moment analysis, the interstitial porosity and axial dispersion coefficient were determined. The frontal analysis method of characteristic points was employed, for the first time with monolithic media, to determine the dynamic binding capacity. The effects of the flow rate and pH on the total recovery of polyclonal IgG and elution profile were evaluated. A comparison with literature data for Protein A chromatography beads demonstrate the superior bed utilization of monolithic media, which gave better performance at lower residence times. Copyright © 2015 Elsevier B.V. All rights reserved.

  15. Strong cation-exchange chromatography of proteins on a sulfoalkylated monolithic cryogel.

    Science.gov (United States)

    Perçin, Işık; Khalaf, Rushd; Brand, Bastian; Morbidelli, Massimo; Gezici, Orhan

    2015-03-20

    A new strong cation exchanger (SCX) monolithic column was synthesized by at-line surface modification of a cryogel prepared by copolymerization of 2-hydroxyethylmethacrylate (HEMA) and glycidylmethacrylate (GMA). Sodium salt of 3-Mercaptopropane sulfonic acid (3-MPS) was used as the ligand to transform the surface of the monolith into a strong cation exchanger. The obtained material was characterized in terms of elemental analysis, infrared spectroscopy (FTIR), Scanning Electron Microscopy (SEM), Brunauer-Emmett-Teller (BET) N2 adsorption, and used as a stationary phase for strong-cation exchange chromatography of some proteins, such as α-chymotrypsinogen, cytochrome c and lysozyme. Water permeability of the column was calculated according to Darcy's law (2.66×10(-13)m(2)). The performance of the monolithic cryogel column was evaluated on the basis of Height Equivalent to a Theoretical Plate (HETP). Retention behavior of the studied proteins was modeled on the basis of Yamamoto model to understand the role of the ion-exchange mechanism in retention behaviors. The considered proteins were successfully separated, and the obtained chromatogram was compared with that obtained with a non-functionalized cryogel column. Copyright © 2015 Elsevier B.V. All rights reserved.

  16. Monolithic pattern-sensitive detector

    Science.gov (United States)

    Berger, Kurt W.

    2000-01-01

    Extreme ultraviolet light (EUV) is detected using a precisely defined reference pattern formed over a shallow junction photodiode. The reference pattern is formed in an EUV absorber preferably comprising nickel or other material having EUV- and other spectral region attenuating characteristics. An EUV-transmissive energy filter is disposed between a passivation oxide layer of the photodiode and the EUV transmissive energy filter. The device is monolithically formed to provide robustness and compactness.

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

    Science.gov (United States)

    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.

  18. Hypercrosslinked large surface area porous polymer monoliths for hydrophilic interaction liquid chromatography of small molecules featuring zwitterionic functionalities attached to gold nanoparticles held in layered structure

    OpenAIRE

    Lv, Yongqin; Lin, Zhixing; Svec, Frantisek

    2012-01-01

    A novel approach to porous polymer monoliths hypercrosslinked to obtain large surface areas and modified with zwitterionic functionalities through the attachment of gold nanoparticles in a layered architecture has been developed. The capillary columns were used for the separation of small molecules in hydrophilic interaction liquid chromatography mode. First, a monolith with a very large surface area of 430 m2/g was prepared by hypercrosslinking from a generic poly(4-methylstyrene-co-vinylben...

  19. Phosphatidylcholine covalently linked to a methacrylate-based monolith as a biomimetic stationary phase for capillary liquid chromatography

    Czech Academy of Sciences Publication Activity Database

    Moravcová, Dana; Carrasco-Correa, E. J.; Planeta, Josef; Lämmerhofer, M.; Wiedmer, S. K.

    2015-01-01

    Roč. 1402, JUL (2015), s. 27-35 ISSN 0021-9673 R&D Projects: GA MV VG20112015021 Institutional support: RVO:68081715 Keywords : Capillary LC * analyte–membrane interaction * monolithic column * phospholipids Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.926, year: 2015 http://hdl.handle.net/11104/0247268

  20. Phosphatidylcholine covalently linked to a methacrylate-based monolith as a biomimetic stationary phase for capillary liquid chromatography

    Czech Academy of Sciences Publication Activity Database

    Moravcová, Dana; Carrasco-Correa, E. J.; Planeta, Josef; Lämmerhofer, M.; Wiedmer, S. K.

    2015-01-01

    Roč. 1402, JUL (2015), s. 27-35 ISSN 0021-9673 R&D Projects: GA MV VG20112015021 Institutional support: RVO:68081715 Keywords : Capillary LC * analyte–membrane interaction * monolithic column * phospholipids Subject RIV: CB - Analytical Chemistry , Separation Impact factor: 3.926, year: 2015 http://hdl.handle.net/11104/0247268

  1. A high boronate avidity monolithic capillary for the selective enrichment of trace glycoproteins.

    Science.gov (United States)

    Li, Daojin; Li, Yang; Li, Xinglin; Bie, Zijun; Pan, Xianghua; Zhang, Qian; Liu, Zhen

    2015-03-06

    Boronate affinity materials, as effective sample enrichment sorbents for glycoproteomic analysis, have attracted increasing attention in recent years. However, most of boronate affinity materials suffer from an apparent limitation, limited binding strength. As a result, extraction of glycoproteins of trace concentration is rather difficult or impossible. In this study, we present a high boronate avidity monolithic capillary. Branched polyethyleneimine (PEI) was used as a scaffold to amplify the number of boronic acid moieties. While 2,4-difluoro-3-formyl-phenylboronic acid (DFFPBA), which exhibited ultrahigh affinity toward cis-diol-containing compounds, was employed as an affinity ligand. Due to the PEI-assisted synergistic multivalent binding, the monolithic column exhibited high boronate avidity toward glycoproteins, with binding constants of 10(-6)-10(-7)M. Such binding strength was the highest among already reported boronic acid-functionalized materials that can be used for glycoproteomic analysis. Besides, the boronate avidity monolithic column exhibited one additional beneficial feature, lowered binding pH (≥6.5). These features greatly favored the selective enrichment of trace glycoproteins from real samples. The feasibility for practical applications was demonstrated with the selective enrichment of trace glycoproteins in human saliva. As compared with other boronate avidity/affinity materials, the boronate avidity monolithic capillary exhibited the best performance. Copyright © 2015 Elsevier B.V. All rights reserved.

  2. Downscaling limits and confinement effects in the miniaturization of porous polymer monoliths in narrow bore capillaries.

    Science.gov (United States)

    Nischang, Ivo; Svec, Frantisek; Fréchet, Jean M J

    2009-09-01

    Monolithic poly(butyl methacrylate-co-ethylene dimethacrylate) columns have been prepared in capillaries ranging in inner diameter from 5 to 75 microm using thermally initiated free-radical polymerization of a mixture of butyl methacrylate, ethylene dimethacrylate, and porogens at different temperatures. Scanning electron microscopy and the measurement of hydrodynamic properties reveal that the downward scalability of the monolithic columns is greatly affected by the confinement effect of the capillary wall resulting from the decreased volume-to-surface ratio as the capillary diameter is decreased. The downscaling process is affected most by the polymerization temperature, the diffusion of the propagating radicals, and the density of coverage of polymerizable groups on the inner walls of the capillary. Optimization of all these factors enables the preparation of monolithic structures in capillaries with inner diameters as low as 5 microm while retaining the desirable properties of monoliths prepared in much larger capillaries. Under these conditions, formation of undesired dense polymer layers attached to the capillary wall was minimized. The chromatographic performance of 10, 25, and 50 microm capillaries evaluated in the reversed phase gradient separation of three proteins showed no change in elution times at identical flow velocities and gradient times, while peak elution width was the smallest with the narrowest capillary.

  3. Fingerprint development for Ginkgo biloba extracts by pressurized capillary electrochromatography: comparison of column types.

    Science.gov (United States)

    Wang, Jiajing; Tanret, Indiana; Mangelings, Debby; Fan, Guorong; Wu, Yutian; Vander Heyden, Yvan

    2010-07-01

    A pressurized capillary electrochromatographic (pCEC) fingerprint of Ginkgo biloba leaf extract was developed on three different types of capillary columns. A commercial column packed with 3-microm particles and an in-house column packed with 5-microm particles were investigated for their performance. Additionally, a monolithic column was included in the fingerprint study as a potential alternative to the conventional packed columns. The effects of experimental parameters, such as the composition of the mobile phase, the concentration and pH of the buffer, and the applied voltage, were studied. Binary mobile phases consisting of acetonitrile and a 5 mM sodium dihydrogen phosphate electrolyte at pH 2.8 were used in gradient elution mode with an applied voltage of 5 kV. Under optimal gradient conditions, at least 45 peaks were observed within 60 min on the commercial packed column, whereas only about 20 peaks were separated on the methacrylate-based monolithic and the in-house packed columns. The commercial column thus clearly outperforms the two other. However, the properties of the monolithic stationary phase still might be adapted (i.e., by changing the polymerization-mixture composition, the porosity, and thus the selectivity of the phase might be changed), which could lead to an improved efficiency.

  4. Development of fluorous porous polymer monolith (FPPM) for the capillary electrochromatographic separation of fluorous analytes based on fluorous-fluorous interaction.

    Science.gov (United States)

    Xu, Zhenpo; Gibson, Graham T T; Oleschuk, Richard D

    2013-01-21

    This is the first report on the CEC separation of fluorous analytes on a fluorous porous polymer monolith (FPPM) stationary phase based on fluorous-fluorous interaction. Monolithic columns do not require retaining frits and can be conveniently photo-patterned within a capillary. Two groups of fluorous compounds, a N-f-Cbz-4-nitro-benzylamine (N) series and a N-f-Cbz-4-phenyl-benzylamine (P) series, each series having compounds differing only by the length of their perfluorinated tag, were employed to evaluate the ability of the fluorinated column to separate fluorous analytes using a variety of mobile phase compositions and separation conditions. Fluorous monoliths showed enhanced separation performance by providing better selectivity, higher resolution and shorter analysis time compared to a similar non-fluorous (reversed phase) monolithic column. Under optimal conditions, column efficiency as high as 234,000 plates per metre was achieved, and all four compounds of the N series were fully resolved in columns. It was found that the non-FPPM column resolves fluorous analytes mainly based on reversed phase interaction while the FPPM column resolves them mainly based on fluorous-fluorous interaction. Results are compared to fluorous monolith columns used in a nano-liquid-chromatographic (nano-LC) separation with gradient elution. The FPPM column required less than one fifth the analysis time in CEC mode than was required in nanoLC mode, with superior separation efficiency and resolution. FPPM stationary phases provide an attractive option for the analysis of perfluorinated analytes, which is expected to be useful in areas such as proteomics for the separation of fluorously tagged proteins, and in environmental analysis where fluorinated species are of increasing concern.

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

    Science.gov (United States)

    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.

  6. Preparation of monolithic affinity media for nano-liquid chromatography applications.

    Science.gov (United States)

    Sproß, Jens; Sinz, Andrea

    2014-01-01

    In this protocol, a strategy is described for preparing affinity media with monolithic materials as stationary phase, which is exemplified for the biotin-avidin interaction pair. The capillary columns prepared in this manner are compatible with nano-liquid chromatographic conditions. Our protocol is easily adapted to the preparation of specific affinity media with different functionalities and as such provides a platform for a multitude of applications.

  7. A monolithic silicon detector telescope

    International Nuclear Information System (INIS)

    Cardella, G.; Amorini, F.; Cabibbo, M.; Di Pietro, A.; Fallica, G.; Franzo, G.; Figuera, P.; Papa, M.; Pappalardo, G.; Percolla, G.; Priolo, F.; Privitera, V.; Rizzo, F.; Tudisco, S.

    1996-01-01

    An ultrathin silicon detector (1 μm) thick implanted on a standard 400 μm Si-detector has been built to realize a monolithic telescope detector for simultaneous charge and energy determination of charged particles. The performances of the telescope have been tested using standard alpha sources and fragments emitted in nuclear reactions with different projectile-target colliding systems. An excellent charge resolution has been obtained for low energy (less than 5 MeV) light nuclei. A multi-array lay-out of such detectors is under construction to charge identify the particles emitted in reactions induced by low energy radioactive beams. (orig.)

  8. Imaging monolithic silicon detector telescopes

    International Nuclear Information System (INIS)

    Amorini, F.; Sipala, V.; Cardella, G.; Boiano, C.; Carbone, B.; Cosentino, L.; Costa, E.; Di Pietro, A.; Emanuele, U.; Fallica, G.; Figuera, P.; Finocchiaro, P.; La Guidara, E.; Marchetta, C.; Pappalardo, A.; Piazza, A.; Randazzo, N.; Rizzo, F.; Russo, G.V.; Russotto, P.

    2008-01-01

    We show the results of some test beams performed on a new monolithic strip silicon detector telescope developed in collaboration with the INFN and ST-microelectronics. Using an appropriate design, the induction on the ΔE stages, generated by the charge released in the E stage, was used to obtain the position of the detected particle. The position measurement, together with the low threshold for particle charge identification, allows the new detector to be used for a large variety of applications due to its sensitivity of only a few microns measured in both directions

  9. Accelerating the quality control of pharmaceuticals using monolithic stationary phases: a review of recent HPLC applications.

    Science.gov (United States)

    Zacharis, Constantinos K

    2009-07-01

    High-performance liquid chromatography (HPLC) is the predominant technique in the quality control of pharmaceutical formulations. HPLC offers highly sensitive and selective analytical methods with increased robustness and separation efficiency. The majority of HPLC-based methodologies are based on the usage of particulate-based columns and cannot be applied at elevated flow rates (> 2 mL/min) due to excessive back-pressure. Therefore, the typical duration of separation cycles is in the range of 5-30 min, making most assays time-consuming, especially when a lot of samples have to be analyzed in a minimum amount of time. Monolithic stationary phases for HPLC offer a very interesting alternative to conventional particulate-based columns. The size of the skeleton and the distribution of the pores of monolithic materials offer the possibility of developing efficient separation protocols at higher flow-rates due to the low pressure-drop across the column. The present review intends to cover the applications of monolithic based HPLC stationary phases in the quality control of pharmaceutical formulations, including identification of active pharmaceutical ingredient, assay, purity, dissolution, blending, and dosage uniformity, etc.

  10. Monolithic media for applications in affinity chromatography.

    Science.gov (United States)

    Sproß, Jens; Sinz, Andrea

    2011-08-01

    Affinity chromatography presents a highly versatile analytical tool, which relies on exploiting highly specific interactions between molecules and their ligands. This review covers the most recent literature on the application of monoliths as stationary phases for various affinity-based chromatographic applications. Different affinity approaches as well as separations using molecularly imprinted monoliths are discussed. Hybrid stationary phases created by embedding of particles or nanoparticles into a monolithic stationary phase are also considered in this review article. The ease of preparation of monoliths and the multitude of functionalization techniques, which have matured during the past years, make monoliths interesting for an increasing number of biochemical and medical applications. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Nanoparticle-Directed Metal-Organic Framework/Porous Organic Polymer Monolithic Supports for Flow-Based Applications.

    Science.gov (United States)

    Darder, María Del Mar; Salehinia, Shima; Parra, José B; Herrero-Martinez, José M; Svec, Frantisek; Cerdà, Víctor; Turnes Palomino, Gemma; Maya, Fernando

    2017-01-18

    A two-step nanoparticle-directed route for the preparation of macroporous polymer monoliths for which the pore surface is covered with a metal-organic framework (MOF) coating has been developed to facilitate the use of MOFs in flow-based applications. The flow-through monolithic matrix was prepared in a column format from a polymerization mixture containing ZnO-nanoparticles. These nanoparticles embedded in the precursor monolith were converted to MOF coatings via the dissolution-precipitation equilibrium after filling the pores of the monolith with a solution of the organic linker. Pore surface coverage with the microporous zeolitic imidazolate framework ZIF-8 resulted in an increase in surface area from 72 to 273 m 2 g -1 . Monolithic polymer containing ZIF-8 coating was implemented as a microreactor catalyzing the Knoevenagel condensation reaction and also in extraction column format enabling the preconcentration of trace levels of toxic chlorophenols in environmental waters. Our approach can be readily adapted to other polymers and MOFs thus enabling development of systems for flow-based MOF applications.

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

    Science.gov (United States)

    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.

  13. Profiling of drug binding proteins by monolithic affinity chromatography in combination with liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Zhang, Xuepei; Wang, Tongdan; Zhang, Hanzhi; Han, Bing; Wang, Lishun; Kang, Jingwu

    2014-09-12

    A new approach for proteome-wide profiling drug binding proteins by using monolithic capillary affinity chromatography in combination with HPLC-MS/MS is reported. Two immunosuppresive drugs, namely FK506 and cyclosporin A, were utilized as the experimental models for proof-of-concept. The monolithic capillary affinity columns were prepared through a single-step copolymerization of the drug derivatives with glycidyl methacrylate and ethylene dimethacrylate. The capillary chromatography with the affinity monolithic column facilitates the purification of the drug binding proteins from the cell lysate. By combining the capillary affinity column purification and the shot-gun proteomic analysis, totally 33 FK506- and 32 CsA-binding proteins including all the literature reported target proteins of these two drugs were identified. Among them, two proteins, namely voltage-dependent anion-selective channel protein 1 and serine/threonine-protein phosphatase PGAM5 were verified by using the recombinant proteins. The result supports that the monolithic capillary affinity chromatography is likely to become a valuable tool for profiling of binding proteins of small molecular drugs as well as bioactive compounds. Copyright © 2014 Elsevier B.V. All rights reserved.

  14. Design model and recommendations of column-foundation connection through socket with rough interfaces

    Directory of Open Access Journals (Sweden)

    R. M. F. Canha

    Full Text Available The present work proposes design models and recommendations for column-foundation connection through socket with rough interfaces, including the shear key configuration, the socket and the precast column base. In the experimental investigations, the behavior of socket and column as a monolithic connection was verified. However, for this to occur, the shear key dimensions must be between the limits suggested by the study. Considering the total transfer of internal forces in the connections, the vertical reinforcement should be designed based on the bending theory. The proposed model for the design of the transverse horizontal reinforcement, considering monolithic behavior of the connection, was found to be in good agreement with the observed experimental results. With adjustments to this model for the socket, a new model for the design of precast column bases is proposed and compared with other model adapted for rough interfaces.

  15. Optimization of lytic phage manufacturing in bioreactor using monolithic supports.

    Science.gov (United States)

    Smrekar, Franc; Ciringer, Mateja; Jančar, Janez; Raspor, Peter; Štrancar, Aleš; Podgornik, Aleš

    2011-08-01

    A process for manufacturing large quantities of lytic bacteriophages was developed. Determination of cultivation termination was found to be essential to achieve high phage quantity and purity. When optimal cultivation termination is missed, phage fraction was found to be highly contaminated with deoxyribonucleic acid released from Escherichia coli cells. Besides, an already established method for monitoring of phage cultivation based on optical density, where its peak indicates point when maximal phage titer is achieved, a new indirect chromatographic method using methacrylate monoliths is proposed for on-line estimation of phage titer. It is based on the measurement of released E. coli deoxyribonucleic acid and shows high correlation with phage titer obtained from plaque assay. Its main advantage is that the information is obtained within few minutes. In addition, the same method can also be used to determine purity of a final phage fraction. Two strategies to obtain highly pure phage fractions are proposed: an immediate purification of phage lysate using monolithic columns or an addition of EDTA before chromatographic purification. The developed protocol was shown to give phage purity above 90% and it is completed within one working day including cultivation and phage titer in the final formulation using developed chromatographic method. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

    Science.gov (United States)

    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.

  17. Monolithic cells for solar fuels.

    Science.gov (United States)

    Rongé, Jan; Bosserez, Tom; Martel, David; Nervi, Carlo; Boarino, Luca; Taulelle, Francis; Decher, Gero; Bordiga, Silvia; Martens, Johan A

    2014-12-07

    Hybrid energy generation models based on a variety of alternative energy supply technologies are considered the best way to cope with the depletion of fossil energy resources and to limit global warming. One of the currently missing technologies is the mimic of natural photosynthesis to convert carbon dioxide and water into chemical fuel using sunlight. This idea has been around for decades, but artificial photosynthesis of organic molecules is still far away from providing real-world solutions. The scientific challenge is to perform in an efficient way the multi-electron transfer reactions of water oxidation and carbon dioxide reduction using holes and single electrons generated in an illuminated semiconductor. In this tutorial review the design of photoelectrochemical (PEC) cells that combine solar water oxidation and CO2 reduction is discussed. In such PEC cells simultaneous transport and efficient use of light, electrons, protons and molecules has to be managed. It is explained how efficiency can be gained by compartmentalisation of the water oxidation and CO2 reduction processes by proton exchange membranes, and monolithic concepts of artificial leaves and solar membranes are presented. Besides transferring protons from the anode to the cathode compartment the membrane serves as a molecular barrier material to prevent cross-over of oxygen and fuel molecules. Innovative nano-organized multimaterials will be needed to realise practical artificial photosynthesis devices. This review provides an overview of synthesis techniques which could be used to realise monolithic multifunctional membrane-electrode assemblies, such as Layer-by-Layer (LbL) deposition, Atomic Layer Deposition (ALD), and porous silicon (porSi) engineering. Advances in modelling approaches, electrochemical techniques and in situ spectroscopies to characterise overall PEC cell performance are discussed.

  18. Development of a silica monolith microbioreactor entrapping highly activated lipase and an experiment toward integration with chromatographic separation of chiral esters.

    Science.gov (United States)

    Kawakami, Koei; Abe, Daisuke; Urakawa, Taiki; Kawashima, Ayako; Oda, Yasuhiro; Takahashi, Ryo; Sakai, Shinji

    2007-11-01

    Microbioreactors are effective for high-throughput production of expensive products from small amounts of substrates. Lipases are versatile enzymes for chiral syntheses, and are highly activated when immobilized in alkyl-substituted silicates by the sol-gel method. For practical application of sol-gel immobilized lipases to a flow system, a microbioreactor loaded with a macroporous silica monolith is well suited, because it can be easily integrated with a chromatographic separator for optical resolution. We attempted to develop a microbioreactor containing a silica monolith-immobilized lipase. A nonshrinkable silica monolith was first formed from a 4:1 mixture of methyltrimethoxysilane (MTMS) and tetramethoxysilane (TMOS). It was then coated with silica precipitates entrapping lipase, derived from a 4:1 mixture of n-butyltrimethoxysilane (BTMS) and TMOS. As a result, monolith treated with the BTMS-based silicate entrapping lipase exhibited approximately ten times higher activity than nontreated monolith-immobilized lipase derived from the MTMS-based silicate, in transesterification between glycidol and vinyl n-butyrate in isooctane. A commercially available chiral column was connected in series to the monolith microbioreactor, and a pulse of substrate solution was supplied at the inlet of the reactor. Successful resolution of the racemic ester produced was achieved in the chromatographic column.

  19. Preparation of a monolitich capillary column with immobilized a-mannose for affinity chromatography of lectins

    NARCIS (Netherlands)

    Tetala, K.K.R.; Chen, B.; Visser, G.M.; Maruska, A.; Kornysova, O.; Beek, van T.A.; Sudhölter, E.J.R.

    2007-01-01

    A simple method for the preparation of an affinity monolithic (also called continuous bed) capillary column for ¿-mannose-specific lectins is described. 2-Hydroxyethyl methacrylate in combination with (+)-N,N´-diallyltartardiamide (DATD) and piperazine diacrylamide (PDA, 1,4-bisacryloyl-piperazine)

  20. Modeling Stone Columns.

    Science.gov (United States)

    Castro, Jorge

    2017-07-11

    This paper reviews the main modeling techniques for stone columns, both ordinary stone columns and geosynthetic-encased stone columns. The paper tries to encompass the more recent advances and recommendations in the topic. Regarding the geometrical model, the main options are the "unit cell", longitudinal gravel trenches in plane strain conditions, cylindrical rings of gravel in axial symmetry conditions, equivalent homogeneous soil with improved properties and three-dimensional models, either a full three-dimensional model or just a three-dimensional row or slice of columns. Some guidelines for obtaining these simplified geometrical models are provided and the particular case of groups of columns under footings is also analyzed. For the latter case, there is a column critical length that is around twice the footing width for non-encased columns in a homogeneous soft soil. In the literature, the column critical length is sometimes given as a function of the column length, which leads to some disparities in its value. Here it is shown that the column critical length mainly depends on the footing dimensions. Some other features related with column modeling are also briefly presented, such as the influence of column installation. Finally, some guidance and recommendations are provided on parameter selection for the study of stone columns.

  1. MONOLITHIC DISK FOR THE FAST CHROMATOGRAPHIC SEPARATION

    Directory of Open Access Journals (Sweden)

    Nurul Hidayat Aprilita

    2010-06-01

    Full Text Available Poly(styrene/divinylbenzene (PS/DVB monolithic disk was prepared by in situ free-radical copolymerization of styrene and divinylbenzene in the presence of decanol and tetrahydrofuran as porogens. PS/DVB monolithic disks were produced in two different lengths 1.5 mm and 3 mm. The disks were used in reversed phase chromatography of proteins with 0.2 % trifuoroacetic acid (TFA and 0.2 % TFA in acetonitrile as mobile phase A and B, respectively. The effect of gradient rate, flow rate, temperature and disk length on the separation of proteins were also studied. PS/DVB monolithic disks allow the rapid separation of proteins in reversed phase chromatography. Keywords: monolithic disk, poly(styrene/divinylbenzene, proteins

  2. Monolithic Time Delay Integrated APD Arrays Project

    Data.gov (United States)

    National Aeronautics and Space Administration — The overall goal of the proposed program by Epitaxial Technologies is to develop monolithic time delay integrated avalanche photodiode (APD) arrays with sensitivity...

  3. Hypercrosslinked large surface area porous polymer monoliths for hydrophilic interaction liquid chromatography of small molecules featuring zwitterionic functionalities attached to gold nanoparticles held in layered structure.

    Science.gov (United States)

    Lv, Yongqin; Lin, Zhixing; Svec, Frantisek

    2012-10-16

    A novel approach to porous polymer monoliths hypercrosslinked to obtain large surface areas and modified with zwitterionic functionalities through the attachment of gold nanoparticles in a layered architecture has been developed. The capillary columns were used for the separation of small molecules in hydrophilic interaction liquid chromatography mode. First, a monolith with a very large surface area of 430 m(2)/g was prepared by hypercrosslinking from a generic poly(4-methylstyrene-co-vinylbenzyl chloride-co-divinylbenzene) monolith via a Friedel-Crafts reaction catalyzed with iron chloride. Free radical bromination then provided this hypercrosslinked monolith with 5.7 at % Br that further reacted with cystamine under microwave irradiation, resulting in a product containing 3.8 at % sulfur. Clipping the disulfide bonds with tris(2-carboxylethyl) phosphine liberated the desired thiol groups that bind the first layer of gold nanoparticles. These immobilized nanoparticles were an intermediate ligand enabling the attachment of polyethyleneimine as a spacer followed by immobilization of the second layer of gold nanoparticles which were eventually functionalized with zwitterionic cysteine. This layered architecture, prepared using 10 nm nanoparticles, contains 17.2 wt % Au, more than twice than that found in the first layer alone. Chromatographic performance of these hydrophilic monolithic columns was demonstrated with the separation of mixtures of nucleosides and peptides in hydrophilic interaction chromatography (HILIC) mode. A column efficiency of 51,000 plates/m was achieved for retained analyte cytosine.

  4. Wideband Monolithic Tile for Reconfigurable Phased Arrays

    Science.gov (United States)

    2017-03-01

    Wideband Monolithic Tile for Reconfigurable Phased Arrays James J. Komiak1, Ryan S. Westafer2, Nancy V. Saldanha2, Randall Lapierre1, R. Todd...Lee2 BAE Systems Electronic Systems1, Georgia Tech Research Institute2 Abstract: A Wideband Monolithic 6 x 6 Tile of interconnected Quad Switches...circuits. The Tile incorporates 36 such Quad Switches, having 288 PHEMT devices controlled by 144 control lines and 300 bias resistors. To the

  5. Decomposition of monolithic web application to microservices

    OpenAIRE

    Zaymus, Mikulas

    2017-01-01

    Solteq Oyj has an internal Wellbeing project for massage reservations. The task of this thesis was to transform the monolithic architecture of this application to microservices. The thesis starts with a detailed comparison between microservices and monolithic application. It points out the benefits and disadvantages microservice architecture can bring to the project. Next, it describes the theory and possible strategies that can be used in the process of decomposition of an existing monoli...

  6. Monolithic ceramic capacitors for high reliability applications

    Science.gov (United States)

    Thornley, E. B.

    1981-01-01

    Monolithic multi-layer ceramic dielectric capacitors are widely used in high reliability applications in spacecraft, launch vehicles, and military equipment. Their relatively low cost, wide range of values, and package styles are attractive features that result in high usage in electronic circuitry in these applications. Design and construction of monolithic ceramic dielectric capacitors, defects that can lead to failure, and methods for defect detection that are being incorporated in military specifications are discussed.

  7. Monolithic multinozzle emitters for nanoelectrospray mass spectrometry

    Science.gov (United States)

    Wang, Daojing [Daly City, CA; Yang, Peidong [Kensington, CA; Kim, Woong [Seoul, KR; Fan, Rong [Pasadena, CA

    2011-09-20

    Novel and significantly simplified procedures for fabrication of fully integrated nanoelectrospray emitters have been described. For nanofabricated monolithic multinozzle emitters (NM.sup.2 emitters), a bottom up approach using silicon nanowires on a silicon sliver is used. For microfabricated monolithic multinozzle emitters (M.sup.3 emitters), a top down approach using MEMS techniques on silicon wafers is used. The emitters have performance comparable to that of commercially-available silica capillary emitters for nanoelectrospray mass spectrometry.

  8. A monolithically integrated magneto-optoelectronic circuit

    Science.gov (United States)

    Saha, D.; Basu, D.; Bhattacharya, P.

    2008-11-01

    The monolithic integration of a spin valve, an amplifier, and a light emitting diode to form a magneto-optoelectronic integrated circuit on GaAs is demonstrated. The circuit converts the spin polarization information in the channel of the spin valve to an amplified change in light intensity with a gain of 20. The monolithic circuit therefore operates as a magnetoelectronic switch which modulates the light intensity of the light emitting diode.

  9. Ionic liquids as porogens in the microwave-assisted synthesis of methacrylate monoliths for chromatographic application

    Energy Technology Data Exchange (ETDEWEB)

    Singco, Brenda; Lin, Chen-Lan; Cheng, Yi-Jie; Shih, Yung-Han [Department of Chemistry and Center for Nanotechnology, CYCU (Chung Yuan Christian University), 200 Chung Pei Road, Chung-Li 320, Taiwan (China); Huang, Hsi-Ya, E-mail: hyhuang@cycu.edu.tw [Department of Chemistry and Center for Nanotechnology, CYCU (Chung Yuan Christian University), 200 Chung Pei Road, Chung-Li 320, Taiwan (China)

    2012-10-09

    Highlights: Black-Right-Pointing-Pointer An efficient and cleaner monoliths preparation utilizing ionic liquids in conjunction with microwave Black-Right-Pointing-Pointer These ionic liquids with varied cation alkyl chain and anion type successfully tuned the morphology of different alkyl methacrylates Black-Right-Pointing-Pointer Small molecules and peptide digests separated well in these monoliths. - Abstract: Several imidazolium-based ionic liquids (ILs) with varying cation alkyl chain length (C{sub 4}-C{sub 10}) and anion type (tetrafluoroborate ([BF{sub 4}]{sup -}), hexafluorophosphate ([PF{sub 6}]{sup -}) and bis(trifluoromethylsulfonyl)imide ([Tf{sub 2}N]{sup -})) were used as reaction media in the microwave polymerization of methacrylate-based stationary phases. Scanning electron micrographs and backpressures of poly(butyl methacrylate-ethylene dimethacrylate) (poly(BMA-EDMA)) monoliths synthesized in the presence of these ionic liquids demonstrated that porosity and permeability decreased when cation alkyl chain length and anion hydrophobicity were increased. Performance of these monoliths was assessed for their ability to separate parabens by capillary electrochromatography (CEC). Intra-batch precision (n = 3 columns) for retention time and peak area ranged was 0.80-1.13% and 3.71-4.58%, respectively. In addition, a good repeatability of RSD{sub Retentiontime} = <0.30% and {approx}1.0%, RSD{sub Peakarea} = <1.30% and <4.3%, and RSD{sub Efficiency} = <0.6% and <11.5% for intra-day and inter-day, respectively exemplify monolith performance reliability for poly(BMA-EDMA) fabricated using 1-hexyl-3-methylimidazolium tetrafluoroborate ([C{sub 6}mim][BF{sub 4}]) porogen. This monolith was also tested for its potential in nanoLC to separate protein digests in gradient mode. ILs as porogens also fabricated different alkyl methacrylate (AMA) (C4-C18) monoliths. Furthermore, employing binary IL porogen mixture such as 1-butyl-3-methylimidazolium tetrafluoroborate

  10. Methacrylate Polymer Monoliths for Separation Applications

    Directory of Open Access Journals (Sweden)

    Robert J. Groarke

    2016-06-01

    Full Text Available This review summarizes the development of methacrylate-based polymer monoliths for separation science applications. An introduction to monoliths is presented, followed by the preparation methods and characteristics specific to methacrylate monoliths. Both traditional chemical based syntheses and emerging additive manufacturing methods are presented along with an analysis of the different types of functional groups, which have been utilized with methacrylate monoliths. The role of methacrylate based porous materials in separation science in industrially important chemical and biological separations are discussed, with particular attention given to the most recent developments and challenges associated with these materials. While these monoliths have been shown to be useful for a wide variety of applications, there is still scope for exerting better control over the porous architectures and chemistries obtained from the different fabrication routes. Conclusions regarding this previous work are drawn and an outlook towards future challenges and potential developments in this vibrant research area are presented. Discussed in particular are the potential of additive manufacturing for the preparation of monolithic structures with pre-defined multi-scale porous morphologies and for the optimization of surface reactive chemistries.

  11. Methacrylate Polymer Monoliths for Separation Applications

    Science.gov (United States)

    Groarke, Robert J.; Brabazon, Dermot

    2016-01-01

    This review summarizes the development of methacrylate-based polymer monoliths for separation science applications. An introduction to monoliths is presented, followed by the preparation methods and characteristics specific to methacrylate monoliths. Both traditional chemical based syntheses and emerging additive manufacturing methods are presented along with an analysis of the different types of functional groups, which have been utilized with methacrylate monoliths. The role of methacrylate based porous materials in separation science in industrially important chemical and biological separations are discussed, with particular attention given to the most recent developments and challenges associated with these materials. While these monoliths have been shown to be useful for a wide variety of applications, there is still scope for exerting better control over the porous architectures and chemistries obtained from the different fabrication routes. Conclusions regarding this previous work are drawn and an outlook towards future challenges and potential developments in this vibrant research area are presented. Discussed in particular are the potential of additive manufacturing for the preparation of monolithic structures with pre-defined multi-scale porous morphologies and for the optimization of surface reactive chemistries. PMID:28773570

  12. Grafting zwitterionic polymer onto cryogel surface enhances protein retention in steric exclusion chromatography on cryogel monolith.

    Science.gov (United States)

    Tao, Shi-Peng; Zheng, Jie; Sun, Yan

    2015-04-10

    Cryogel monoliths with interconnected macropores (10-100μm) and hydrophilic surfaces can be employed as chromatography media for protein retention in steric exclusion chromatography (SXC). SXC is based on the principle that the exclusion of polyethylene glycol (PEG) on both a hydrophilic chromatography surface and a protein favors their association, leading to the protein retention on the chromatography surface. Elution of the retained protein can be achieved by reducing PEG concentration. In this work, the surface of polyacrylamide-based cryogel monolith was modified by grafting zwitterionic poly(carboxybetaine methacrylate) (pCBMA), leading the increase in the surface hydrophilicity. Observation by scanning electron microscopy revealed the presence of the grafted pCBMA chain clusters on the cryogel surface, but pCBMA grafting did not result in the changes of the physical properties of the monolith column, and the columns maintained good recyclability in SXC. The effect of the surface grafting on the SXC behavior of γ-globulin was investigated in a wide flow rate range (0.6-12cm/min). It was found that the dynamic retention capacity increased 1.4-1.8 times by the zwitterionic polymer grafting in the flow rate range of 1.5-12cm/min. The mechanism of enhanced protein retention on the zwitterionic polymer-grafted surface was proposed. The research proved that zwitterionic polymer modification was promising for the development of new materials for SXC applications. Copyright © 2015 Elsevier B.V. All rights reserved.

  13. ( Anogeissus leiocarpus ) timber columns

    African Journals Online (AJOL)

    A procedure for designing axially loaded Ayin (Anogeissus leiocarpus) wood column or strut has been investigated. Instead of the usual categorization of columns into short, intermediate and slender according to the value of slenderness ratio, a continuous column formula representing the three categories was derived.

  14. RpeakChrom: Novel R package for the automated characterization and optimization of column efficiency in high-performance liquid chromatography analysis.

    Science.gov (United States)

    Peris-Díaz, Manuel David; Alcoriza-Balaguer, Maria Isabel; García-Cañaveras, Juan Carlos; Santonja, Francisco; Sentandreu, Enrique; Lahoz, Agustín

    2017-11-01

    Characterization of chromatographic columns using the traditional van Deemter method is limited by the necessity of calculating extra-column variance, issue particularly relevant when modeling asymmetrical peaks eluted from monolithic columns. A novel R package that implements Parabolic Variance Modified Gaussian approach for accurate peak modeling, van Deemter equation and two alternatives approaches, based on van Deemter, has been developed to calculate the height equivalent to a theoretical plate (HETP). To assess package capabilities conventional packed reverse-phase and monolithic HPLC columns were characterized. Peaks eluted from the monolithic column showed a high value of factor asymmetry due, in part, to the contribution of extra-column factors. Such deviation can be circumvented by the two alternatives approaches implemented in the R-package. Furthermore, increased values of eddy diffusion and mass transfer kinetics terms in HETP were observed for the packed column, while accuracy was below 9% in all cases. These results showed the usefulness of the R-package for both modeling chromatographic peaks and assessing column efficiency. The RpeakChrom package could become a helpful tool for testing new stationary phases during column development and to evaluate column during its lifetime. This R tool is freely available from CRAN (https://CRAN.R-project.org/package=RpeakChrom). © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Taking a Large Monolith to Use for Teaching Soil Morphology.

    Science.gov (United States)

    Smith, B. R.; And Others

    1989-01-01

    Described is a technique for taking a large monolith for the purpose of teaching soil structure. Materials and procedures are detailed. A survey of 93 students indicated that the larger monolith was preferred over the commonly used narrow ones. (CW)

  16. Fracture resistance of monolithic zirconia molar crowns with reduced thickness

    OpenAIRE

    Nakamura, Keisuke; Harada, A.; Inagaki, R.; Kanno, Taro; Niwano, Y.; Milleding, Percy; Ørtengren, Ulf Thore

    2015-01-01

    This is the accepted manuscript version. Published version is available at Acta Odontologica Scandinavica Objectives. The purpose of the present study was to analyze the relationship between fracture load of monolithic zirconia crowns and axial/occlusal thickness, and to evaluate the fracture resistance of monolithic zirconia crowns with reduced thickness in comparison with that of monolithic lithium disilicate crowns with regular thickness. Materials and methods. Monolithic zi...

  17. Eigenpolarization theory of monolithic nonplanar ring oscillators

    Science.gov (United States)

    Nilsson, Alan C.; Gustafson, Eric K.; Byer, Robert L.

    1989-01-01

    Diode-laser-pumped monolithic nonplanar ring oscillators (NPROs) in an applied magnetic field can operate as unidirectional traveling-wave lasers. The diode laser pumping, monolithic construction, and unidirectional oscillation lead to narrow linewidth radiation. Here, a comprehensive theory of the eigenpolarizations of a monolithic NPRO is presented. It is shown how the properties of the integral optical diode that forces unidirectional operation depend on the choice of the gain medium, the applied magnetic field, the output coupler, and the geometry of the nonplanar ring light path. Using optical equivalence theorems to gain insight into the polarization characteristics of the NPRO, a strategy for designing NPROs with low thresholds and large loss nonreciprocities is given. An analysis of the eigenpolarizations for one such NPRO is presented, alternative optimization approaches are considered, and the prospects for further reducing the linewidths of these lasers are briefly discussed.

  18. Small Column Ion Exchange

    International Nuclear Information System (INIS)

    Huff, Thomas

    2010-01-01

    Small Column Ion Exchange (SCIX) leverages a suite of technologies developed by DOE across the complex to achieve lifecycle savings. Technologies are applicable to multiple sites. Early testing supported multiple sites. Balance of SRS SCIX testing supports SRS deployment. A forma Systems Engineering Evaluation (SEE) was performed and selected Small Column Ion Exchange columns containing Crystalline Silicotitanate (CST) in a 2-column lead/lag configuration. SEE considered use of Spherical Resorcinol-Formaldehyde (sRF). Advantages of approach at SRS include: (1) no new buildings, (2) low volume of Cs waste in solid form compared to aqueous strip effluent; and availability of downstream processing facilities for immediate processing of spent resin.

  19. Highly improved operation of monolithic BGO-PET blocks

    Science.gov (United States)

    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

  20. The influence of connecting pile cap-column in the mechanisms of break in the two pile caps

    Directory of Open Access Journals (Sweden)

    A. C. MESQUITA

    Full Text Available Abstract The paper analyzes the two pile caps with partially embedded socket and subject a center load. Three models were experimentally tested, varying the type of conformation of the column and walls of the socket, with a smooth, the other rough, and a monolithic two pile cap, used for reference. The roughening of the column-socket interface was examined with the aim of verifying the difference of the distribution of compressive and tensile stresses in the strut an tie model used for design. The experimental test to show that the two pile caps with conformation rough of the column and walls of the socket, support more load in comparison with two pile caps with smooth of the column and walls of the socket. Both however underperformed the monolithic two pile cap, with values of 66% and 36% respectively.

  1. UPDATE ON MONOLITHIC FUEL FABRICATION METHODS

    Energy Technology Data Exchange (ETDEWEB)

    C. R. Clark; J. F. Jue; G. A. Moore; N. P. Hallinan; B. H. Park; D. E. Burkes

    2006-10-01

    Efforts to develop a viable monolithic research reactor fuel plate have continued at Idaho National Laboratory. These efforts have concentrated on both fabrication process refinement and scale-up to produce full sized fuel plates. Progress at INL has led to fabrication of hot isostatic pressed uranium-molybdenum bearing monolithic fuel plates. These miniplates are part of the RERTR-8 miniplate irradiation test. Further progress has also been made on friction stir weld processing which has been used to fabricate full size fuel plates which will be irradiated in the ATR and OSIRIS reactors.

  2. Macroporous Monolithic Polymers: Preparation and Applications

    Science.gov (United States)

    Arrua, Ruben Dario; Strumia, Miriam Cristina; Alvarez Igarzabal, Cecilia Inés

    2009-01-01

    In the last years, macroporous monolithic materials have been introduced as a new and useful generation of polymers used in different fields. These polymers may be prepared in a simple way from a homogenous mixture into a mold and contain large interconnected pores or channels allowing for high flow rates at moderate pressures. Due to their porous characteristics, they could be used in different processes, such as stationary phases for different types of chromatography, high-throughput bioreactors and in microfluidic chip applications. This review reports the contributions of several groups working in the preparation of different macroporous monoliths and their modification by immobilization of specific ligands on the products for specific purposes.

  3. Technology development for SOI monolithic pixel detectors

    International Nuclear Information System (INIS)

    Marczewski, J.; Domanski, K.; Grabiec, P.; Grodner, M.; Jaroszewicz, B.; Kociubinski, A.; Kucharski, K.; Tomaszewski, D.; Caccia, M.; Kucewicz, W.; Niemiec, H.

    2006-01-01

    A monolithic detector of ionizing radiation has been manufactured using silicon on insulator (SOI) wafers with a high-resistivity substrate. In our paper the integration of a standard 3 μm CMOS technology, originally designed for bulk devices, with fabrication of pixels in the bottom wafer of a SOI substrate is described. Both technological sequences have been merged minimizing thermal budget and providing suitable properties of all the technological layers. The achieved performance proves that fully depleted monolithic active pixel matrix might be a viable option for a wide spectrum of future applications

  4. Increased thermal conductivity monolithic zeolite structures

    Science.gov (United States)

    Klett, James; Klett, Lynn; Kaufman, Jonathan

    2008-11-25

    A monolith comprises a zeolite, a thermally conductive carbon, and a binder. The zeolite is included in the form of beads, pellets, powders and mixtures thereof. The thermally conductive carbon can be carbon nano-fibers, diamond or graphite which provide thermal conductivities in excess of about 100 W/mK to more than 1,000 W/mK. A method of preparing a zeolite monolith includes the steps of mixing a zeolite dispersion in an aqueous colloidal silica binder with a dispersion of carbon nano-fibers in water followed by dehydration and curing of the binder is given.

  5. Monolithic JFET preamplifier for ionization chamber calorimeter

    International Nuclear Information System (INIS)

    Radeka, V.; Rescia, S.; Manfredi, P.F.; Speziali, V.

    1990-10-01

    A monolithic charge sensitive preamplifier using exclusively n-channel diffused JFETs has been designed and is now being fabricated by INTERFET Corp. by means of a dielectrically isolated process which allows preserving as much as possible the technology upon which discrete JFETs are based. A first prototype built by means of junction isolated process has been delivered. The characteristics of monolithically integrated JFETs compare favorably with discrete devices. First results of tests of a preamplifier which uses these devices are reported. 4 refs

  6. Immobilized enzyme reactor chromatography: Optimization of protein retention and enzyme activity in monolithic silica stationary phases

    International Nuclear Information System (INIS)

    Besanger, Travis R.; Hodgson, Richard J.; Green, James R.A.; Brennan, John D.

    2006-01-01

    Our group recently reported on the application of protein-doped monolithic silica columns for immobilized enzyme reactor chromatography, which allowed screening of enzyme inhibitors present in mixtures using mass spectrometry for detection. The enzyme was immobilized by entrapment within a bimodal meso/macroporous silica material prepared by a biocompatible sol-gel processing route. While such columns proved to be useful for applications such as screening of protein-ligand interactions, significant amounts of entrapped proteins leached from the columns owing to the high proportion of macropores within the materials. Herein, we describe a detailed study of factors affecting the morphology of protein-doped bioaffinity columns and demonstrate that specific pH values and concentrations of poly(ethylene glycol) can be used to prepare essentially mesoporous columns that retain over 80% of initially loaded enzyme in an active and accessible form and yet still retain sufficient porosity to allow pressure-driven flow in the low μL/min range. Using the enzyme γ-glutamyl transpeptidase (γ-GT), we further evaluated the catalytic constants of the enzyme entrapped in capillary columns with different silica morphologies as a function of flowrate and backpressure using the enzyme reactor assay mode. It was found that the apparent activity of the enzyme was highest in mesoporous columns that retained high levels of enzyme. In such columns, enzyme activity increased by ∼2-fold with increases in both flowrate (from 250 to 1000 nL/min) and backpressure generated (from 500 to 2100 psi) during the chromatographic activity assay owing to increases in k cat and decreases in K M , switching from diffusion controlled to reaction controlled conditions at ca. 2000 psi. These results suggest that columns with minimal macropore volumes (<5%) are advantageous for the entrapment of soluble proteins for bioaffinity and bioreactor chromatography

  7. Enhancing mass transfer and ethanol production in syngas fermentation of Clostridium carboxidivorans P7 through a monolithic biofilm reactor

    International Nuclear Information System (INIS)

    Shen, Yanwen; Brown, Robert; Wen, Zhiyou

    2014-01-01

    Highlights: • Syngas fermentation process is limited by gas-to-liquid mass transfer. • A novel monolithic biofilm reactor (MBR) for efficient mass transfer was developed. • MBR with slug flow resulted in higher k L a than bubble column reactor (BCR). • MBR enhanced ethanol productivity by 53% compared to BCR. • MBR was demonstrated as a promising reactor configuration for syngas fermentation. - Abstract: Syngas fermentation is a promising process for producing fuels and chemicals from lignocellulosic biomass. Currently syngas fermentation faces several engineering challenges, with gas-to-liquid mass transfer limitation representing the major bottleneck. The aim of this work is to evaluate the performance of a monolithic biofilm reactor (MBR) as a novel reactor configuration for syngas fermentation. The volumetric mass transfer coefficient (k L a) of the MBR was evaluated in abiotic conditions within a wide range of gas flow rates (i.e., gas velocity in monolithic channels) and liquid flow rates (i.e., liquid velocity in the channels). The k L a values of the MBR were higher than those of a controlled bubble column reactor (BCR) in certain conditions, due to the slug flow pattern in the monolithic channels. A continuous syngas fermentation using Clostridium carboxidivorans P7 was conducted in the MBR system under varying operational conditions, with the variables including syngas flow rate, liquid recirculation between the monolithic column and reservoir, and dilution rate. It was found that the syngas fermentation performance – measured by such parameters as syngas utilization efficiency, ethanol concentration and productivity, and ratio of ethanol to acetic acid – depended not only on the mass transfer efficiency but also on the biofouling or abrading of the biofilm attached on the monolithic channel wall. At a condition of 300 mL/min of syngas flow rate, 500 mL/min of liquid flow rate, and 0.48 day −1 of dilution rate, the MBR produced much higher

  8. JCE Feature Columns

    Science.gov (United States)

    Holmes, Jon L.

    1999-05-01

    The Features area of JCE Online is now readily accessible through a single click from our home page. In the Features area each column is linked to its own home page. These column home pages also have links to them from the online Journal Table of Contents pages or from any article published as part of that feature column. Using these links you can easily find abstracts of additional articles that are related by topic. Of course, JCE Online+ subscribers are then just one click away from the entire article. Finding related articles is easy because each feature column "site" contains links to the online abstracts of all the articles that have appeared in the column. In addition, you can find the mission statement for the column and the email link to the column editor that I mentioned above. At the discretion of its editor, a feature column site may contain additional resources. As an example, the Chemical Information Instructor column edited by Arleen Somerville will have a periodically updated bibliography of resources for teaching and using chemical information. Due to the increase in the number of these resources available on the WWW, it only makes sense to publish this information online so that you can get to these resources with a simple click of the mouse. We expect that there will soon be additional information and resources at several other feature column sites. Following in the footsteps of the Chemical Information Instructor, up-to-date bibliographies and links to related online resources can be made available. We hope to extend the online component of our feature columns with moderated online discussion forums. If you have a suggestion for an online resource you would like to see included, let the feature editor or JCE Online (jceonline@chem.wisc.edu) know about it. JCE Internet Features JCE Internet also has several feature columns: Chemical Education Resource Shelf, Conceptual Questions and Challenge Problems, Equipment Buyers Guide, Hal's Picks, Mathcad

  9. [Preparation of monolithic materials and their applications in proteomic analysis].

    Science.gov (United States)

    Liang, Yu; Zhang, Lihua; Zhang, Yukui

    2011-09-01

    Proteomics is one of the core contents of life science in the post-genomic era, among which it is very important to develop the analytical techniques with high resolution, high sensitivity, high accuracy and high throughput. With the advantages of facile preparation, fast mass transfer, low backpressure and easy modification, monolithic materials have been widely used in proteomic analysis. This review summarizes the preparation methods of different kinds of monolithic materials (including organic polymer monoliths, silica-based monoliths, organic-inorganic hybrid silica monoliths) and their applications in proteomic study such as the digestion of proteins, the separation of proteins or peptides, high throughput analysis integrating online digestion, separation and identification.

  10. Behavior of Reinforced Hybrid Concrete Corbel-Column Connection with Vertical Construction Joint

    Directory of Open Access Journals (Sweden)

    Ammar Yasir Ali

    2017-03-01

    Full Text Available In this paper, shear behavior of reinforced hybrid concrete connection of corbel-column is experimentally investigated. Nine homogenous and hybrid concrete corbel-column connections subjected to vertical applied loads were constructed and tested within two test groups (A, B. The experimental program included the effect of several variables such as type of hybrid concrete;high strength concrete (HSC or steel fiber reinforced concrete (SFRC, monolithic casting of hybrid concrete connection, and presence of construction joint at the interface of corbel-column. Experimental results showed significant effects of concrete hybridization on the structural behavior of connection specimens such as: ultimate strength, cracking loads, cracking patterns, and failure modes. Hybridization process in group (A included hybrid connection of corbel-column with HSC or SFRC corbel instated of NSC. This process led to increase the capacity of connection by (26%, 38% and shear cracking loads by (20%, 120% respectively. Moreover, connections of hybrid concrete corbels cast monolithically improved the shear capacity of corbels by (19%, 42% for HSC or SFRC respectively. In group (B, presence of construction joint at connection region reduced the shear capacity of connectionsby (10% to 22% and cracking loads by (23%-62% compared with connections cast monolithically.

  11. Monolithic graphene oxide sheets with controllable composition.

    Science.gov (United States)

    Chu, Jae Hwan; Kwak, Jinsung; Kim, Sung-Dae; Lee, Mi Jin; Kim, Jong Jin; Park, Soon-Dong; Choi, Jae-Kyung; Ryu, Gyeong Hee; Park, Kibog; Kim, Sung Youb; Kim, Ji Hyun; Lee, Zonghoon; Kim, Young-Woon; Kwon, Soon-Yong

    2014-02-28

    Graphene oxide potentially has multiple applications and is typically prepared by solution-based chemical means. To date, the synthesis of a monolithic form of graphene oxide that is crucial to the precision assembly of graphene-based devices has not been achieved. Here we report the physical approach to produce monolithic graphene oxide sheets on copper foil using solid carbon, with tunable oxygen-to-carbon composition. Experimental and theoretical studies show that the copper foil provides an effective pathway for carbon diffusion, trapping the oxygen species dissolved in copper and enabling the formation of monolithic graphene oxide sheets. Unlike chemically derived graphene oxide, the as-synthesized graphene oxide sheets are electrically active, and the oxygen-to-carbon composition can be tuned during the synthesis process. As a result, the resulting graphene oxide sheets exhibit tunable bandgap energy and electronic properties. Our solution-free, physical approach may provide a path to a new class of monolithic, two-dimensional chemically modified carbon sheets.

  12. Distillation Column Flooding Predictor

    Energy Technology Data Exchange (ETDEWEB)

    George E. Dzyacky

    2010-11-23

    The Flooding Predictor™ is a patented advanced control technology proven in research at the Separations Research Program, University of Texas at Austin, to increase distillation column throughput by over 6%, while also increasing energy efficiency by 10%. The research was conducted under a U. S. Department of Energy Cooperative Agreement awarded to George Dzyacky of 2ndpoint, LLC. The Flooding Predictor™ works by detecting the incipient flood point and controlling the column closer to its actual hydraulic limit than historical practices have allowed. Further, the technology uses existing column instrumentation, meaning no additional refining infrastructure is required. Refiners often push distillation columns to maximize throughput, improve separation, or simply to achieve day-to-day optimization. Attempting to achieve such operating objectives is a tricky undertaking that can result in flooding. Operators and advanced control strategies alike rely on the conventional use of delta-pressure instrumentation to approximate the column’s approach to flood. But column delta-pressure is more an inference of the column’s approach to flood than it is an actual measurement of it. As a consequence, delta pressure limits are established conservatively in order to operate in a regime where the column is never expected to flood. As a result, there is much “left on the table” when operating in such a regime, i.e. the capacity difference between controlling the column to an upper delta-pressure limit and controlling it to the actual hydraulic limit. The Flooding Predictor™, an innovative pattern recognition technology, controls columns at their actual hydraulic limit, which research shows leads to a throughput increase of over 6%. Controlling closer to the hydraulic limit also permits operation in a sweet spot of increased energy-efficiency. In this region of increased column loading, the Flooding Predictor is able to exploit the benefits of higher liquid

  13. Nuclear reactor control column

    International Nuclear Information System (INIS)

    Bachovchin, D.M.

    1982-01-01

    The nuclear reactor control column comprises a column disposed within the nuclear reactor core having a variable cross-section hollow channel and containing balls whose vertical location is determined by the flow of the reactor coolant through the column. The control column is divided into three basic sections wherein each of the sections has a different cross-sectional area. The uppermost section of the control column has the greatest crosssectional area, the intermediate section of the control column has the smallest cross-sectional area, and the lowermost section of the control column has the intermediate cross-sectional area. In this manner, the area of the uppermost section can be established such that when the reactor coolant is flowing under normal conditions therethrough, the absorber balls will be lifted and suspended in a fluidized bed manner in the upper section. However, when the reactor coolant flow falls below a predetermined value, the absorber balls will fall through the intermediate section and into the lowermost section, thereby reducing the reactivity of the reactor core and shutting down the reactor

  14. Buckling of liquid columns

    NARCIS (Netherlands)

    Habibi, M.; Rahmani, Y.; Bonn, D.; Ribe, N.M.

    2010-01-01

    Under appropriate conditions, a column of viscous liquid falling onto a rigid surface undergoes a buckling instability. Here we show experimentally and theoretically that liquid buckling exhibits a hitherto unsuspected complexity involving three different modes—viscous, gravitational, and

  15. Solvent extraction columns

    International Nuclear Information System (INIS)

    Middleton, P.; Smith, J.R.

    1979-01-01

    In pulsed columns for use in solvent extraction processes, e.g. the reprocessing of nuclear fuel, the horizontal perforated plates inside the column are separated by interplate spacers manufactured from metallic neutron absorbing material. The spacer may be in the form of a spiral or concentric circles separated by radial limbs, or may be of egg-box construction. Suitable neutron absorbing materials include stainless steel containing boron or gadolinium, hafnium metal or alloys of hafnium. (UK)

  16. On the underestimated impact of the gelation temperature on macro- and mesoporosity in monolithic silica.

    Science.gov (United States)

    Meinusch, Rafael; Ellinghaus, Rüdiger; Hormann, Kristof; Tallarek, Ulrich; Smarsly, Bernd M

    2017-06-07

    The preparation of monolithic SiO 2 with bimodal porosity using a special sol-gel procedure ("Nakanishi process") generally shows a pronounced sensitivity towards several physico-chemical parameters of the initial solution (concentrations, precursors, pH, temperature, etc.). Thus, temporal and spatial variations of these parameters during the sol-gel reactions can affect the final meso- and macropore space with respect to the pore size distributions and homogeneity. In this study we thoroughly examine the sol-gel reaction in terms of the impact of temperature accuracy and homogeneity during the gelation and their effect on meso- and macropore space. The in-depth characterization of the macroporosity in monolithic SiO 2 rods, prepared by utilizing a highly homogeneous and accurate temperature profile, shows that a decrease of only 1.5 °C during the reaction doubles the mean size of the macropores in the analyzed temperature ranges (22.0-28.0 °C and 33.5-36.5 °C). Rheological measurements of the gelation points and the viscosity of the starting solutions prove that a higher reaction rate is the main reason for this marked temperature-sensitivity. Furthermore, the mesoporosity is affected to a surprising extent by the applied small temperature differences during the gelation reaction. This phenomenon is shown to be mainly caused by the temperature-dependent differences in macropore and skeleton dimensions and an inhomogeneous distribution of mesopore sizes within the skeleton. In essence, our study reveals that the impact of temperature on the formation of meso- and macroscale dimensions during the sol-gel process has been underestimated so far. The impact of a poor temperature homogeneity during monolith synthesis is exemplarily demonstrated by the application of monolithic silica capillary columns in HPLC.

  17. Fracture Analysis of Debonded Sandwich Columns Under Axial Compression

    DEFF Research Database (Denmark)

    May, A.; Avilés, F.; Berggreen, Christian

    A sandwich structure consists of two strong and stiff face sheets bonded to a weak low density core. The large separation between the face sheets provides increased bending rigidity and strength at low weight cost. Thus, sandwich structures frequently present better mechanical properties than...... monolithic structures of the same weight. The vast range of applications of such materials includes wind turbines, marine, and aerospace industries. In this work, geometrically nonlinear finite element analysis is conducted to investigate the fracture parameters and debond propagation of sandwich columns...... containing a face-to-core debond subjected to axial compression. Bidimensional finite element models of sandwich columns containing different size debonds centered at one face/core interface were developed and used in conjunction with linear elastic fracture mechanics to predict the stress intensity factors...

  18. Impact of biomolecule solute size on the transport and performance characteristics of analytical porous polymer monoliths.

    Science.gov (United States)

    Nischang, Ivo

    2014-08-08

    Porous monolithic poly(styrene-co-divinylbenzene) stationary phases in 4.6mm ID analytical format have been investigated with respect to their transport properties probed by solutes of biological origin varying vastly in size. Elucidation of several properties of these benchmark and robust materials gave complementary insight. These are: (i) the porous polymers' apparent dry-state microscopic appearance, (ii) the columns porosity probed by the biomolecules and modulated by mobile phase solvent composition, (iii) the impact of probe solute size on apparent retention at varying mobile phase solvent compositions, and (iv) the elution performance under both nonretained and retained elution conditions. By varying the volume percentage of acetonitrile in the mobile phase, it is demonstrated that the monolithic scaffold shows a variable porosity experienced in particular by the larger sized solutes, while the smaller solutes are gradually less affected. The nanoscale swelling and solvation of porous monolithic adsorbents resulting in gel porosity varied with mobile phase solvent composition was, therefore, indicated. The plate height curves for the solutes under nonretained conditions show a moderate increase at increased flow velocity while approaching plateau values. These plateau values were in conjunction with a trend of a decreased performance at an increased molecular weight of the solute. The systematic shape of the plate height curves at increased flow velocity indicates pre-asymptotic dispersion. This is because the column bed aspect ratio of length-to-diameter is equal or smaller than 10. Imposing retention on the solutes at a constant flow velocity deteriorates isocratic elution performance, more pronouncedly for the larger sized solutes at even weak retention. This is explained with slow pore fluid-gel interface diffusion. Additionally, the apparent retention factor for elution of the probe solutes becomes a function of flow rate, consequently a function of

  19. Test of the TRAPPISTe monolithic detector system

    Science.gov (United States)

    Soung Yee, L.; Álvarez, P.; Martin, E.; Cortina, E.; Ferrer, C.

    2013-12-01

    A monolithic pixel detector named TRAPPISTe-2 has been developed in Silicon-on-Insulator (SOI) technology. A p-n junction is implanted in the bottom handle wafer and connected to readout electronics integrated in the top active layer. The two parts are insulated from each other by a buried oxide layer resulting in a monolithic detector. Two small pixel matrices have been fabricated: one containing a 3-transistor readout and a second containing a charge sensitive amplifier readout. These two readout structures have been characterized and the pixel matrices were tested with an infrared laser source. The readout circuits are adversely affected by the backgate effect, which limits the voltage that can be applied to the metal back plane to deplete the sensor, thus narrowing the depletion width of the sensor. Despite the low depletion voltages, the integrated pixel matrices were able to respond to and track a laser source.

  20. Monolithic pixel detectors for high energy physics

    CERN Document Server

    Snoeys, W

    2013-01-01

    Monolithic pixel detectors integrating sensor matrix and readout in one piece of silicon have revolutionized imaging for consumer applications, but despite years of research they have not yet been widely adopted for high energy physics. Two major requirements for this application, radiation tolerance and low power consumption, require charge collection by drift for the most extreme radiation levels and an optimization of the collected signal charge over input capacitance ratio ( Q / C ). It is shown that monolithic detectors can achieve Q / C for low analog power consumption and even carryout the promise to practically eliminate analog power consumption, but combining suf fi cient Q / C , collection by drift, and integration of readout circuitry within the pixel remains a challenge. An overview is given of different approaches to address this challenge, with possible advantages and disadvantages.

  1. Update On Monolithic Fuel Fabrication Development

    Energy Technology Data Exchange (ETDEWEB)

    C. R Clark; J. M. Wight; G. C. Knighton; G. A. Moore; J. F. Jue

    2005-11-01

    Efforts to develop a viable monolithic research reactor fuel plate have continued at Idaho National Laboratory. These efforts have concentrated on both fabrication process refinement and scale-up to produce full sized fuel plates. Advancements have been made in the production of U-Mo foil including full sized foils. Progress has also been made in the friction stir welding and transient liquid phase bonding fabrication processes resulting in better bonding, more stable processes and the ability to fabricate larger fuel plates.

  2. FLUIDIZED BED STEAM REFORMER MONOLITH FORMATION

    Energy Technology Data Exchange (ETDEWEB)

    Jantzen, C

    2006-12-22

    Fluidized Bed Steam Reforming (FBSR) is being considered as an alternative technology for the immobilization of a wide variety of aqueous high sodium containing radioactive wastes at various DOE facilities in the United States. The addition of clay, charcoal, and a catalyst as co-reactants converts aqueous Low Activity Wastes (LAW) to a granular or ''mineralized'' waste form while converting organic components to CO{sub 2} and steam, and nitrate/nitrite components, if any, to N{sub 2}. The waste form produced is a multiphase mineral assemblage of Na-Al-Si (NAS) feldspathoid minerals with cage-like structures that atomically bond radionuclides like Tc-99 and anions such as SO{sub 4}, I, F, and Cl. The granular product has been shown to be as durable as LAW glass. Shallow land burial requires that the mineralized waste form be able to sustain the weight of soil overburden and potential intrusion by future generations. The strength requirement necessitates binding the granular product into a monolith. FBSR mineral products were formulated into a variety of monoliths including various cements, Ceramicrete, and hydroceramics. All but one of the nine monoliths tested met the <2g/m{sup 2} durability specification for Na and Re (simulant for Tc-99) when tested using the Product Consistency Test (PCT; ASTM C1285). Of the nine monoliths tested the cements produced with 80-87 wt% FBSR product, the Ceramicrete, and the hydroceramic produced with 83.3 wt% FBSR product, met the compressive strength and durability requirements for an LAW waste form.

  3. FRACTURE-RESISTANT MONOLITHIC DENTAL CROWNS

    Science.gov (United States)

    Zhang, Yu; Mai, Zhisong; Barani, Amir; Bush, Mark; Lawn, Brian

    2016-01-01

    Objective To quantify the splitting resistance of monolithic zirconia, lithium disilicate and nanoparticle-composite dental crowns. Methods Fracture experiments were conducted on anatomically-correct monolithic crown structures cemented to standard dental composite dies, by axial loading of a hard sphere placed between the cusps. The structures were observed in situ during fracture testing, and critical loads to split the structures were measured. Extended finite element modeling (XFEM), with provision for step-by-step extension of embedded cracks, was employed to simulate full failure evolution. Results Experimental measurements and XFEM predictions were self consistent within data scatter. In conjunction with a fracture mechanics equation for critical splitting load, the data were used to predict load-sustaining capacity for crowns on actual dentin substrates and for loading with a sphere of different size. Stages of crack propagation within the crown and support substrate were quantified. Zirconia crowns showed the highest fracture loads, lithium disilicate intermediate, and dental nanocomposite lowest. Dental nanocomposite crowns have comparable fracture resistance to natural enamel. Significance The results confirm that monolithic crowns are able to sustain high bite forces. The analysis indicates what material and geometrical properties are important in optimizing crown performance and longevity. PMID:26792623

  4. Characterization of SOI monolithic detector system

    Science.gov (United States)

    Álvarez-Rengifo, P. L.; Soung Yee, L.; Martin, E.; Cortina, E.; Ferrer, C.

    2013-12-01

    A monolithic active pixel sensor for charged particle tracking was developed. This research is performed within the framework of an R&D project called TRAPPISTe (Tracking Particles for Physics Instrumentation in SOI Technology) whose aim is to evaluate the feasibility of developing a Monolithic Active Pixel Sensor (MAPS) with Silicon-on-Insulator (SOI) technology. Two chips were fabricated: TRAPPISTe-1 and TRAPPISTe-2. TRAPPISTe-1 was produced at the WINFAB facility at the Université catholique de Louvain (UCL), Belgium, in a 2 μm fully depleted (FD-SOI) CMOS process. TRAPPISTe-2 was fabricated with the LAPIS 0.2 μm FD-SOI CMOS process. The electrical characterization on single transistor test structures and of the electronic readout for the TRAPPISTe series of monolithic pixel detectors was carried out. The behavior of the prototypes’ electronics as a function of the back voltage was studied. Results showed that both readout circuits exhibited sensitivity to the back voltage. Despite this unwanted secondary effect, the responses of TRAPPISTe-2 amplifiers can be improved by a variation in the circuit parameters.

  5. Fracture-resistant monolithic dental crowns.

    Science.gov (United States)

    Zhang, Yu; Mai, Zhisong; Barani, Amir; Bush, Mark; Lawn, Brian

    2016-03-01

    To quantify the splitting resistance of monolithic zirconia, lithium disilicate and nanoparticle-composite dental crowns. Fracture experiments were conducted on anatomically-correct monolithic crown structures cemented to standard dental composite dies, by axial loading of a hard sphere placed between the cusps. The structures were observed in situ during fracture testing, and critical loads to split the structures were measured. Extended finite element modeling (XFEM), with provision for step-by-step extension of embedded cracks, was employed to simulate full failure evolution. Experimental measurements and XFEM predictions were self-consistent within data scatter. In conjunction with a fracture mechanics equation for critical splitting load, the data were used to predict load-sustaining capacity for crowns on actual dentin substrates and for loading with a sphere of different size. Stages of crack propagation within the crown and support substrate were quantified. Zirconia crowns showed the highest fracture loads, lithium disilicate intermediate, and dental nanocomposite lowest. Dental nanocomposite crowns have comparable fracture resistance to natural enamel. The results confirm that monolithic crowns are able to sustain high bite forces. The analysis indicates what material and geometrical properties are important in optimizing crown performance and longevity. Copyright © 2015 Academy of Dental Materials. All rights reserved.

  6. Metal oxide nanorod arrays on monolithic substrates

    Energy Technology Data Exchange (ETDEWEB)

    Gao, Pu-Xian; Guo, Yanbing; Ren, Zheng

    2018-01-02

    A metal oxide nanorod array structure according to embodiments disclosed herein includes a monolithic substrate having a surface and multiple channels, an interface layer bonded to the surface of the substrate, and a metal oxide nanorod array coupled to the substrate surface via the interface layer. The metal oxide can include ceria, zinc oxide, tin oxide, alumina, zirconia, cobalt oxide, and gallium oxide. The substrate can include a glass substrate, a plastic substrate, a silicon substrate, a ceramic monolith, and a stainless steel monolith. The ceramic can include cordierite, alumina, tin oxide, and titania. The nanorod array structure can include a perovskite shell, such as a lanthanum-based transition metal oxide, or a metal oxide shell, such as ceria, zinc oxide, tin oxide, alumina, zirconia, cobalt oxide, and gallium oxide, or a coating of metal particles, such as platinum, gold, palladium, rhodium, and ruthenium, over each metal oxide nanorod. Structures can be bonded to the surface of a substrate and resist erosion if exposed to high velocity flow rates.

  7. Electrically driven monolithic subwavelength plasmonic interconnect circuits.

    Science.gov (United States)

    Liu, Yang; Zhang, Jiasen; Liu, Huaping; Wang, Sheng; Peng, Lian-Mao

    2017-10-01

    In the post-Moore era, an electrically driven monolithic optoelectronic integrated circuit (OEIC) fabricated from a single material is pursued globally to enable the construction of wafer-scale compact computing systems with powerful processing capabilities and low-power consumption. We report a monolithic plasmonic interconnect circuit (PIC) consisting of a photovoltaic (PV) cascading detector, Au-strip waveguides, and electrically driven surface plasmon polariton (SPP) sources. These components are fabricated from carbon nanotubes (CNTs) via a CMOS (complementary metal-oxide semiconductor)-compatible doping-free technique in the same feature size, which can be reduced to deep-subwavelength scale (~λ/7 to λ/95, λ = 1340 nm) compared with the 14-nm technique node. An OEIC could potentially be configured as a repeater for data transport because of its "photovoltaic" operation mode to transform SPP energy directly into electricity to drive subsequent electronic circuits. Moreover, chip-scale throughput capability has also been demonstrated by fabricating a 20 × 20 PIC array on a 10 mm × 10 mm wafer. Tailoring photonics for monolithic integration with electronics beyond the diffraction limit opens a new era of chip-level nanoscale electronic-photonic systems, introducing a new path to innovate toward much faster, smaller, and cheaper computing frameworks.

  8. An overview of monolithic zirconia in dentistry

    Directory of Open Access Journals (Sweden)

    Özlem Malkondu

    2016-07-01

    Full Text Available Zirconia restorations have been used successfully for years in dentistry owing to their biocompatibility and good mechanical properties. Because of their lack of translucency, zirconia cores are generally veneered with porcelain, which makes restorations weaker due to failure of the adhesion between the two materials. In recent years, all-ceramic zirconia restorations have been introduced in the dental sector with the intent to solve this problem. Besides the elimination of chipping, the reduced occlusal space requirement seems to be a clear advantage of monolithic zirconia restorations. However, scientific evidence is needed to recommend this relatively new application for clinical use. This mini-review discusses the current scientific literature on monolithic zirconia restorations. The results of in vitro studies suggested that monolithic zirconia may be the best choice for posterior fixed partial dentures in the presence of high occlusal loads and minimal occlusal restoration space. The results should be supported with much more in vitro and particularly in vivo studies to obtain a final conclusion.

  9. Five points on columns

    Directory of Open Access Journals (Sweden)

    Kathleen S Rockland

    2010-06-01

    Full Text Available Abstract “Column,” like “gene,” has both conceptual and linguistic shortcomings. The simple question “what is a column” is not easy to answer and the word itself is not easy to replace. In the present article, I have selected five points, in no way comprehensive or canonical, but which may nevertheless serve as a prompt and aid for further discussions and reevaluation. These are: that anatomical columns are not solid structures, that they are part of locally interdigitating systems, that any delimited column also participates in a widely distributed network, that columns are not an obligatory cortical feature, and that columns (as “modules” occur widely in the brain in non-cortical structures. I focus on the larger scale macrocolumns, mainly from an anatomical perspective. My position is that cortical organization is inherently dynamic and likely to incorporate multiple processing styles. One can speculate that the distributed mappings within areas like piriform cortex may resemble at least one mode of neocortical processing strategy.

  10. Decoding the Pantheon Columns

    Directory of Open Access Journals (Sweden)

    Gerd Grasshoff

    2014-06-01

    Full Text Available The goal of this study has been to reconstruct the design principles underlying the construction of the Pantheon’s portico columns as well as to demonstrate how digital investigation methods and models can be used to improve our understanding of ancient architectural knowledge. Thanks to the data of the Bern Digital Pantheon Model, a synthesis of all the scanned surface points obtained during a digitization campaign of the Karman Center for Advanced Studies in the Humanities of the University of Bern in 2005, we have been able to determine empirically the column profiles of the portico with unprecedented precision. A second stage of our investigation involved explaining the profile of the column shafts by a construction model that takes into account the parameters recommended by Vitruvius and design methods such as those that can be found in the construction drawings discovered at Didyma. Our analysis shows that the design principles of the portico’s columns can be successfully reconstructed, and has led to the surprising result that at least two different variants of a simple circle construction were used. Finally, we have been able to deduce from the distribution of the different profile types among the columns that the final profiles were designed and executed in Rome.

  11. Assembly for connecting the column ends of two capillary columns

    International Nuclear Information System (INIS)

    Kolb, B.; Auer, M.; Pospisil, P.

    1984-01-01

    In gas chromatography, the column ends of two capillary columns are inserted into a straight capillary from both sides forming annular gaps. The capillary is located in a tee out of which the capillary columns are sealingly guided, and to which carrier gas is supplied by means of a flushing flow conduit. A ''straight-forward operation'' having capillary columns connected in series and a ''flush-back operation'' are possible. The dead volume between the capillary columns can be kept small

  12. Slender CRC Columns

    OpenAIRE

    Aarup, Bendt; Jensen, Lars Rom; Ellegaard, Peter

    2005-01-01

    CRC is a high-performance steel fibre reinforced concrete with a typical compressive strength of 150 MPa. Design methods for a number of structural elements have been developed since CRC was invented in 1986, but the current project set out to further investigate the range of columns for which current design guides can be used. The columns tested had a slenderness varying from 1.11 to 12.76 and a reinforcement ratio (area of rebar to area of concrete) ranging from 0 to 8.8 %. A total of 77 te...

  13. Evaluation of the resistance to progressive collapse of monolithic reinforced concrete frame buildingswith separate amplified floors

    Directory of Open Access Journals (Sweden)

    Domarova Ekaterina Vladimirovna

    2014-02-01

    Full Text Available In the article the authors propose a simplified method of dynamic analysis of the resistance to progressive collapse of a fragment of the building bearing system with amplified floors. This method is based on representing the building bearing system as a dynamic model with a denumerable number of degrees of freedom, in which the resistance of the system is provided mainly by the behavior of the columns. The degrees of freedom number is determined by the number of floors «hanging» to amplified floors. Thecontribution of slabs in the total system resistance is not taken into account. Stress-strain state of the columns is determined by the non-linear resistance diagram, including three stages: elastic, elastic with cracks and plastic stage connected with plastic yield in the steel of the columns. The criterion of sustainability to the progressive collapse is relative strain of steel of the undestroyed columns. A numerical example of the calculation of the building resistance to progressive collapse in case of sudden destruction of one vertical element based on proposed theoretical method is offered. A model with two numbers of degrees was considered. The suggested method allows estimating the strength, deformability and stability of monolithic reinforced concrete frame buildings with separate amplified floors. In the future it is intended to complicate the model by the accounting for the influence of deformation and constructive solution of the slabs on the stiffness characteristics of the model as a system with a finite number of degrees of freedom.

  14. Practical column design guide

    CERN Document Server

    Nitsche, M

    2017-01-01

    This book highlights the aspects that need to be considered when designing distillation columns in practice. It discusses the influencing parameters as well as the equations governing them, and presents several numerical examples. The book is intended both for experienced designers and for those who are new to the subject.

  15. Columns in Clay

    Science.gov (United States)

    Leenhouts, Robin

    2010-01-01

    This article describes a clay project for students studying Greece and Rome. It provides a wonderful way to learn slab construction techniques by making small clay column capitols. With this lesson, students learn architectural vocabulary and history, understand the importance of classical architectural forms and their influence on today's…

  16. Steel column base classification

    OpenAIRE

    Jaspart, J.P.; Wald, F.; Weynand, K.; Gresnigt, A.M.

    2008-01-01

    The influence of the rotational characteristics of the column bases on the structural frame response is discussed and specific design criteria for stiffness classification into semi-rigid and rigid joints are derived. The particular case of an industrial portal frame is then considered. Peer reviewed

  17. European Analytical Column

    DEFF Research Database (Denmark)

    Karlberg, B.; Grasserbauer, M.; Andersen, Jens Enevold Thaulov

    2009-01-01

    The European Analytical Column has once more invited a guest columnist to give his views on various matters related to analytical chemistry in Europe. This year, we have invited Professor Manfred Grasserbauer of the Vienna University of Technology to present some of the current challenges for Eur...

  18. Selective oxidation of cyclohexene through gold functionalized silica monolith microreactors

    Science.gov (United States)

    Alotaibi, Mohammed T.; Taylor, Martin J.; Liu, Dan; Beaumont, Simon K.; Kyriakou, Georgios

    2016-04-01

    Two simple, reproducible methods of preparing evenly distributed Au nanoparticle containing mesoporous silica monoliths are investigated. These Au nanoparticle containing monoliths are subsequently investigated as flow reactors for the selective oxidation of cyclohexene. In the first strategy, the silica monolith was directly impregnated with Au nanoparticles during the formation of the monolith. The second approach was to pre-functionalize the monolith with thiol groups tethered within the silica mesostructure. These can act as evenly distributed anchors for the Au nanoparticles to be incorporated by flowing a Au nanoparticle solution through the thiol functionalized monolith. Both methods led to successfully achieving even distribution of Au nanoparticles along the length of the monolith as demonstrated by ICP-OES. However, the impregnation method led to strong agglomeration of the Au nanoparticles during subsequent heating steps while the thiol anchoring procedure maintained the nanoparticles in the range of 6.8 ± 1.4 nm. Both Au nanoparticle containing monoliths as well as samples with no Au incorporated were tested for the selective oxidation of cyclohexene under constant flow at 30 °C. The Au free materials were found to be catalytically inactive with Au being the minimum necessary requirement for the reaction to proceed. The impregnated Au-containing monolith was found to be less active than the thiol functionalized Au-containing material, attributable to the low metal surface area of the Au nanoparticles. The reaction on the thiol functionalized Au-containing monolith was found to depend strongly on the type of oxidant used: tert-butyl hydroperoxide (TBHP) was more active than H2O2, likely due to the thiol induced hydrophobicity in the monolith.

  19. Pharmaceutical-grade pre-miR-29 purification using an agmatine monolithic support.

    Science.gov (United States)

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

    2014-11-14

    MicroRNA-based therapeutic applications have fostered a growing interest in the development of microRNAs purification processes in order to obtain the final product with high purity degree, good quality and biologically active. The pre-miR-29 deficiency or overexpression has been associated to a number of clinically important diseases, and its therapeutic application can be considered. Monolithic columns emerged as a new class of chromatographic supports used in the plasmid DNA purification platforms, being an interesting alternative to the conventional particle-based columns. Thus, the current work describes, for the first time, a new affinity chromatography method that combines the high selectivity of agmatine ligands with the versatility of monoliths to specifically and efficiently purify pre-miR-29 from other small RNA species and Rhodovulum sulfidophilum impurities. The effect of different flow rates on pre-miR-29 separation was also evaluated. Moreover, breakthrough experiments were designed to study the effect of different RNA concentrations on the modified monolithic support binding capacity, being verified that the dynamic binding capacity for RNA molecules is dependent of the feed concentration. In order to achieve higher efficiency and selectivity, three different binding and elution strategies based on increased sodium chloride (1.75-3M) or arginine (100mM) and decreased ammonium sulfate (2.4-0M) stepwise gradients are described to purify pre-miR-29. As a matter of fact, by employing elution strategies using sodium chloride or arginine, an improvement in the final pre-miR-29 yields (97.33 and 94.88%, respectively) as well as purity (75.21 and 90.11%, respectively) were obtained. Moreover, the quality control analysis revealed that the level of impurities (proteins, endotoxins, sRNA) in the final pre-miR-29 sample was negligible. In fact, this new monolithic support arises as a powerful instrument on the microRNA purification to be used in further

  20. Application of monolithic affinity HPLC column for rapid determination of malt glycoproteins

    Czech Academy of Sciences Publication Activity Database

    Benkovská, Dagmar; Flodrová, Dana; Bobálová, Janette

    2013-01-01

    Roč. 36, č. 5 (2013), s. 561-572 ISSN 1082-6076 R&D Projects: GA MŠk 1M0570 Institutional research plan: CEZ:AV0Z4031919 Keywords : concanavalin A * glycosylation * barley Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 0.638, year: 2013

  1. Narrow-bore core–shell particles and monolithic columns in the analysis of silybin diastereoisomers

    Czech Academy of Sciences Publication Activity Database

    Marhol, Petr; Gažák, Radek; Bednář, P.; Křen, Vladimír

    2011-01-01

    Roč. 34, 16-17 (2011), s. 2206-2213 ISSN 1615-9306 R&D Projects: GA MŠk(CZ) ME10027; GA ČR GAP207/10/0288 Institutional research plan: CEZ:AV0Z50200510 Keywords : chromolith * kinetex * Core - shell Subject RIV: CC - Organic Chemistry Impact factor: 2.733, year: 2011

  2. Determination of ghrelin analogs in plasma samples by liquid chromatography-mass spectrometry using monolithic column

    Czech Academy of Sciences Publication Activity Database

    Zemenová, Jana; Železná, Blanka; Maletínská, Lenka; Sýkora, D.

    2016-01-01

    Roč. 22, Suppl S2 (2016), S105 ISSN 1075-2617. [European Peptide Symposium /34./ and International Peptide Symposium /8./. 04.09.2016-09.09.2016, Leipzig] Institutional support: RVO:61388963 Keywords : ghrelin * LC-MS Subject RIV: CE - Biochemistry

  3. Microchip-based monolithic column for high performance liquid chromatography Project

    Data.gov (United States)

    National Aeronautics and Space Administration — Fabricate the microchannels using DDL facilities. Develop a process for in situ polymerization inside the microchannels and optimize the chemistry Perform separation...

  4. Evaluation of steric exclusion chromatography on cryogel column for the separation of serum proteins.

    Science.gov (United States)

    Wang, Chuan; Bai, Shu; Tao, Shi-Peng; Sun, Yan

    2014-03-14

    Steric exclusion chromatography (SXC) is a new mode of protein chromatography, in which large proteins are retained on hydrophilic stationary phase surface due to the steric exclusion of polyethylene glycol (PEG) in the mobile phase, and thereafter the retained proteins can be eluted by reducing PEG concentration. In this work, SXC was evaluated on a polyacrylamide cryogel monolith. Microscopic observation of γ-globulin precipitates on the gel surface in SXC was reported for the first time. Due to the compact packing of protein precipitates on the stationary phase surface, the dynamic retention capacity of the cryogel monolith for γ-globulin reached 20 mg/mL bed volume, much higher than those of cryogel beds in adsorption-based chromatography. The effect of molecular weight and concentration of PEG, solution pH and salt concentration on protein retention capacity was in agreement with the earlier work on SXC. Because the cryogel monoliths with interconnected macropores (10-100 μm) allow much easy flow-through of viscous PEG buffer, the SXC can be operated at low back pressure. Hence, the cryogel monoliths are more suitable for SXC than other monoliths of narrow pores reported previously. In the separation of bovine serum proteins, albumin was recovered in the breakthrough fraction with high purity, and globulin was over eight times concentrated in the elution pool. This work has, thus, demonstrated the rapid serum protein separation and concentration by SXC on the cryogel monolith columns. Copyright © 2014 Elsevier B.V. All rights reserved.

  5. Fine-grain concrete from mining waste for monolithic construction

    Science.gov (United States)

    Lesovik, R. V.; Ageeva, M. S.; Lesovik, G. A.; Sopin, D. M.; Kazlitina, O. V.; Mitrokhin, A. A.

    2018-03-01

    The technology of a monolithic construction is a well-established practice among most Russian real estate developers. The strong points of the technology are low cost of materials and lower demand for qualified workers. The monolithic construction uses various types of reinforced slabs and foamed concrete, since they are easy to use and highly durable; they also need practically no additional treatment.

  6. Time-based position estimation in monolithic scintillator detectors

    NARCIS (Netherlands)

    Tabacchini, V.; Borghi, G.; Schaart, D.R.

    2015-01-01

    Gamma-ray detectors based on bright monolithic scintillation crystals coupled to pixelated photodetectors are currently being considered for several applications in the medical imaging field. In a typical monolithic detector, both the light intensity and the time of arrival of the earliest

  7. A novel photocatalytic monolith reactor for multiphase heterogeneous photocatalysis

    NARCIS (Netherlands)

    Du, P.; Carneiro, J.T.; Moulijn, J.A.; Mul, Guido

    2008-01-01

    A novel reactor for multi-phase photocatalysis is presented, the so-called internally illuminated monolith reactor (IIMR). In the concept of the IIMR, side light emitting fibers are placed inside the channels of a ceramic monolith, equipped with a TiO2 photocatalyst coated on the wall of each

  8. Hydrogel coated monoliths for enzymatic hydrolysis of penicillin G

    NARCIS (Netherlands)

    De Lathouder, K.M.; 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

  9. Energy Absorption of Monolithic and Fibre Reinforced Aluminium Cylinders

    NARCIS (Netherlands)

    De Kanter, J.L.C.G.

    2006-01-01

    Summary accompanying the thesis: Energy Absorption of Monolithic and Fibre Reinforced Aluminium Cylinders by Jens de Kanter This thesis presents the investigation of the crush behaviour of both monolithic aluminium cylinders and externally fibre reinforced aluminium cylinders. The research is based

  10. Monolithic LTCC seal frame and lid

    Energy Technology Data Exchange (ETDEWEB)

    Krueger, Daniel S.; Peterson, Kenneth A.; Stockdale, Dave; Duncan, James Brent; Riggs, Bristen

    2016-06-21

    A method for forming a monolithic seal frame and lid for use with a substrate and electronic circuitry comprises the steps of forming a mandrel from a ceramic and glass based material, forming a seal frame and lid block from a ceramic and glass based material, creating a seal frame and lid by forming a compartment and a plurality of sidewalls in the seal frame and lid block, placing the seal frame and lid on the mandrel such that the mandrel fits within the compartment, and cofiring the seal frame and lid block.

  11. Safety characteristics of the monolithic CFC divertor

    International Nuclear Information System (INIS)

    Zucchetti, M.; Merola, M.; Matera, R.

    1994-01-01

    The main distinguishing feature of the monolithic CFC divertor is the use of a single material, a carbon fibre reinforced carbon, for the protective armour, the heat sink and the cooling channels. This removes joint interface problems which are one of the most important concerns related to the reference solutions of the ITER CDA divertor. An activation analysis of the different coolant options for this concept is presented. It turns out that neither short-term nor long-term activation are a concern for any coolants investigated. Therefore the proposed concept proves to be attractive from a safety stand-point also. ((orig.))

  12. Safety characteristics of the monolithic CFC divertor

    Science.gov (United States)

    Zucchetti, M.; Merola, M.; Matera, R.

    1994-09-01

    The main distinguishing feature of the monolithic CFC divertor is the use of a single material, a carbon fibre reinforced carbon, for the protective armour, the heat sink and the cooling channels. This removes joint interface problems which are one of the most important concerns related to the reference solutions of the ITER CDA divertor. An activation analysis of the different coolant options for this concept is presented. It turns out that neither short-term nor long-term activation are a concern for any coolants investigated. Therefore the proposed concept proves to be attractive from a safety stand-point also.

  13. The art and science of forming packed analytical high-performance liquid chromatography columns.

    Science.gov (United States)

    Kirkland, J J; Destefano, J J

    2006-09-08

    Columns of packed particles still are the most popular devices for high-performance liquid chromatography (HPLC) separations because of their great utility, excellent performance and wide variety. However, the forming of packed beds for efficient, stable columns traditionally has been an art where the basics of how to form optimum beds generally was not well understood. The recent development of monolith rods was introduced in part to overcome the difficulty of producing stable beds of packing particles. However, these materials are less versatile than packed particle columns. Technology developments in recent years have produced a better understanding among those skilled in the practice of how to form optimized packed beds, and this has led to widely available, high-quality commercial columns. This presentation discusses the developments that led to the present state of column packing technology. Important steps in the packing of efficient, stable beds are described. The key step of selecting the best solvent for the slurry packing method is emphasized. Factors affecting the mechanical stability of packed columns also are discussed. The early art of packing columns now has evolved into a more scientific approach that allows the packing of good columns with a minimum of effort and time.

  14. Nine Words - Nine Columns

    DEFF Research Database (Denmark)

    Trempe Jr., Robert B.; Buthke, Jan

    2016-01-01

    of computational and mechanical processes towards an anesthetic. Each team received a single word, translating and evolving that word first into a double-curved computational surface, next a ruled computational surface, and then a physically shaped foam mold via a 6-axis robot. The foam molds then operated...... as formwork for the shaping of wood veneer. The resulting columns ‘wear’ every aspect of this design pipeline process and display the power of process towards an architectural resolution....

  15. Slender CRC Columns

    DEFF Research Database (Denmark)

    Aarup, Bendt; Jensen, Lars Rom; Ellegaard, Peter

    2005-01-01

    in standard fire conditions. The tests showed good correlation between test results and results calculated according to established deisgn guides. The fire tests demonstrate that the load capacity of slender columns can be reduced very quickly due to thermal stresses and a reduction of stiffness - also...... in cases where temperature at the rebar is still relatively low. However, guidelines for achieving acceptable fire resistance can be determined based on the test results....

  16. Nine Words - Nine Columns

    DEFF Research Database (Denmark)

    Trempe Jr., Robert B.; Buthke, Jan

    2016-01-01

    This book records the efforts of a one-week joint workshop between Master students from Studio 2B of Arkitektskolen Aarhus and Master students from the Harbin Institute of Technology in Harbin, China. The workshop employed nine action words to instigate team-based investigation into the effects o...... as formwork for the shaping of wood veneer. The resulting columns ‘wear’ every aspect of this design pipeline process and display the power of process towards an architectural resolution....

  17. Less common applications of monoliths: V. Monolithic scaffolds modified with nanostructures for chromatographic separations and tissue engineering.

    Science.gov (United States)

    Krenkova, Jana; Foret, Frantisek; Svec, Frantisek

    2012-06-01

    Scaffolds modified with nanostructures are recently finding use in a broad range of applications spanning from chromatographic separations to tissue engineering. This continuation of the review series on design and applications of monolithic materials covers some of the less common monoliths including use of nanostructures in preparation, modifications, and applications. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Growth techniques for monolithic YBCO solenoidal magnets

    International Nuclear Information System (INIS)

    Scruggs, S.J.; Putman, P.T.; Fang, H.; Alessandrini, M.; Salama, K.

    2006-01-01

    The possibility of growing large single domain YBCO solenoids by the use of a large seed has been investigated. There are two known methods for producing a similar solenoid. This first is a conventional top seeded melt growth process followed by a post processing machining step to create the bore. The second involves using multiple seeds spaced around the magnet bore. The appeal of the new technique lies in decreasing processing time compared to the single seed technique, while avoiding alignment problems found in the multiple seeding technique. By avoiding these problems, larger diameter monoliths can be produced. Large diameter monoliths are beneficial because the maximum magnetic field produced by a trapped field magnet is proportional to the radius of the sample. Furthermore, the availability of trapped field magnets with large diameter could enable their use in applications that traditionally have been considered to require wound electromagnets, such as beam bending magnets for particle accelerators or electric propulsion. A comparison of YBCO solenoids grown by the use of a large seed and grown by the use of two small seeds simulating multiple seeding is made. Trapped field measurements as well as microstructure evaluation were used in characterization of each solenoid. Results indicate that high quality growth occurs only in the vicinity of the seeds for the multiple seeded sample, while the sample with the large seeded exhibited high quality growth throughout the entire sample

  19. Catastrophic failure of a monolithic zirconia prosthesis.

    Science.gov (United States)

    Chang, Jae-Seung; Ji, Woon; Choi, Chang-Hoon; Kim, Sunjai

    2015-02-01

    Recently, monolithic zirconia restorations have received attention as an alternative to zirconia veneered with feldspathic porcelain to eliminate chipping failures of veneer ceramics. In this clinical report, a patient with mandibular edentulism received 4 dental implants in the interforaminal area, and a screw-retained monolithic zirconia prosthesis was fabricated. The patient also received a maxillary complete removable dental prosthesis over 4 anterior roots. At the 18-month follow-up, all of the zirconia cylinders were seen to be fractured, and the contacting abutment surfaces had lost structural integrity. The damaged abutments were replaced with new abutments, and a new prosthesis was delivered with a computer-assisted design and computer-assisted manufacturing fabricated titanium framework with denture teeth and denture base resins. At the 6-month recall, the patient did not have any problems. Dental zirconia has excellent physical properties; however, care should be taken to prevent excessive stresses on the zirconia cylinders when a screw-retained zirconia restoration is planned as a definitive prosthesis. Copyright © 2015 Editorial Council for the Journal of Prosthetic Dentistry. Published by Elsevier Inc. All rights reserved.

  20. A numerical study on seismic response of self-centring precast segmental columns at different post-tensioning forces

    Directory of Open Access Journals (Sweden)

    Ehsan Nikbakht

    Full Text Available Precast bridge columns have shown increasing demand over the past few years due to the advantages of such columns when compared against conventional bridge columns, particularly due to the fact that precast bridge columns can be constructed off site and erected in a short period of time. The present study analytically investigates the behaviour of self-centring precast segmental bridge columns under nonlinear-static and pseudo-dynamic loading at different prestressing strand levels. Self-centring segmental columns are composed of prefabricated reinforced concrete segments which are connected by central post-tensioning (PT strands. The present study develops a three dimensional (3D nonlinear finite element model for hybrid post-tensioned precast segmental bridge columns. The model is subjected to constant axial loading and lateral reverse cyclic loading. The lateral force displacement results of the analysed columns show good agreement with the experimental response of the columns. Bonded post-tensioned segmental columns at 25%, 40% and 70% prestressing strand stress levels are analysed and compared with an emulative monolithic conventional column. The columns with a higher initial prestressing strand levels show greater initial stiffness and strength but show higher stiffness reduction at large drifts. In the time-history analysis, the column samples are subjected to different earthquake records to investigate the effect post-tensioning force levels on their lateral seismic response in low and higher seismicity zones. The results indicate that, for low seismicity zones, post-tensioned segmental columns with a higher initial stress level deflect lower lateral peak displacement. However, in higher seismicity zones, applying a high initial stress level should be avoided for precast segmental self-centring columns with low energy dissipation capacity.

  1. Efficiency of short, small-diameter columns for reversed-phase liquid chromatography under practical operating conditions.

    Science.gov (United States)

    Ma, Yan; Chassy, Alexander W; Miyazaki, Shota; Motokawa, Masanori; Morisato, Kei; Uzu, Hideyuki; Ohira, Masayoshi; Furuno, Masahiro; Nakanishi, Kazuki; Minakuchi, Hiroyoshi; Mriziq, Khaled; Farkas, Tivadar; Fiehn, Oliver; Tanaka, Nobuo

    2015-02-27

    Prototype small-size (1.0mm I.D., 5cm long) columns for reversed-phase HPLC were evaluated in relation to instrument requirements. The performance of three types of columns, monolithic silica and particulate silica (2μm, totally porous and 2.6μm, core-shell particles) was studied in the presence of considerable or minimal extra-column effects, while the detector contribution to band broadening was minimized by employing a small size UV-detector cell (6- or 90nL). A micro-LC instrument having small system volume (column band variance of only 0.01-0.02μL(2). The three columns generated about 8500 theoretical plates for solutes with retention factor, k>1-3 (depending on the column), in acetonitrile/water mobile phase (65/35=vol/vol) at 0.05mL/min, with the instrument specified above. The column efficiency was lower by up to 30% than that observed with a 2.1mm I.D. commercial column. The small-size columns also provided 8000-8500 theoretical plates for well retained solutes with a commercial ultrahigh-pressure liquid chromatography (UHPLC) instrument when extra-column contributions were minimized. While a significant extra-column effect was observed for early eluting solutes (kcolumn) with methanol/water (20/80=vol/vol) as weak-wash solvent, the use of methanol/water=50/50 as wash solvent affected the column efficiency for most analytes. The results suggest that the band compression effect by the weak-wash solvent associated with partial-loop injection may provide a practical means to reducing the extra-column effect for small-size columns, while the use of an instrument with minimum extra-column effect is highly desirable. Copyright © 2015 Elsevier B.V. All rights reserved.

  2. Research and Development of Monolithic Active Pixel Sensors for the Detection of the Elementary Particles

    International Nuclear Information System (INIS)

    Li, Y.

    2007-09-01

    In order to develop high spatial resolution and readout speed vertex detectors for the future International Linear Collider (ILC), fast CMOS Monolithic Active Pixel Sensors (MAPS) are studied on this work. Two prototypes of MAPS, MIMOSA 8 and MIMOSA 16, based on the same micro-electronic architecture were developed in CMOS processes with different thickness of epitaxial layer. The size of pixel matrix is 32 x 128: 8 columns of the pixel array are readout directly with analog outputs and the other 24 columns are connected to the column level auto-zero discriminators. The Correlated Double Sampling (CDS) structures are successfully implemented inside pixel and discriminator. The photo diode type pixels with different diode sizes are used in these prototypes. With a 55 Fe X-ray radioactive source, the important parameters, such as Temporal Noise, Fixed Pattern Noise (FPN), Signal-to-Noise Ratio (SNR), Charge-to-Voltage conversion Factor (CVF) and Charge Collection Efficiency (CCE), are studied as function of readout speed and diode size. For MIMOSA 8, the effect of fast neutrons irradiation is also. Two beam tests campaigns were made: at DESY with a 5 GeV electrons beam and at CERN with a 180 GeV pions beam. Detection Efficiency and Spatial Resolution are studied in function of the discriminator threshold. For these two parameters, the influences of diode size and SNR of the central pixel of a cluster are also discussed. In order to improve the spatial resolution of the digital outputs, a very compact (25 μm x 1 mm) and low consumption (300 μW) column level ADC is designed in AMS 0.35 μm OPTO process. Based on successive approximation architecture, the auto-offset cancellation structure is integrated. A new column level auto-zero discriminator using static latch is also designed. (author)

  3. Chromatographic Monoliths for High-Throughput Immunoaffinity Isolation of Transferrin from Human Plasma

    Directory of Open Access Journals (Sweden)

    Irena Trbojević-Akmačić

    2016-06-01

    Full Text Available Changes in protein glycosylation are related to different diseases and have a potential as diagnostic and prognostic disease biomarkers. Transferrin (Tf glycosylation changes are common marker for congenital disorders of glycosylation. However, biological interindividual variability of Tf N-glycosylation and genes involved in glycosylation regulation are not known. Therefore, high-throughput Tf isolation method and large scale glycosylation studies are needed in order to address these questions. Due to their unique chromatographic properties, the use of chromatographic monoliths enables very fast analysis cycle, thus significantly increasing sample preparation throughput. Here, we are describing characterization of novel immunoaffinity-based monolithic columns in a 96-well plate format for specific high-throughput purification of human Tf from blood plasma. We optimized the isolation and glycan preparation procedure for subsequent ultra performance liquid chromatography (UPLC analysis of Tf N-glycosylation and managed to increase the sensitivity for approximately three times compared to initial experimental conditions, with very good reproducibility. This work is licensed under a Creative Commons Attribution 4.0 International License.

  4. Influence of different carbon monolith preparation parameters on pesticide adsorption

    Directory of Open Access Journals (Sweden)

    Vukčević Marija

    2013-01-01

    Full Text Available The capacity of carbon monolith for pesticide removal from water, and the mechanism of pesticide interaction with carbon surface were examined. Different carbon monolith samples were obtained by varying the carbonization and activation parameters. In order to examine the role of surface oxygen groups in pesticide adsorption, carbon monolith surface was functionalized by chemical treatment in HNO3, H2O2 and KOH. The surface properties of the obtained samples were investigated by BET surface area, pore size distribution and temperature-programmed desorption. Adsorption of pesticides from aqueous solution onto activated carbon monolith samples was studied by using five pesticides belonging to different chemical groups (acetamiprid, dimethoate, nicosulfuron, carbofuran and atrazine. Presented results show that higher temperature of carbonization and the amount of activating agent allow obtaining microporous carbon monolith with higher amount of surface functional groups. Adsorption properties of the activated carbon monolith were more readily affected by the amount of the surface functional groups than by specific surface area. Results obtained by carbon monolith functionalisation showed that π-π interactions were the main force for adsorption of pesticides with aromatic structure, while acidic groups play an important role in adsorption of pesticides with no aromatic ring in the chemical structure.

  5. Biomimetic small peptide functionalized affinity monoliths for monoclonal antibody purification.

    Science.gov (United States)

    Wang, Xiangyu; Xia, Donghai; Han, Hai; Peng, Kun; Zhu, Peijie; Crommen, Jacques; Wang, Qiqin; Jiang, Zhengjin

    2018-08-09

    The rapid development of monoclonal antibodies (mAbs) in therapeutic and diagnostic applications has necessitated the advancement of mAbs purification technologies. In this study, a biomimetic small peptide ligand 3,5-di-tert-butyl-4-hydroxybenzoic acid-Arg-Arg-Gly (DAAG) functionalized monolith was fabricated through a metal ion chelation-based multi-step approach. The resulting monolith showed good chromatographic performance. Compared with the Ni 2+ based IMAC monolith, the DAAG functionalized monolith exhibited not only excellent specificity but also higher dynamic binding capacity (DBC). The 10% DBC and 50% DBC for hIgG reached as high values as 26.0 and 34.6 mg/mL, respectively, at a ligand density of 8.8 μmol/mL, due to the high porosity and accessibility of the monolithic matrix. Moreover, the stability of the DAAG functionalized monolith in successive breakthrough experiments indicates that it has a promising potential for long-term use in mAbs purification. Finally, the DAAG functionalized monolith was successfully applied to the purification of trastuzumab or human immunoglobulin G (hIgG) from biological samples. Copyright © 2018 Elsevier B.V. All rights reserved.

  6. Column: Every Last Byte

    Directory of Open Access Journals (Sweden)

    Simson Garfinkel

    2011-06-01

    Full Text Available Inheritance powder is the name that was given to poisons, especially arsenic, that were commonly used in the 17th and early 18th centuries to hasten the death of the elderly. For most of the 17th century, arsenic was deadly but undetectable, making it nearly impossible to prove that someone had been poisoned. The first arsenic test produced a gas—hardly something that a scientist could show to a judge. Faced with a growing epidemic of poisonings, doctors and chemists spent decades searching for something better.(see PDF for full column

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

    Science.gov (United States)

    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.

  8. Annular pulse column development studies

    International Nuclear Information System (INIS)

    Benedict, G.E.

    1980-01-01

    The capacity of critically safe cylindrical pulse columns limits the size of nuclear fuel solvent extraction plants because of the limited cross-sectional area of plutonium, U-235, or U-233 processing columns. Thus, there is a need to increase the cross-sectional area of these columns. This can be accomplished through the use of a column having an annular cross section. The preliminary testing of a pilot-plant-scale annular column has been completed and is reported herein. The column is made from 152.4-mm (6-in.) glass pipe sections with an 89-mm (3.5-in.) o.d. internal tube, giving an annular width of 32-mm (1.25-in.). Louver plates are used to swirl the column contents to prevent channeling of the phases. The data from this testing indicate that this approach can successfully provide larger-cross-section critically safe pulse columns. While the capacity is only 70% of that of a cylindrical column of similar cross section, the efficiency is almost identical to that of a cylindrical column. No evidence was seen of any non-uniform pulsing action from one side of the column to the other

  9. 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.

    Science.gov (United States)

    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 clenbuterol determination by HPLC from biological samples.

  10. Purification of papain using reactive green 5 attached supermacroporous monolithic cryogel.

    Science.gov (United States)

    Uygun, Deniz Aktaş; Akduman, Begüm; Uygun, Murat; Akgöl, Sinan; Denizli, Adil

    2012-06-01

    Supermacroporous poly(2-hydroxyethyl methacrylate) [poly(HEMA)] monolithic cryogel was prepared by radical cryocopolymerization of HEMA with N,N'-methylene bisacrylamide as crosslinker. Reactive Green 5 dye was immobilized to the cryogel with nucleophilic substitution reaction, and this dye attached cryogel column was used for affinity purification of papain from Carica papaya latex. Reactive Green 5-immobilized poly(HEMA) cryogel was characterized by swelling studies, Fourier transform infrared spectroscopy, scanning electron microscopy, and energy dispersive X-ray analysis. Maximum papain adsorption capacity was found to be 68.5 mg/g polymer while nonspecific papain adsorption onto plain cryogel was negligible (3.07 mg/g polymer). Papain from C. papaya was purified 42-fold in single step with dye attached cryogel, and purity of papain was shown by silver-stained sodium dodecyl sulfate-polyacrylamide gel electrophoresis.

  11. Monolithic fuel injector and related manufacturing method

    Science.gov (United States)

    Ziminsky, Willy Steve [Greenville, SC; Johnson, Thomas Edward [Greenville, SC; Lacy, Benjamin [Greenville, SC; York, William David [Greenville, SC; Stevenson, Christian Xavier [Greenville, SC

    2012-05-22

    A monolithic fuel injection head for a fuel nozzle includes a substantially hollow vesicle body formed with an upstream end face, a downstream end face and a peripheral wall extending therebetween, an internal baffle plate extending radially outwardly from a downstream end of the bore, terminating short of the peripheral wall, thereby defining upstream and downstream fuel plenums in the vesicle body, in fluid communication by way of a radial gap between the baffle plate and the peripheral wall. A plurality of integral pre-mix tubes extend axially through the upstream and downstream fuel plenums in the vesicle body and through the baffle plate, with at least one fuel injection hole extending between each of the pre-mix tubes and the upstream fuel plenum, thereby enabling fuel in the upstream plenum to be injected into the plurality of pre-mix tubes. The fuel injection head is formed by direct metal laser sintering.

  12. Determining leach rates of monolithic waste forms

    International Nuclear Information System (INIS)

    Gilliam, T.M.; Dole, L.R.

    1986-01-01

    The ANS 16.1 Leach Procedure provides a conservative means of predicting long-term release from monolithic waste forms, offering a simple and relatively quick means of determining effective solid diffusion coefficients. As presented here, these coefficients can be used in a simple model to predict maximum release rates or be used in more complex site-specific models to predict actual site performance. For waste forms that pass the structural integrity test, this model also allows the prediction of EP-Tox leachate concentrations from these coefficients. Thus, the results of the ANS 16.1 Leach Procedure provide a powerful tool that can be used to predict the waste concentration limits in order to comply with the EP-Toxicity criteria for characteristically nonhazardous waste. 12 refs., 3 figs

  13. Present status of the MONOLITH project

    International Nuclear Information System (INIS)

    Petrukhin, A.A.

    2001-01-01

    MONOLITH is a proposed massive (34 kt) magnetized tracking calorimeter at the Gran Sasso laboratory in Italy, optimized for the detection of atmospheric muon neutrinos. The main goal is to establish (or reject) the neutrino oscillation hypothesis through an explicit observation of the full first oscillation swing. The Δm 2 sensitivity range for this measurement comfortably covers the complete Super-Kamiokande allowed region. Other measurements include studies of matter effects, the NC up/down ratio, ν bar / ν ratio, the study of cosmic ray muons in the multi-TeV range, and auxiliary measurements from the CERN to Gran Sasso neutrino beam. Depending on approval, data taking with the part of the detector could start towards the end of 2004

  14. Transparent monolithic metal ion containing nanophase aerogels

    Energy Technology Data Exchange (ETDEWEB)

    Risen, W. M., Jr.; Hu, X.; Ji, S.; Littrell, K.

    1999-12-01

    The formation of monolithic and transparent transition metal containing aerogels has been achieved through cooperative interactions of high molecular weight functionalized carbohydrates and silica precursors, which strongly influence the kinetics of gelation. After initial gelation, subsequent modification of the ligating character of the system, coordination of the group VIII metal ions, and supercritical extraction afford the aerogels. The structures at the nanophase level have been probed by photon and electron transmission and neutron scattering techniques to help elucidate the basis for structural integrity together with the small entity sizes that permit transparency in the visible range. They also help with understanding the chemical reactivities of the metal-containing sites in these very high surface area materials. These results are discussed in connection with new reaction studies.

  15. Two-column sequential injection chromatography for fast isocratic separation of two analytes of greatly differing chemical properties.

    Science.gov (United States)

    Šatínský, Dalibor; Chocholouš, Petr; Válová, Olga; Hanusová, Lucia; Solich, Petr

    2013-09-30

    This paper deals with a novel approach to separate two analytes with different chemical properties and different lipophilicity. The newly described methodology is based on the two column system that was used for isocratic separation of two analytes with very different lipophilicity-dexamethasone and cinchocaine. Simultaneous separation of model compounds cinchocaine and dexamethasone was carried under the following conditions in two-column sequential injection chromatography system (2-C SIC). A 25×4.6 mm C-18 monolithic column was used in the first dimension for retention and separation of dexamethasone with mobile phase acetonitrile:water 30:70 (v/v), flow rate 0.9 mL min(-1) and consumption of 1.7 mL. A 10×4.6 mm C-18 monolithic column with 5×4.6 mm C-18 precolumn was used in the second dimension for retention and separation of cinchocaine using mobile phase acetonitrile:water 60:40 (v/v), flow rate 0.9 mL min(-1) and consumption 1.5 mL. Whole analysis time including both mobile phase's aspirations and both column separations was performed in less than 4 min. The method was fully validated and used for determination of cinchocaine and dexamethasone in pharmaceutical otic drops. The developed 2-C SIC method was compared with HPLC method under the isocratic conditions of separation on monolithic column (25×4.6 mm C-18). Spectrophotometric detection of both compounds was performed at wavelength 240 nm. System repeatability and method precision were found in the range (0.39-3.12%) for both compounds. Linearity of determination was evaluated in the range 50-500 μg mL(-1) and coefficients of determination were found to be r(2)=0.99912 for dexamethasone and r(2)=0.99969 for cinchocaine. Copyright © 2013 Elsevier B.V. All rights reserved.

  16. Column-to-column packing variation of disposable pre-packed columns for protein chromatography.

    Science.gov (United States)

    Schweiger, Susanne; Hinterberger, Stephan; Jungbauer, Alois

    2017-12-08

    In the biopharmaceutical industry, pre-packed columns are the standard for process development, but they must be qualified before use in experimental studies to confirm the required performance of the packed bed. Column qualification is commonly done by pulse response experiments and depends highly on the experimental testing conditions. Additionally, the peak analysis method, the variation in the 3D packing structure of the bed, and the measurement precision of the workstation influence the outcome of qualification runs. While a full body of literature on these factors is available for HPLC columns, no comparable studies exist for preparative columns for protein chromatography. We quantified the influence of these parameters for commercially available pre-packed and self-packed columns of disposable and non-disposable design. Pulse response experiments were performed on 105 preparative chromatography columns with volumes of 0.2-20ml. The analyte acetone was studied at six different superficial velocities (30, 60, 100, 150, 250 and 500cm/h). The column-to-column packing variation between disposable pre-packed columns of different diameter-length combinations varied by 10-15%, which was acceptable for the intended use. The column-to-column variation cannot be explained by the packing density, but is interpreted as a difference in particle arrangement in the column. Since it was possible to determine differences in the column-to-column performance, we concluded that the columns were well-packed. The measurement precision of the chromatography workstation was independent of the column volume and was in a range of±0.01ml for the first peak moment and±0.007 ml 2 for the second moment. The measurement precision must be considered for small columns in the range of 2ml or less. The efficiency of disposable pre-packed columns was equal or better than that of self-packed columns. Copyright © 2017 The Author(s). Published by Elsevier B.V. All rights reserved.

  17. Monolithic Rare Earth Doped PTR Glass Laser, Phase II

    Data.gov (United States)

    National Aeronautics and Space Administration — The main goal of the project is to demonstrate the feasibility of a monolithic solid state laser on the basis of PTR glass co-doped with luminescent rare earth ions....

  18. Packaged, cascadable wideband monolithic feedback amplifiers for radar systems applications

    OpenAIRE

    Alleva, V.; Calori, M.; Cetronio, A.; Lanzieri, C.; Proietti, C.; Rapisarda, S.

    1990-01-01

    Design criteria and fabrication of a packaged, monolithic, cascadable, feedback amplifier are presented. The good performances in term of bandwidth, gain, flatness, reproducibility and reliability makes this component highly suitable for many radar applications.

  19. Reliability Analysis and Optimal Design of Monolithic Vertical Wall Breakwaters

    DEFF Research Database (Denmark)

    Sørensen, John Dalsgaard; Burcharth, Hans F.; Christiani, E.

    1994-01-01

    Reliability analysis and reliability-based design of monolithic vertical wall breakwaters are considered. Probabilistic models of the most important failure modes, sliding failure, failure of the foundation and overturning failure are described . Relevant design variables are identified and relia...

  20. Plant oil-based shape memory polymer using acrylic monolith

    Directory of Open Access Journals (Sweden)

    T. Tsujimoto

    2015-09-01

    Full Text Available This article deals with the synthesis of a plant oil-based material using acrylic monolith. An acrylic monolith bearing oxirane groups was prepared via simple technique that involved the dissolution of poly(glycidyl methacrylate-comethyl methacrylate (PGMA in ethanolic – aqueous solution by heating and subsequent cooling. The PGMA monolith had topologically porous structure, which was attributed to the phase separation of the polymer solution. The PGMA monolith was impregnated by epoxidized soybean oil (ESO containing thermally-latent catalyst, and the subsequent curing produced a crosslinked material with relatively good transparency. The Young’s modulus and the tensile strength of polyESO/PGMA increased compared with the ESO homopolymer. The strain at break of polyESO/PGMA was larger than that of the ESO homopolymer and crosslinked PGMA. Furthermore, polyESO/PGMA exhibited good shape memory-recovery behavior.

  1. Application of monolithic chromatographic supports in virus research.

    Science.gov (United States)

    Krajacic, Mladen; Ravnikar, Maja; Štrancar, Aleš; Gutiérrez-Aguirre, Ion

    2017-11-01

    Key properties of monolithic chromatographic supports, make them suitable for separation and/or concentration of large biomolecules, especially virus particles and viral genomes. One by one, the studies that have been completed so far, contributed to the knowledge that monolith chromatography has hardly any limitation to be applied in virus research. Viruses of different sizes, possessing icosahedral structure and symmetrical morphology, as well as rod-shaped or filamentous viruses with helical structure, even enveloped ones, all of them could be successfully managed by means of monolith chromatography. Same is true for viral genomes, primarily when being distinct from other nucleic acid forms present in a host cell. This review is exclusively focused on viruses. It describes the application of monolith chromatography to different problematics within the virus research field. The reviewed achievements offer new possibilities and trigger new aspects in virology. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. Effect of accelerated aging on translucency of monolithic zirconia

    Directory of Open Access Journals (Sweden)

    O. Abdelbary

    2016-12-01

    Conclusion: Thickness of zirconia has significant effect on translucency. Aging has significant effect on thinner sections of zirconia. More research is required on zirconia towards making the material more translucent for its potential use as esthetic monolithic restoration.

  3. Monolithic Perovskite Silicon Tandem Solar Cells with Advanced Optics

    Energy Technology Data Exchange (ETDEWEB)

    Goldschmidt, Jan C.; Bett, Alexander J.; Bivour, Martin; Blasi, Benedikt; Eisenlohr, Johannes; Kohlstadt, Markus; Lee, Seunghun; Mastroianni, Simone; Mundt, Laura; Mundus, Markus; Ndione, Paul; Reichel, Christian; Schubert, Martin; Schulze, Patricia S.; Tucher, Nico; Veit, Clemens; Veurman, Welmoed; Wienands, Karl; Winkler, Kristina; Wurfel, Uli; Glunz, Stefan W.; Hermle, Martin

    2016-11-14

    For high efficiency monolithic perovskite silicon tandem solar cells, we develop low-temperature processes for the perovskite top cell, rear-side light trapping, optimized perovskite growth, transparent contacts and adapted characterization methods.

  4. Exploring the effect of mesopore size reduction on the column performance of silica-based open tubular capillary columns.

    Science.gov (United States)

    Hara, Takeshi; Futagami, Shunta; De Malsche, Wim; Baron, Gino V; Desmet, Gert

    2018-06-01

    We report on a modification in the hydrothermal treatment process of monolithic silica layers used in porous-layered open tubular (PLOT) columns. Lowering the temperature from the customary 95 °C to 80 °C, the size of the mesopores reduced by approximately about 35% from 12-13.5 nm to 7.5-9 nm, while the specific pore volume essentially remains unaltered. This led to an increase of the specific surface area (SA) of about 40%, quasi-independent of the porous layer thickness. The increased surface area provided a corresponding increase in retention, somewhat more (48%) than expected based on the increase in SA for the thin layer columns, and somewhat less than expected (34%) for the thick layer columns. The recipes were applied in 5 μm i.d.-capillaries with a length of 60 cm. Efficiencies under retained conditions amounted up to N = 137,000 for the PLOT column with a layer thickness (d f ) of 300 nm and to N = 109,000 for the PLOT column with d f  = 550 nm. Working under conditions of similar retention, the narrow pore/high SA columns produced with the new 80 °C recipe generated the same number of theoretical plates as the wide pore size/low SA columns produced with the 95 °C recipe. This shows the 80 °C-hydrothermal treatment process allows for an increase in the phase ratio of the PLOT columns without affecting their intrinsic mass transfer properties and separation kinetics. This is further corroborated by the fact that the plate height curves generated with the new and former recipe can both be well-fitted with the Golay-Aris equation without having to change the intra-layer diffusion coefficient. Copyright © 2018 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

    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

  6. Column: File Cabinet Forensics

    Directory of Open Access Journals (Sweden)

    Simson Garfinkel

    2011-12-01

    Full Text Available Researchers can spend their time reverse engineering, performing reverse analysis, or making substantive contributions to digital forensics science. Although work in all of these areas is important, it is the scientific breakthroughs that are the most critical for addressing the challenges that we face.Reverse Engineering is the traditional bread-and-butter of digital forensics research. Companies like Microsoft and Apple deliver computational artifacts (operating systems, applications and phones to the commercial market. These artifacts are bought and used by billions. Some have evil intent, and (if society is lucky, the computers end up in the hands of law enforcement. Unfortunately the original vendors rarely provide digital forensics tools that make their systems amenable to analysis by law enforcement. Hence the need for reverse engineering.(see PDF for full column

  7. Sol-Gel Synthesis of Non-Silica Monolithic Materials

    Science.gov (United States)

    Gaweł, Bartłomiej; Gaweł, Kamila; Øye, Gisle

    2010-01-01

    Monolithic materials have become very popular because of various applications, especially within chromatography and catalysis. Large surface areas and multimodal porosities are great advantages for these applications. New sol-gel preparation methods utilizing phase separation or nanocasting have opened the possibility for preparing materials of other oxides than silica. In this review, we present different synthesis methods for inorganic, non-silica monolithic materials. Some examples of application of the materials are also included.

  8. Evaluation of translucency of monolithic zirconia and framework zirconia materials

    OpenAIRE

    Tuncel, ?lkin; Turp, I??l; ???mez, Asl?han

    2016-01-01

    PURPOSE The opacity of zirconia is an esthetic disadvantage that hinders achieving natural and shade-matched restorations. The aim of this study was to evaluate the translucency of non-colored and colored framework zirconia and monolithic zirconia. MATERIALS AND METHODS The three groups tested were: non-colored framework zirconia, colored framework zirconia with the A3 shade according to Vita Classic Scale, and monolithic zirconia (n=5). The specimens were fabricated in the dimensions of 15?1...

  9. Extended Leach Testing of Simulated LAW Cast Stone Monoliths

    Energy Technology Data Exchange (ETDEWEB)

    Serne, R. Jeffrey [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Westsik, Joseph H. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Williams, Benjamin D. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Jung, H. B. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Wang, Guohui [Pacific Northwest National Lab. (PNNL), Richland, WA (United States)

    2015-07-09

    This report describes the results from long-term laboratory leach tests performed at Pacific Northwest National Laboratory (PNNL) for Washington River Protection Solutions (WRPS) to evaluate the release of key constituents from monoliths of Cast Stone prepared with four simulated low-activity waste (LAW) liquid waste streams. Specific objectives of the Cast Stone long-term leach tests described in this report focused on four activities: 1. Extending the leaching times for selected ongoing EPA-1315 tests on monoliths made with LAW simulants beyond the conventional 63-day time period up to 609 days reported herein (with some tests continuing that will be documented later) in an effort to evaluate long-term leaching properties of Cast Stone to support future performance assessment activities. 2. Starting new EPA-1315 leach tests on archived Cast Stone monoliths made with four LAW simulants using two leachants (deionized water [DIW] and simulated Hanford Integrated Disposal Facility (IDF) Site vadose zone pore water [VZP]). 3. Evaluating the impacts of varying the iodide loading (starting iodide concentrations) in one LAW simulant (7.8 M Na Hanford Tank Waste Operations Simulator (HTWOS) Average) by manufacturing new Cast Stone monoliths and repeating the EPA-1315 leach tests using DIW and the VZP leachants. 4. Evaluating the impacts of using a non-pertechnetate form of Tc that is present in some Hanford tanks. In this activity one LAW simulant (7.8 M Na HTWOS Average) was spiked with a Tc(I)-tricarbonyl gluconate species and then solidified into Cast Stone monoliths. Cured monoliths were leached using the EPA-1315 leach protocol with DIW and VZP. The leach results for the Tc-Gluconate Cast Stone monoliths were compared to Cast Stone monoliths pertechnetate.

  10. Performance characteristics between monolithic and microservice-based systems

    OpenAIRE

    Flygare, Robin; Holmqvist, Anthon

    2017-01-01

    A new promising technology to face the problem of scalability and availability is the microservice architecture. The problem with this architecture is that there is no significant study that clearly proves the performance differences compared to the monolithic architecture. Our thesis aims to provide a more conclusive answer of how the microservice architecture differs performance wise compared to the monolithic architecture. In this study, we conducted several experiments on a self-developed...

  11. Towards a Technique for Extracting Microservices from Monolithic Enterprise Systems

    OpenAIRE

    Levcovitz, Alessandra; Terra, Ricardo; Valente, Marco Tulio

    2016-01-01

    The idea behind microservices architecture is to develop a single large, complex application as a suite of small, cohesive, independent services. On the other way, monolithic systems get larger over the time, deviating from the intended architecture, and becoming risky and expensive to evolve. This paper describes a technique to identify and define microservices on monolithic enterprise systems. As the major contribution, our evaluation shows that our approach was able to identify relevant ca...

  12. 100% reflectivity from a monolithic dielectric microstructured surface

    OpenAIRE

    Brückner, F.; Clausnitzer, T.; Burmeister, O.; Friedrich, D.; Kley, E.; Danzmann, K.; Tünnermann, A.; Schnabel, R.

    2008-01-01

    Here, we propose a new mirror architecture which is solely based upon a monolithic dielectric micro-structured surface. Hence, the mirror device, which consists of a possibly mono-crystalline bulk material, can in principle simultaneously provide perfect reflectivity and lowest mechanical loss. By specifically structuring the monolithic surface, resulting in T-shaped ridges of a subwavelength grating, a resonant behavior of light coupling can be realized, leading to theoretically 100% reflect...

  13. Sol-Gel Synthesis of Non-Silica Monolithic Materials

    Directory of Open Access Journals (Sweden)

    Bartłomiej Gaweł

    2010-04-01

    Full Text Available Monolithic materials have become very popular because of various applications, especially within chromatography and catalysis. Large surface areas and multimodal porosities are great advantages for these applications. New sol-gel preparation methods utilizing phase separation or nanocasting have opened the possibility for preparing materials of other oxides than silica. In this review, we present different synthesis methods for inorganic, non-silica monolithic materials. Some examples of application of the materials are also included.

  14. Sol-Gel Synthesis of Non-Silica Monolithic Materials

    OpenAIRE

    Gawe?, Bart?omiej; Gawe?, Kamila; ?ye, Gisle

    2010-01-01

    Monolithic materials have become very popular because of various applications, especially within chromatography and catalysis. Large surface areas and multimodal porosities are great advantages for these applications. New sol-gel preparation methods utilizing phase separation or nanocasting have opened the possibility for preparing materials of other oxides than silica. In this review, we present different synthesis methods for inorganic, non-silica monolithic materials. Some examples of appl...

  15. Buckling of a holey column.

    Science.gov (United States)

    Pihler-Puzović, D; Hazel, A L; Mullin, T

    2016-09-14

    We report the results from a combined experimental and numerical investigation of buckling in a novel variant of an elastic column under axial load. We find that including a regular line of centred holes in the column can prevent conventional, global, lateral buckling. Instead, the local microstructure introduced by the holes allows the column to buckle in an entirely different, internal, mode in which the holes are compressed in alternate directions, but the column maintains the lateral reflection symmetry about its centreline. The internal buckling mode can be accommodated within a smaller external space than the global one; and it is the preferred buckling mode over an intermediate range of column lengths for sufficiently large holes. For very short or sufficiently long columns a modification of the classical, global, lateral buckling is dominant.

  16. Sequence-specific DNA solid-phase extraction in an on-chip monolith: Towards detection of antibiotic resistance genes.

    Science.gov (United States)

    Knob, Radim; Nelson, Daniel B; Robison, Richard A; Woolley, Adam T

    2017-11-10

    Antibiotic resistance of bacteria is a growing problem and presents a challenge for prompt treatment in patients with sepsis. Currently used methods rely on culturing or amplification; however, these steps are either time consuming or suffer from interference issues. A microfluidic device was made from black polypropylene, with a monolithic column modified with a capture oligonucleotide for sequence selective solid-phase extraction of a complementary target from a lysate sample. Porous properties of the monolith allow flow and hybridization of a target complementary to the probe immobilized on the column surface. Good flow-through properties enable extraction of a 100μL sample and elution of target DNA in 12min total time. Using a fluorescently labeled target oligonucleotide related to Verona Integron-Mediated Metallo-β-lactamase it was possible to extract and detect a 1pM sample with 83% recovery. Temperature-mediated elution by heating above the duplex melting point provides a clean extract without any agents that interfere with base pairing, allowing various labeling methods or further downstream processing of the eluent. Further integration of this extraction module with a system for isolation and lysis of bacteria from blood, as well as combining with single-molecule detection should allow rapid determination of antibiotic resistance. Copyright © 2017 Elsevier B.V. All rights reserved.

  17. Application and optimization of organic-inorganic hybrid monolithic capillary electrochromatography for in vivo cefdinir determination with microdialysis.

    Science.gov (United States)

    Chen, Zhao; Bi, Xiaoli; Li, Ji; Tang, Yuanjun; Fan, Guorong; Sun, Dongmei

    2016-01-01

    In this study, an organic-inorganic hybrid monolithic capillary column was applied and optimized for the determination of cefdinir in plasma, and the electro-osmotic flow that usually hinders migration in reverse polarity became a driving force. The Sample used for pharmacokinetic research was collected by microdialysis using phosphate buffer (pH 7.4) as perfusate, and a volume of 60 μL fluid was mixed with 140 μL of acetonitrile. By using a silica-allyldimethyldodecylammonium monolithic column (100 μm inner diameter, 21 cm effective length and 31.2 cm total length), and a mobile phase consisting of phosphate and acetonitrile (pH 4.5, 50:50, v/v), at a voltage of 20 kV, the analytes were successfully separated with the background within 2.5 min. The detection wavelength was 214 nm. The calibration curve showed a good linearity (r(2) = 0.9994) over the concentration range of 0.2-50 μg/mL. The proposed method showed good specificity, linearity, sensitivity, precision and recovery, and the introduction of field amplified sample stacking helped to improve the low recovery caused by microdialysis. This method was successfully applied to quantify cefdinir in rat plasma to support a pre-clinical pharmacokinetic trial. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Cortical columns for quick brains

    OpenAIRE

    Stoop, Ralph L.; Saase, Victor; Wagner, Clemens; Stoop, Britta; Stoop, Ruedi

    2012-01-01

    It is widely believed that the particular wiring observed within cortical columns boosts neural computation. We use rewiring of neural networks performing real-world cognitive tasks to study the validity of this argument. In a vast survey of wirings within the column we detect, however, no traces of the proposed effect. It is on the mesoscopic inter-columnar scale that the existence of columns - largely irrespective of their inner organization - enhances the speed of information transfer and ...

  19. Nano-Doped Monolithic Materials for Molecular Separation

    Directory of Open Access Journals (Sweden)

    Caleb Acquah

    2017-01-01

    Full Text Available Monoliths are continuous adsorbents that can easily be synthesised to possess tuneable meso-/macropores, convective fluid transport, and a plethora of chemistries for ligand immobilisation. They are grouped into three main classes: organic, inorganic, and hybrid, based on their chemical composition. These classes may also be differentiated by their unique morphological and physicochemical properties which are significantly relevant to their specific separation applications. The potential applications of monoliths for molecular separation have created the need to enhance their characteristic properties including mechanical strength, electrical conductivity, and chemical and thermal stability. An effective approach towards monolith enhancement has been the doping and/or hybridization with miniaturized molecular species of desirable functionalities and characteristics. Nanoparticles are usually preferred as dopants due to their high solid phase dispersion features which are associated with improved intermolecular adsorptive interactions. Examples of such nanomaterials include, but are not limited to, carbon-based, silica-based, gold-based, and alumina nanoparticles. The incorporation of these nanoparticles into monoliths via in situ polymerisation and/or post-modification enhances surface adsorption for activation and ligand immobilisation. Herein, insights into the performance enhancement of monoliths as chromatographic supports by nanoparticles doping are presented. In addition, the potential and characteristics of less common nanoparticle materials such as hydroxyapatite, ceria, hafnia, and germania are discussed. The advantages and challenges of nanoparticle doping of monoliths are also discussed.

  20. Rapid identification of synthetic colorants in food samples by using indium oxide nanoparticle-functionalized porous polymer monolith coupled with HPLC-MS/MS.

    Science.gov (United States)

    Qi, Ruifang; Zhou, Xiao; Li, Xiqian; Ma, Jiutong; Lu, Chunmei; Mu, Jun; Zhang, Xuguang; Jia, Qiong

    2014-12-07

    A synthetic protocol for the preparation of an indium oxide nanoparticle-functionalized poly(methacrylic acid-glycidyl methacrylate-ethylene dimethacrylate-ethanediamine) monolithic column is reported. Various techniques, including scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, and thermal gravimetric analysis-derivative thermogravimetric analysis were employed to characterize the synthesized monolith. The modified monolithic column was coupled with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) for determining synthetic colorants in various food samples. Under optimized conditions, good linearity was obtained for all the targets with squared regression coefficients greater than 0.9982. The limits of detection (S/N = 3) for 12 synthetic colorants were in the range of 0.012-2.97 μg kg(-1). The intra-day and inter-day relative standard deviations, ranging from 2.7% to 8.5%, were within the acceptable range. The developed method was successfully applied to the determination of synthetic colorants in food samples (candy, milk, jelly, jam, canned food, juice, and carbonated drink). Target recoveries at different spiked levels ranged from 73.5% to 112.1% with relative standard deviations of less than 10.3%.

  1. Preparation and characterization of hydrophilic hybrid monoliths via thiol-ene click polymerization and their applications in chromatographic analysis and glycopeptides enrichment.

    Science.gov (United States)

    Bai, Jingyao; Liu, Zhongshan; Wang, Hongwei; You, Xin; Ou, Junjie; Shen, Yehua; Ye, Mingliang

    2017-05-19

    A macroporous hydrophilic organic-silica hybrid monolithic column was synthesized via photoinitiated thiol-ene click polymerization reaction of 1-thioglycerol-modified polyhedral oligomeric vinylsilsesquioxane (vinylPOSS) and dithiothreitol (DTT) in a binary porogenic system consisting of tetrahydrofuran (THF) and dodecanol. 1-Thioglycerol was used to modify vinylPOSS in order to form a precursor with good solubility in the binary porogenic system. The influences of both the ratio of 1-thioglycerol/vinylPOSS and the porogenic solvents on the morphology and permeability of hybrid monoliths were studied in detail. The physical properties of hybrid monolith were characterized by scanning electron microscopy (SEM), Fourier transform infrared (FT-IR) spectroscopy and nitrogen adsorption/desorption measurement. The chromatographic performance was evaluated by separation of neutral polar compounds in capillary liquid chromatography (cLC). The resulting column possessed homogeneous macroporous structure and showed hydrophilic interaction liquid chromatography (HILIC) separation mechanism with high efficiency of 65,000Nm -1 for formamide. Ultimately, the hybrid matrix was grafted with hydrazine groups and then exhibited the ability of glycopeptides enrichment. Copyright © 2016 Elsevier B.V. All rights reserved.

  2. Monoliths: A Review of the Basics, Preparation Methods and Their Relevance to Oxidation

    Directory of Open Access Journals (Sweden)

    Sandeeran Govender

    2017-02-01

    Full Text Available Considerable research has been conducted on monolithic catalysts for various applications. Strategies toward coating monoliths are of equal interest and importance. In this paper, the preparation of monoliths and monolithic catalysts have been summarized. More specifically, a brief explanation for the manufacturing of ceramic and metallic monoliths has been provided. Also, different methods for coating γ-alumina, as a secondary support, are included. Techniques used to deposit metal-based species, zeolites and carbon onto monoliths are discussed. Furthermore, monoliths extruded with metal oxides, zeolites and carbon are described. The main foci are on the reasoning and understanding behind the preparation of monolithic catalysts. Ideas and concerns are also contributed to encourage better approaches when designing these catalysts. More importantly, the relevance of monolithic structures to reactions, such as the selective oxidation of alkanes, catalytic combustion for power generation and the preferential oxidation of carbon monoxide, has been described.

  3. Biasable, Balanced, Fundamental Submillimeter Monolithic Membrane Mixer

    Science.gov (United States)

    Siegel, Peter; Schlecht, Erich; Mehdi, Imran; Gill, John; Velebir, James; Tsang, Raymond; Dengler, Robert; Lin, Robert

    2010-01-01

    This device is a biasable, submillimeter-wave, balanced mixer fabricated using JPL s monolithic membrane process a simplified version of planar membrane technology. The primary target application is instrumentation used for analysis of atmospheric constituents, pressure, temperature, winds, and other physical and chemical properties of the atmospheres of planets and comets. Other applications include high-sensitivity gas detection and analysis. This innovation uses a balanced configuration of two diodes allowing the radio frequency (RF) signal and local oscillator (LO) inputs to be separated. This removes the need for external diplexers that are inherently narrowband, bulky, and require mechanical tuning to change frequency. Additionally, this mixer uses DC bias-ability to improve its performance and versatility. In order to solve problems relating to circuit size, the GaAs membrane process was created. As much of the circuitry as possible is fabricated on-chip, making the circuit monolithic. The remainder of the circuitry is precision-machined into a waveguide block that holds the GaAs circuit. The most critical alignments are performed using micron-scale semiconductor technology, enabling wide bandwidth and high operating frequencies. The balanced mixer gets superior performance with less than 2 mW of LO power. This can be provided by a simple two-stage multiplier chain following an amplifier at around 90 GHz. Further, the diodes are arranged so that they can be biased. Biasing pushes the diodes closer to their switching voltage, so that less LO power is required to switch the diodes on and off. In the photo, the diodes are at the right end of the circuit. The LO comes from the waveguide at the right into a reduced-height section containing the diodes. Because the diodes are in series to the LO signal, they are both turned on and off simultaneously once per LO cycle. Conversely, the RF signal is picked up from the RF waveguide by the probe at the left, and flows

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

    Science.gov (United States)

    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.

  5. Experimental analysis of reinforced concrete columns strengthened with self-compacting concrete and connectors

    Directory of Open Access Journals (Sweden)

    P. P. Nascimento

    Full Text Available There are many problems involving cases of destruction of buildings and other structures. The columns can deteriorate for several reasons such as the evolution and changing habits of the loads. The experimental phase of this work was based on a test involving nine reinforced concrete columns under combined bending and axial compression, at an initial eccentricity of 60 mm. Two columns were used as reference, one having the original dimensions of the column and the other, monolithic, had been cast along the thickness of the strengthened piece. The remaining columns received a 35 mm thick layer of self-compacting concrete on their compressed face. For the preparation of the interface between the two materials, this surface was scarified and furrowed and connectors were inserted onto the columns' shear reinforcement in various positions and amounts.As connectors, 5 mm diameter steel bars were used (the same as for stirrups, bent in the shape of a "C" with 25 mm coatings. >As a conclusion, not only the quantity, but mainly, the location of the connectors used in the link between substrate and reinforcement is crucial to increase strength and to change failure mode.

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

    Directory of Open Access Journals (Sweden)

    Filatov Valery

    2018-01-01

    Full Text Available 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.

  7. Solid oxide fuel cell with monolithic core

    Science.gov (United States)

    McPheeters, C.C.; Mrazek, F.C.

    1988-08-02

    A solid oxide fuel cell in which fuel and oxidant gases undergo an electrochemical reaction to produce an electrical output includes a monolithic core comprised of a corrugated conductive sheet disposed between upper and lower generally flat sheets. The corrugated sheet includes a plurality of spaced, parallel, elongated slots which form a series of closed, linear, first upper and second lower gas flow channels with the upper and lower sheets within which a fuel gas and an oxidant gas respectively flow. Facing ends of the fuel cell are generally V-shaped and provide for fuel and oxidant gas inlet and outlet flow, respectively, and include inlet and outlet gas flow channels which are continuous with the aforementioned upper fuel gas and lower oxidant gas flow channels. The upper and lower flat sheets and the intermediate corrugated sheet are preferably comprised of ceramic materials and are securely coupled together such as by assembly in the green state and sintering together during firing at high temperatures. A potential difference across the fuel cell, or across a stacked array of similar fuel cells, is generated when an oxidant gas such as air and a fuel such as hydrogen gas is directed through the fuel cell at high temperatures, e.g., between 700 C and 1,100 C. 8 figs.

  8. Properties of glass-bonded zeolite monoliths

    International Nuclear Information System (INIS)

    Lewis, M.A.; Fischer, D.F.; Murphy, C.D.

    1994-01-01

    It has been shown that mineral waste forms can be used to immobilize waste salt generated during the pyrochemical processing of spent fuel from the Integral Fast Reactor (IFR). Solid, leach resistant monoliths were formed by hot-pressing mixtures of salt-occluded zeolite A powders and glass frit at 990 K and 28 MPa. Additional samples have now been fabricated and tested. Normalized release rates for all elements, including iodide and chloride, were less than 1 g/m 2 d in 28-day tests in deionized water and in brine at 363 K (90 degrees C). Preliminary results indicate that these rates fall with time with both leachants and that the zeolite phase in the glass-bonded zeolite does not function as an ion exchanger. Some material properties were measured. The Poisson ratio and Young's modulus were slightly smaller in glass-bonded zeolite than in borosilicate glass. Density depended on zeolite fraction. The glass-bonded zeolite represents a promising mineral waste form for IFR salt

  9. Characterisation of methacrylate monoliths for bacteriophage purification.

    Science.gov (United States)

    Smrekar, Franc; Ciringer, Mateja; Strancar, Aleš; Podgornik, Aleš

    2011-04-29

    Binding of three different bacteriophages (phages), namely T7, lambda and M13 on methacrylate monoliths was investigated. Phage M13 exhibited the highest dynamic binding capacity of 4.5×10(13) pfu/mL while T7 and lambda showed capacity of 1×10(13) pfu/mL, all corresponding to values of around 1mg/mL. Interestingly, capacity for lambda phage was increased 5-fold by increasing NaCl concentration in a loaded sample from 0 to 0.2M while there was a constant capacity decrease for T7 and M13 phages. Under optimal conditions, recovery for all three phages approached 100%. Measurement of a pressure drop increase during loading enabled estimation of adsorbed phage layer thickness. At a maximal capacity it was calculated to be around 50 nm for T7 phage and 60 nm for lambda phage matching closely capside size thus indicating monolayer adsorption while 80 nm layer thickness was estimated for M13 phage showing its orientation along the pore. Copyright © 2010 Elsevier B.V. All rights reserved.

  10. Mush Column Magma Chambers

    Science.gov (United States)

    Marsh, B. D.

    2002-12-01

    Magma chambers are a necessary concept in understanding the chemical and physical evolution of magma. The concept may well be similar to a transfer function in circuit or time series analysis. It does what needs to be done to transform source magma into eruptible magma. In gravity and geodetic interpretations the causative body is (usually of necessity) geometrically simple and of limited vertical extent; it is clearly difficult to `see' through the uppermost manifestation of the concentrated magma. The presence of plutons in the upper crust has reinforced the view that magma chambers are large pots of magma, but as in the physical representation of a transfer function, actual magma chambers are clearly distinct from virtual magma chambers. Two key features to understanding magmatic systems are that they are vertically integrated over large distances (e.g., 30-100 km), and that all local magmatic processes are controlled by solidification fronts. Heat transfer considerations show that any viable volcanic system must be supported by a vertically extensive plumbing system. Field and geophysical studies point to a common theme of an interconnected stack of sill-like structures extending to great depth. This is a magmatic Mush Column. The large-scale (10s of km) structure resembles the vertical structure inferred at large volcanic centers like Hawaii (e.g., Ryan et al.), and the fine scale (10s to 100s of m) structure is exemplified by ophiolites and deeply eroded sill complexes like the Ferrar dolerites of the McMurdo Dry Valleys, Antarctica. The local length scales of the sill reservoirs and interconnecting conduits produce a rich spectrum of crystallization environments with distinct solidification time scales. Extensive horizontal and vertical mushy walls provide conditions conducive to specific processes of differentiation from solidification front instability to sidewall porous flow and wall rock slumping. The size, strength, and time series of eruptive behavior

  11. C₁₈-bound porous silica monolith particles as a low-cost high-performance liquid chromatography stationary phase with an excellent chromatographic performance.

    Science.gov (United States)

    Ali, Faiz; Cheong, Won Jo

    2014-12-01

    Ground porous silica monolith particles with an average particle size of 2.34 μm and large pores (363 Å) exhibiting excellent chromatographic performance have been synthesized on a relatively large scale by a sophisticated sol-gel procedure. The particle size distribution was rather broad, and the d(0.1)/d(0.9) ratio was 0.14. The resultant silica monolith particles were chemically modified with chlorodimethyloctadecylsilane and end-capped with a mixture of hexamethyldisilazane and chlorotrimethylsilane. Very good separation efficiency (185,000/m) and chromatographic resolution were achieved when the C18 -bound phase was evaluated for a test mixture of five benzene derivatives after packing in a stainless-steel column (1.0 mm × 150 mm). The optimized elution conditions were found to be 70:30 v/v acetonitrile/water with 0.1% trifluoroacetic acid at a flow rate of 25 μL/min. The column was also evaluated for fast analysis at a flow rate of 100 μL/min, and all the five analytes were eluted within 3.5 min with reasonable efficiency (ca. 60,000/m) and resolution. The strategy of using particles with reduced particle size and large pores (363 Å) combined with C18 modification in addition to partial-monolithic architecture has resulted in a useful stationary phase (C18 -bound silica monolith particles) of low production cost showing excellent chromatographic performance. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. Fracture resistance of monolithic zirconia molar crowns with reduced thickness.

    Science.gov (United States)

    Nakamura, Keisuke; Harada, Akio; Inagaki, Ryoichi; Kanno, Taro; Niwano, Yoshimi; Milleding, Percy; Örtengren, Ulf

    2015-01-01

    The purpose of the present study was to analyze the relationship between fracture load of monolithic zirconia crowns and axial/occlusal thickness and to evaluate the fracture resistance of monolithic zirconia crowns with reduced thickness in comparison with that of monolithic lithium disilicate crowns with regular thickness. Monolithic zirconia crowns (Lava Plus Zirconia, 3M/ESPE) with specified axial/occlusal thicknesses and lithium disilicate crowns (IPS e.max press, Ivoclar/Vivadent) with regular thickness were fabricated using a dental CAD/CAM system and a press technique, respectively. The crowns cemented onto dies were loaded until fracture. Based on measurements of the crown thickness made by micro-CT and the fracture load, multiple regression analysis was performed. It was revealed that the occlusal thickness significantly affected the fracture load (p zirconia crowns, the fracture load of the zirconia crowns with the occlusal thickness of 0.5 mm (5558 ± 522 N) was significantly higher than that of lithium disilicate crowns with an occlusal thickness of 1.5 mm (3147 ± 409 N). Within the limitations of the present study, it is suggested that monolithic zirconia crown with chamfer width of 0.5 mm and occlusal thickness of 0.5 mm can be used in the molar region in terms of fracture resistance.

  13. Estimation of methacrylate monolith binding capacity from pressure drop data.

    Science.gov (United States)

    Podgornik, Aleš; Smrekar, Vida; Krajnc, Peter; Strancar, Aleš

    2013-01-11

    Convective chromatographic media comprising of membranes and monoliths represent an important group of chromatographic supports due to their flow-unaffected chromatographic properties and consequently fast separation and purification even of large biological macromolecules. Consisting of a single piece of material, common characterization procedures based on analysis of a small sample assuming to be representative for the entire batch, cannot be applied. Because of that, non-invasive characterization methods are preferred. In this work pressure drop was investigated for an estimation of dynamic binding capacity (DBC) of proteins and plasmid DNA for monoliths with different pore sizes. It was demonstrated that methacrylate monolith surface area is reciprocally proportional to pore diameter and that pressure drop on monolith is reciprocally proportional to square pore size demonstrating that methacrylate monolith microstructure is preserved by changing pore size. Based on these facts mathematical formalism has been derived predicting that DBC is in linear correlation with the square root of pressure drop. This was experimentally confirmed for ion-exchange and hydrophobic interactions for proteins and plasmid DNA. Furthermore, pressure drop was also applied for an estimation of DBC in grafted layers of different thicknesses as estimated from the pressure drop data. It was demonstrated that the capacity is proportional to the estimated grafted layer thickness. Copyright © 2012 Elsevier B.V. All rights reserved.

  14. Edge chipping and flexural resistance of monolithic ceramics☆

    Science.gov (United States)

    Zhang, Yu; Lee, James J.-W.; Srikanth, Ramanathan; Lawn, Brian R.

    2014-01-01

    Objective Test the hypothesis that monolithic ceramics can be developed with combined esthetics and superior fracture resistance to circumvent processing and performance drawbacks of traditional all-ceramic crowns and fixed-dental-prostheses consisting of a hard and strong core with an esthetic porcelain veneer. Specifically, to demonstrate that monolithic prostheses can be produced with a much reduced susceptibility to fracture. Methods Protocols were applied for quantifying resistance to chipping as well as resistance to flexural failure in two classes of dental ceramic, microstructurally-modified zirconias and lithium disilicate glass–ceramics. A sharp indenter was used to induce chips near the edges of flat-layer specimens, and the results compared with predictions from a critical load equation. The critical loads required to produce cementation surface failure in monolithic specimens bonded to dentin were computed from established flexural strength relations and the predictions validated with experimental data. Results Monolithic zirconias have superior chipping and flexural fracture resistance relative to their veneered counterparts. While they have superior esthetics, glass–ceramics exhibit lower strength but higher chip fracture resistance relative to porcelain-veneered zirconias. Significance The study suggests a promising future for new and improved monolithic ceramic restorations, with combined durability and acceptable esthetics. PMID:24139756

  15. Column-Oriented Database Systems (Tutorial)

    NARCIS (Netherlands)

    D. Abadi; P.A. Boncz (Peter); S. Harizopoulos

    2009-01-01

    textabstractColumn-oriented database systems (column-stores) have attracted a lot of attention in the past few years. Column-stores, in a nutshell, store each database table column separately, with attribute values belonging to the same column stored contiguously, compressed, and densely packed, as

  16. Monolithic Chip-Integrated Absorption Spectrometer from 3-5 microns, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — A monolithically integrated indium phosphide (InP) to silicon-on-sapphire (SoS) platform is being proposed for a monolithic portable or handheld spectrometer between...

  17. Monolithic View of Galaxy Formation and Evolution

    Directory of Open Access Journals (Sweden)

    Cesare Chiosi

    2014-07-01

    Full Text Available We review and critically discuss the current understanding of galaxy formation and evolution limited to Early Type Galaxies (ETGs as inferred from the observational data and briefly contrast the hierarchical and quasi-monolithic paradigms of formation and evolution. Since in Cold Dark Matter (CDM cosmogony small scale structures typically collapse early and form low-mass haloes that subsequently can merge to assembly larger haloes, galaxies formed in the gravitational potential well of a halo are also expected to merge thus assembling their mass hierarchically. Mergers should occur all over the Hubble time and large mass galaxies should be in place only recently. However, recent observations of high redshift galaxies tell a different story: massive ETGs are already in place at high redshift. To this aim, we propose here a revision of the quasi-monolithic scenario as an alternative to the hierarchical one, in which mass assembling should occur in early stages of a galaxy lifetime and present recent models of ETGs made of Dark and Baryonic Matter in a Λ-CDM Universe that obey the latter scheme. The galaxies are followed from the detachment from the linear regime and Hubble flow at z ≥ 20 down to the stage of nearly complete assembly of the stellar content (z ∼ 2 − 1 and beyond.  It is found that the total mass (Mh = MDM + MBM and/or initial over-density of the proto-galaxy drive the subsequent star formation histories (SFH. Massive galaxies (Mh ~ _1012M⊙ experience a single, intense burst of star formation (with rates ≥ 103M⊙/yr at early epochs, consistently with observations, with a weak dependence on the initial over-density; intermediate mass haloes (Mh~_ 1010 − 1011M⊙ have star formation histories that strongly depend on their initial over-density; finally, low mass haloes (Mh ~_ 109M⊙ always have erratic, burst-like star forming histories. The present-day properties (morphology, structure, chemistry and photometry of the

  18. Monolithic PDMS passband filters for fluorescence detection.

    Science.gov (United States)

    Llobera, Andreu; Demming, Stefanie; Joensson, Haakan N; Vila-Planas, J; Andersson-Svahn, Helene; Büttgenbach, Stephanus

    2010-08-07

    We present the fabrication and characteristics of monolithically integrated ink dyed poly(dimethylsiloxane) (PDMS) filters for optical sensing in disposable lab-on-a-chip. This represents a migration of auxillary functions onto the disposable chip with the goal of producing truly portable systems. Filters made from commercially available ink (Pelikan) directly mixed into PDMS oligomer without the use of any additional solvents were patterned with standard soft lithography technologies. Furthermore, a fabrication process based on capillary forces is presented allowing PDMS coloration of arbitrary shapes. Different filters of varying thickness fabricated using red, green and blue ink in four different concentrations were characterized. The optimal performance was found with filter thicknesses of 250 microm and ink to PDMS ratios of 0.1 (mL ink : mL PDMS oligomer) resulting in a transmittance ranging from -15.1 dB to -12.3 dB in the stopband and from -4.0 dB to -2.5 dB in the passband. Additionally, we demonstrate the robustness of this approach as the ink dyed PDMS filters do not exhibit temporal ageing due to diffusion or autofluorescence. We also show that such filters can easily be integrated in fluorescence systems, with stopbands efficient enough to allow fluorescence measurements under non-optimal conditions (broadband excitation, 180 degrees configuration). Integrated ink dyed PDMS filters add robust optical functionalities to disposable microdevices at a low cost and will enable the use of these devices for a wide range of fluorescence and absorbance based biological and chemical analysis.

  19. Cerec anterior crowns: restorative options with monolithic ceramic materials.

    Science.gov (United States)

    Reich, Sven; Fiedlar, Kurt

    2013-01-01

    The aim of this article is to discuss the different types of monolithic ceramic crowns that can be placed on anterior teeth with existing shoulder preparations. Anterior crowns were indicated for the teeth 12 to 22 in the present case. The patient, a 65-year-old male, had received all-ceramic crowns 20 years earlier, which had started to develop cracks and palatal fractures over the last few years. The patient's teeth were prepared and four sets of crowns were fabricated using different monolithic ceramic materials: IPS e.max CAD, Cerec Blocs C In, VITABLOCS Real Life, and ENAMIC. Both shade characterization and crystallization firing were performed on the monolithic lithium disilicate glass ceramic crowns. The silicate ceramic crowns received glaze firing alone. The crowns made of hybrid ceramic (ENAMIC) were treated with a polymer sealant.

  20. Monolithic optoelectronic integrated broadband optical receiver with graphene photodetectors

    Directory of Open Access Journals (Sweden)

    Cheng Chuantong

    2017-07-01

    Full Text Available Optical receivers with potentially high operation bandwidth and low cost have received considerable interest due to rapidly growing data traffic and potential Tb/s optical interconnect requirements. Experimental realization of 65 GHz optical signal detection and 262 GHz intrinsic operation speed reveals the significance role of graphene photodetectors (PDs in optical interconnect domains. In this work, a novel complementary metal oxide semiconductor post-backend process has been developed for integrating graphene PDs onto silicon integrated circuit chips. A prototype monolithic optoelectronic integrated optical receiver has been successfully demonstrated for the first time. Moreover, this is a firstly reported broadband optical receiver benefiting from natural broadband light absorption features of graphene material. This work is a perfect exhibition of the concept of monolithic optoelectronic integration and will pave way to monolithically integrated graphene optoelectronic devices with silicon ICs for three-dimensional optoelectronic integrated circuit chips.

  1. Monolithic optoelectronic integrated broadband optical receiver with graphene photodetectors

    Science.gov (United States)

    Cheng, Chuantong; Huang, Beiju; Mao, Xurui; Zhang, Zanyun; Zhang, Zan; Geng, Zhaoxin; Xue, Ping; Chen, Hongda

    2017-07-01

    Optical receivers with potentially high operation bandwidth and low cost have received considerable interest due to rapidly growing data traffic and potential Tb/s optical interconnect requirements. Experimental realization of 65 GHz optical signal detection and 262 GHz intrinsic operation speed reveals the significance role of graphene photodetectors (PDs) in optical interconnect domains. In this work, a novel complementary metal oxide semiconductor post-backend process has been developed for integrating graphene PDs onto silicon integrated circuit chips. A prototype monolithic optoelectronic integrated optical receiver has been successfully demonstrated for the first time. Moreover, this is a firstly reported broadband optical receiver benefiting from natural broadband light absorption features of graphene material. This work is a perfect exhibition of the concept of monolithic optoelectronic integration and will pave way to monolithically integrated graphene optoelectronic devices with silicon ICs for three-dimensional optoelectronic integrated circuit chips.

  2. Sedimentation assisted preparation of ground particles of silica monolith and their C18 modification resulting in a chromatographic phase of improved separation efficiency.

    Science.gov (United States)

    Ali, Ashraf; Ali, Faiz; Cheong, Won Jo

    2017-11-24

    The sedimentation procedure has been adopted in production of ground silica monolith particles to improve chromatographic separation efficiency of the resultant phase. First, silica monolith particles have been successfully prepared in a large scale by a sol-gel process followed by grinding. The particles after calcination were separated by sedimentation into three zones using an Imhoff sedimentation cone. The particles of the bottom zone were derivatized with a C18 ligand and end-capped. The sedimentation process was found to not only eliminate troublesome minute particles but also narrow down the particle size distribution. The resultant phase was packed in glass lined stainless steel micro-columns. The average number of theoretical plates (N) of the columns for a test mixture was 47,000 and 29,300 for the 300 and 150mm columns (1mm internal diameter), corresponding to 157,000/m and 195,000/m, respectively. Copyright © 2017 Elsevier B.V. All rights reserved.

  3. Water Column Sonar Data Collection

    Data.gov (United States)

    National Oceanic and Atmospheric Administration, Department of Commerce — The collection and analysis of water column sonar data is a relatively new avenue of research into the marine environment. Primary uses include assessing biological...

  4. Preparation of poly(γ-glutamic acid)/hydroxyapatite monolith via biomineralization for bone tissue engineering.

    Science.gov (United States)

    Park, Sung-Bin; Hasegawa, Urara; van der Vlies, André J; Sung, Moon-Hee; Uyama, Hiroshi

    2014-01-01

    A hybrid monolith of poly(γ-glutamic acid) and hydroxyapatite (PGA/HAp monolith) was prepared via biomineralization and used as a macroporous cell scaffold in bone tissue engineering. The PGA monolith having a bimodal pore size distribution was used as a substrate to induce biomineralization. The PGA/HAp monolith was obtained by immersing the PGA monolith in simulated body fluid. Pretreatment with CaCl2 enhanced the apatite-forming ability of the PGA monolith. Murine osteoblastic MC3T3-E1 cells efficiently attached and proliferated on the PGA/HAp monolith. MTT assay showed that both the PGA and PGA/HAp monolith did not have apparent cytotoxicity. Moreover, the PGA and PGA/HAp monoliths adsorbed bone morphogenetic protein-2 (BMP-2) by electrostatic interaction which was slowly released in the medium during cell culture. The PGA/HAp monolith enhanced BMP-2 induced alkaline phosphatase activity compared to the PGA monolith and a polystyrene culture plate. Thus, these PGA/HAp monoliths may have potential in bone tissue engineering.

  5. Optimizing the experimental design of soil columns in saturated and unsaturated transport experiments.

    Science.gov (United States)

    Lewis, Jeffrey; Sjöstrom, Jan

    2010-06-25

    Soil column experiments in both the saturated and unsaturated regimes are widely used for applied and theoretical studies in such diverse fields as transport model evaluation, fate and transport of pesticides, explosives, microbes, heavy metals and non aqueous phase liquids, and for evapotranspiration studies. The apparent simplicity of constructing soil columns conceals a number of technical issues which can seriously affect the outcome of an experiment, such as the presence or absence of macropores, artificial preferential flow paths, non-ideal infiltrate injection and unrealistic moisture regimes. This review examines the literature to provide an analysis of the state of the art for constructing both saturated and unsaturated soil columns. Common design challenges are discussed and best practices for potential solutions are presented. This article discusses both basic principles and the practical advantages and disadvantages of various experimental approaches. Both repacked and monolith-type columns are discussed. The information in this review will assist soil scientists, hydrogeologists and environmental professionals in optimizing the construction and operation of soil column experiments in order to achieve their objectives, while avoiding serious design flaws which can compromise the integrity of their results. 2010 Elsevier B.V. All rights reserved.

  6. Behavior of Confined Columns under Different Techniques

    OpenAIRE

    Mostafa Osman; Ata El-Kareim Shoeib Soliman

    2015-01-01

    Since columns are the most important elements of the structures, failure of one column in a critical location can cause a progressive collapse. In this respect, the repair and strengthening of columns is a very important subject to reduce the building failure and to keep the columns capacity. Twenty columns with different parameters is tested and analysis. Eleven typical confined reinforced concrete (RC) columns with different types of techniques are assessment. And also,...

  7. Paladin Enterprises: Monolithic particle physics models global climate.

    CERN Multimedia

    2002-01-01

    Paladin Enterprises presents a monolithic particle model of the universe which will be used by them to build an economical fusion energy system. The model is an extension of the work done by James Clerk Maxwell. Essentially, gravity is unified with electro-magnetic forces and shown to be a product of a closed loop current system, i.e. a particle - monolithic or sub atomic. This discovery explains rapid global climate changes which are evident in the geological record and also provides an explanation for recent changes in the global climate.

  8. LIQUID-LIQUID EXTRACTION COLUMNS

    Science.gov (United States)

    Thornton, J.D.

    1957-12-31

    This patent relates to liquid-liquid extraction columns having a means for pulsing the liquid in the column to give it an oscillatory up and down movement, and consists of a packed column, an inlet pipe for the dispersed liquid phase and an outlet pipe for the continuous liquid phase located in the direct communication with the liquid in the lower part of said column, an inlet pipe for the continuous liquid phase and an outlet pipe for the dispersed liquid phase located in direct communication with the liquid in the upper part of said column, a tube having one end communicating with liquid in the lower part of said column and having its upper end located above the level of said outlet pipe for the dispersed phase, and a piston and cylinder connected to the upper end of said tube for applying a pulsating pneumatic pressure to the surface of the liquid in said tube so that said surface rises and falls in said tube.

  9. Constitutive Theory Developed for Monolithic Ceramic Materials

    Science.gov (United States)

    Janosik, Lesley A.

    1998-01-01

    with these service conditions by developing a multiaxial viscoplastic constitutive model that accounts for time-dependent hereditary material deformation (such as creep and stress relaxation) in monolithic structural ceramics. Using continuum principles of engineering mechanics, we derived the complete viscoplastic theory from a scalar dissipative potential function.

  10. Radiotracer Imaging of Sediment Columns

    Science.gov (United States)

    Moses, W. W.; O'Neil, J. P.; Boutchko, R.; Nico, P. S.; Druhan, J. L.; Vandehey, N. T.

    2010-12-01

    Nuclear medical PET and SPECT cameras routinely image radioactivity concentration of gamma ray emitting isotopes (PET - 511 keV; SPECT - 75-300 keV). We have used nuclear medical imaging technology to study contaminant transport in sediment columns. Specifically, we use Tc-99m (T1/2 = 6 h, Eγ = 140 keV) and a SPECT camera to image the bacteria mediated reduction of pertechnetate, [Tc(VII)O4]- + Fe(II) → Tc(IV)O2 + Fe(III). A 45 mL bolus of Tc-99m (32 mCi) labeled sodium pertechnetate was infused into a column (35cm x 10cm Ø) containing uranium-contaminated subsurface sediment from the Rifle, CO site. A flow rate of 1.25 ml/min of artificial groundwater was maintained in the column. Using a GE Millennium VG camera, we imaged the column for 12 hours, acquiring 44 frames. As the microbes in the sediment were inactive, we expected most of the iron to be Fe(III). The images were consistent with this hypothesis, and the Tc-99m pertechnetate acted like a conservative tracer. Virtually no binding of the Tc-99m was observed, and while the bolus of activity propagated fairly uniformly through the column, some inhomogeneity attributed to sediment packing was observed. We expect that after augmentation by acetate, the bacteria will metabolically reduce Fe(III) to Fe(II), leading to significant Tc-99m binding. Imaging sediment columns using nuclear medicine techniques has many attractive features. Trace quantities of the radiolabeled compounds are used (micro- to nano- molar) and the half-lives of many of these tracers are short (Image of Tc-99m distribution in a column containing Rifle sediment at four times.

  11. Performance evaluation of a rectifier column using gamma column scanning

    Directory of Open Access Journals (Sweden)

    Aquino Denis D.

    2017-12-01

    Full Text Available Rectifier columns are considered to be a critical component in petroleum refineries and petrochemical processing installations as they are able to affect the overall performance of these facilities. It is deemed necessary to monitor the operational conditions of such vessels to optimize processes and prevent anomalies which could pose undesired consequences on product quality that might lead to huge financial losses. A rectifier column was subjected to gamma scanning using a 10-mCi Co-60 source and a 2-inch-long detector in tandem. Several scans were performed to gather information on the operating conditions of the column under different sets of operating parameters. The scan profiles revealed unexpected decreases in the radiation intensity at vapour levels between trays 2 and 3, and between trays 4 and 5. Flooding also occurred during several scans which could be attributed to parametric settings.

  12. Post column derivatisation analyses review. Is post-column derivatisation incompatible with modern HPLC columns?

    Science.gov (United States)

    Jones, Andrew; Pravadali-Cekic, Sercan; Dennis, Gary R; Shalliker, R Andrew

    2015-08-19

    Post Column derivatisation (PCD) coupled with high performance liquid chromatography or ultra-high performance liquid chromatography is a powerful tool in the modern analytical laboratory, or at least it should be. One drawback with PCD techniques is the extra post-column dead volume due to reaction coils used to enable adequate reaction time and the mixing of reagents which causes peak broadening, hence a loss of separation power. This loss of efficiency is counter-productive to modern HPLC technologies, -such as UHPLC. We reviewed 87 PCD methods published from 2009 to 2014. We restricted our review to methods published between 2009 and 2014, because we were interested in the uptake of PCD methods in UHPLC environments. Our review focused on a range of system parameters including: column dimensions, stationary phase and particle size, as well as the geometry of the reaction loop. The most commonly used column in the methods investigated was not in fact a modern UHPLC version with sub-2-micron, (or even sub-3-micron) particles, but rather, work-house columns, such as, 250 × 4.6 mm i.d. columns packed with 5 μm C18 particles. Reaction loops were varied, even within the same type of analysis, but the majority of methods employed loop systems with volumes greater than 500 μL. A second part of this review illustrated briefly the effect of dead volume on column performance. The experiment evaluated the change in resolution and separation efficiency of some weak to moderately retained solutes on a 250 × 4.6 mm i.d. column packed with 5 μm particles. The data showed that reaction loops beyond 100 μL resulted in a very serious loss of performance. Our study concluded that practitioners of PCD methods largely avoid the use of UHPLC-type column formats, so yes, very much, PCD is incompatible with the modern HPLC column. Copyright © 2015. Published by Elsevier B.V.

  13. Monolithic CMOS pixel detector for international linear collider ...

    Indian Academy of Sciences (India)

    the vertex detector elements and thus existing CCDs are not adequate. New CCD architectures are ... sizes of the 292 detector elements (chips) are summarized in tables 1 and 2. The baseline time structure of ... an R&D contract, we developed a conceptual design for a monolithic CMOS device. (chip) that achieves the ILC ...

  14. Monolithic CMOS pixel detector for international linear collider ...

    Indian Academy of Sciences (India)

    Toggle navigation. Logo of the Indian Academy of Sciences. Indian Academy of Sciences. Home · About ... Home; Journals; Pramana – Journal of Physics; Volume 69; Issue 6. Monolithic CMOS pixel detector for international linear ... Keywords. Vertex detector; international linear collider; linear collider; high energy physics.

  15. CMOS Monolithic Active Pixel Sensors (MAPS): developments and future outlook

    NARCIS (Netherlands)

    Turchetta, R.; Fant, A.; Gasiorek, P.; Esbrand, C.; Griffiths, J.A.; Metaxas, M.G.; Royle, G.J.; Speller, R.; Venanzi, C.; van der Stelt, P.F.; Verheij, H.; Li, G.; Theodoridis, S.; Georgiou, H.; Cavouras, D.; Hall, G.; Noy, M.; Jones, J.; Leaver, J.; Machin, D.; Greenwood, S.; Khaleeq, M.; Schulerud, H.; Østby, J.M.; Triantis, F.; Asimidis, A.; Bolanakis, D.; Manthos, N.; Longo, R.; Bergamaschi, A.

    2007-01-01

    Re-invented in the early 1990s, on both sides of the Atlantic, Monolithic Active Pixel Sensors (MAPS) in a CMOS technology are today the most sold solid-state imaging devices, overtaking the traditional technology of Charge-Coupled Devices (CCD). The slow uptake of CMOS MAPS started with low-end

  16. Status of the Monolithic Suspensions for Advanced Virgo

    Science.gov (United States)

    Travasso, F.; Virgo Collaboration

    2018-02-01

    Successfully implemented in GEO and Virgo+, the monolithic suspensions are one of the most important upgrades in the second generation of gravitational wave interferometric detectors, including Advanced LIGO (aLIGO) and Advanced Virgo (AdV). Characterized by a very low thermal noise, monolithic suspensions are essential for improving the interferometers sensitivity at low frequencies (10-100Hz). In Advanced Virgo their installation was delayed because of a contamination problem in the vacuum system: dust produced by scroll pumps was injected in the main vacuum chambers during the venting processes, damaging the fibers and ultimately causing their repeated failure. The effort to explain and resolve this issue was useful to further confirm the suspensions’ reliability and our control on the production process. Moreover, we developed and implemented new tools and procedures to certify each part of the monolithic suspensions. In the meanwhile, in order to join aLIGO during its second Observation Run (O2), a temporary steel suspension was implemented, based on the initial Virgo design. That solution allowed us to contribute to the first three-detector observation of a gravitational wave (GW) ([1]), and to the first observation of a coalescing neutron star binary ([2]) In the near future the monolithic suspensions will be reinstalled along with additional upgrades of Virgo.

  17. High density fuels using dispersion and monolithic fuel

    Energy Technology Data Exchange (ETDEWEB)

    Gomes, Daniel S.; Silva, Antonio T.; Abe, Alfredo Y.; Muniz, Rafael O.R.; Giovedi, Claudia, E-mail: dsgomes@ipen.br, E-mail: teixeira@ipen.br, E-mail: alfredo@ctmsp.mar.mil.br, E-mail: rafael.orm@gmail.com, E-mail: claudia.giovedi@ctmsp.mar.mil.br [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil); Universidade de São Paulo (USP), SP (Brazil). Departamento de Engenharia Naval e Oceânica

    2017-07-01

    Fuel plates used in high-performance research reactors need to be converted to low-enrichment uranium fuel; the fuel option based on a monolithic formulation requires alloys to contain 6 - 10 wt% Mo. In this case, the fuel plates are composed of the metallic alloy U-10Mo surrounded by a thin zirconium layer encapsulated in aluminum cladding. This study reviewed the physical properties of monolithic forms. The constraints produced during the manufacturing process were analyzed and compared to those of dispersed fuel. The bonding process used for dispersion fuels differs from the techniques applied to foil bonding used for pure alloys. The quality of monolithic plates depends on the fabrication method, which usually involves hot isostatic pressing and the thermal annealing effect of residual stress, which degrades the uranium cubic phase. The preservation of the metastable phase has considerable influence on fuel performance. The physical properties of the foil fuel under irradiation are superior to those of aluminum-dispersed fuels. The fuel meat, using zirconium as the diffusion barrier, prevents the interaction layer from becoming excessively thick. The problem with dispersed fuel is breakaway swelling with a medium fission rate. It has been observed that the fuel dispersed in aluminum was minimized in monolithic forms. The pure alloys exhibited a suitable response from a rate at least twice as much as the fission rate of dispersions. The foils can support fissile material concentration combined with a reduced swelling rate. (author)

  18. A Monolithic Perovskite Structure for Use as a Magnetic Regenerator

    DEFF Research Database (Denmark)

    Pryds, Nini; Clemens, Frank; Menon, Mohan

    2011-01-01

    and the influence of the sintering on the adiabatic temperature change, were investigated. Comparisons between the extruded monolithic structure before and after the sintering showed that an increase of the adiabatic temperature change was seen after the sintering. Furthermore, calculations show...

  19. A radiation hard bipolar monolithic front-end readout

    CERN Document Server

    Baschirotto, A; Cappelluti, I; Castello, R; Cermesoni, M; Gola, A; Pessina, G; Pistolesi, E; Rancoita, P G; Seidman, A

    1999-01-01

    A fast bipolar monolithic charge sensitive preamplifier (CSP), implemented in the monolithic 2 mu m BiCMOS technology (called HF2CMOS) was designed and built in a quad monolithic chip. Studies of radiation effects in the CSP $9 performance, from non-irradiated and up to neutron irradiation of 5.3*10/sup 14/ n/cm/sup 2/, have confirmed that the use of bipolar npn transistors is suitable for the radiation level of the future LHC collider environment. The CSP $9 presents a new circuit solution for obtaining adequate slew rate performances which results in an integral linearity better than 0.8554330n 5 V at 20 ns of shaping time, regardless of the bias current selected for the CSP. This way $9 the bias current of the CSP can be set for optimizing the power dissipation with respect to series and parallel noise, especially useful when the CSP is put in a radiation environment. A prototype test with a novel monolithic 20 ns $9 time constant RC-CR shaper, capable to sum up four inputs has been also realized, featurin...

  20. Monolithic natural gas storage delivery system based on sorbents

    Energy Technology Data Exchange (ETDEWEB)

    Hornbostel, Marc; Krishnan, Gopala N.; Sanjurjo, Angel

    2016-09-27

    The invention provides methods for producing a strong, light, sorbent-based storage/dispenser system for gases and fuels. The system comprises a porous monolithic material with an adherent strong impervious skin that is capable of storing a gas under pressure in a safe and usable manner.

  1. Study of monolithic prestressed reinforced concrete overhead road.

    Directory of Open Access Journals (Sweden)

    Ya.I. Kovalchyk

    2011-12-01

    Full Text Available Results of inspection and testing of monolithic prestressed reinforced concrete road trestle built in Kyiv are considered. The analysis of the gained results has shown that parametres correspond to the requirements of current standards on design of bridges.

  2. Monolithic CMOS pixel detector for international linear collider ...

    Indian Academy of Sciences (India)

    the vertex detector elements and thus existing CCDs are not adequate. New CCD architectures are under development [2] but have yet to achieve the required perfor- mance. For these reasons there is an increased importance on the development of monolithic CMOS pixel detectors that allow extremely fast non-sequential ...

  3. Environmentally Benign Production of Stretchable and Robust Superhydrophobic Silicone Monoliths.

    Science.gov (United States)

    Davis, Alexander; Surdo, Salvatore; Caputo, Gianvito; Bayer, Ilker S; Athanassiou, Athanassia

    2018-01-24

    Superhydrophobic materials hold an enormous potential in sectors as important as aerospace, food industries, or biomedicine. Despite this great promise, the lack of environmentally friendly production methods and limited robustness remain the two most pertinent barriers to the scalability, large-area production, and widespread use of superhydrophobic materials. In this work, highly robust superhydrophobic silicone monoliths are produced through a scalable and environmentally friendly emulsion technique. It is first found that stable and surfactantless water-in-polydimethylsiloxane (PDMS) emulsions can be formed through mechanical mixing. Increasing the internal phase fraction of the precursor emulsion is found to increase porosity and microtexture of the final monoliths, rendering them superhydrophobic. Silica nanoparticles can also be dispersed in the aqueous internal phase to create micro/nanotextured monoliths, giving further improvements in superhydrophobicity. Due to the elastomeric nature of PDMS, superhydrophobicity can be maintained even while the material is mechanically strained or compressed. In addition, because of their self-similarity, the monoliths show outstanding robustness to knife-scratch, tape-peel, and finger-wipe tests, as well as rigorous sandpaper abrasion. Superhydrophobicity was also unchanged when exposed to adverse environmental conditions including corrosive solutions, UV light, extreme temperatures, and high-energy droplet impact. Finally, important properties for eventual adoption in real-world applications including self-cleaning, stain-repellence, and blood-repellence are demonstrated.

  4. Mechanical monolithic horizontal sensor for low frequency seismic noise measurement.

    Science.gov (United States)

    Acernese, Fausto; Giordano, Gerardo; Romano, Rocco; De Rosa, Rosario; Barone, Fabrizio

    2008-07-01

    This paper describes a mechanical monolithic horizontal sensor for geophysical applications developed at the University of Salerno. The instrument is basically a monolithic tunable folded pendulum, shaped with precision machining and electric discharge machining, that can be used both as seismometer and, in a force-feedback configuration, as accelerometer. The monolithic mechanical design and the introduction of laser interferometric techniques for the readout implementation makes it a very compact instrument, very sensitive in the low frequency seismic noise band, with a very good immunity to environmental noises. Many changes have been produced since last version (2007), mainly aimed to the improvement of the mechanics and of the optical readout of the instrument. In fact, we have developed and tested a prototype with elliptical hinges and mechanical tuning of the resonance frequency together with a laser optical lever and a new laser interferometer readout system. The theoretical sensitivity curve for both laser optical lever and laser interferometric readouts, evaluated on the basis of suitable theoretical models, shows a very good agreement with the experimental measurements. Very interesting scientific result is the measured natural resonance frequency of the instrument of 70 mHz with a Q=140 in air without thermal stabilization. This result demonstrates the feasibility of a monolithic folded pendulum sensor with a natural resonance frequency of the order of millihertz with a more refined mechanical tuning.

  5. Development of a simple technique for the coating of monolithic silica with pristine boron nitride nanotubes (BNNTs): HPLC chromatographic applications.

    Science.gov (United States)

    Guillaume, Yves Claude; André, Claire

    2017-03-01

    In this paper, a novel and very simple homogeneous coating of a monolithic silica HPLC support using pristine boron nitride nanotubes (BNNTs) was d0.escribed. The chromatographic support was coated with BNNTs in a non covalent way to preserve the nanotube structure. A solution of BNNTs dispersed in dimethylacetamide (DMAc) was pumped through the column at a flow-rate of 0.3mL/min for 24h at room temperature. Strong interaction between amino groups and the BNNT surfaces induces the adsorption of the BNNTs on the silica, while the stable solvation in DMAc hampers further adsorption of the tubes. The excellent stability of the non covalent BNNT-coating on the monolithic silica in view of application for HPLC was also demonstrated. It was shown that this novel stationary phase was efficient for the HPLC isocratic or gradient mode separation of molecules of different structure such as phenol derivatives, alkylbenzene or doping agents (steroids). As well, this simple technique of BNNT immobilization offers new perspectives for the BNNT-coating on the surfaces of a wide range of solid substrates. Copyright © 2016 Elsevier B.V. All rights reserved.

  6. Semi-high-throughput isolation and N-glycan analysis of human fibrinogen using monolithic supports bearing monoclonal anti-human fibrinogen antibodies.

    Science.gov (United States)

    Vidic, Urška; Trbojević-Akmačić, Irena; Černigoj, Urh; Albers, Malena; Gašperšič, Jernej; Pučić-Baković, Maja; Vidič, Jana; Štrancar, Aleš; Lauc, Gordan

    2017-11-01

    Fibrinogen (FIB) is a secretory glycoprotein synthesized by hepatocytes that has a key role in blood clotting. Its glycosylation has not been studied in detail and little is known about the biological variability of FIB N-glycosylation, mainly due to the lack of fast, simple, and robust approaches to purify FIB from blood plasma samples. In recent years, customised chromatographic monoliths have been used for a variety of biological applications due to their unique characteristics. Here we describe development and optimisation of monolithic supports bearing monoclonal anti-human fibrinogen antibodies in a single column as well as in multi-well plate formats with high FIB specificity and binding capacity for fast immunoaffinity purification of FIB from human blood samples. The developed semi-high-throughput workflow has been successfully applied for FIB immunoaffinity isolation and subsequent ultra performance liquid chromatography N-glycosylation analysis in ten healthy human individuals, demonstrating the potential of monolithic supports in glycomics studies. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Bubble columns : Structures or stability?

    NARCIS (Netherlands)

    Harteveld, W.K.

    2005-01-01

    The aim of the thesis is to contribute to the understanding of the hydrodynamics of the gravity driven bubbly flow that can be found in bubble columns. Special attention is paid to the large scale structures that have a strong impact on several key parameters such as the degree of mixing, mass and

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

    Science.gov (United States)

    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.

  9. Capillary methacrylate-based monoliths by grafting from/to γ-ray polymerization on a tentacle-type reactive surface for the liquid chromatographic separations of small molecules and intact proteins.

    Science.gov (United States)

    Simone, Patrizia; Pierri, Giuseppe; Capitani, Donatella; Ciogli, Alessia; Angelini, Giancarlo; Ursini, Ornella; Gentile, Gennaro; Cavazzini, Alberto; Villani, Claudio; Gasparrini, Francesco

    2017-05-19

    Capillary methacrylate-based monoliths were prepared for the high performance liquid chromatography (HPLC) separation of both small molecules and large biomolecules. An efficient grafting from/to synthetic approach was adopted introducing a network of activated sites in the inner wall surface using the new silanization agent (N-trimethoxysilylpropyl)-polyethylenimine. Copolymerization of lauryl methacrylate monomer and 1,6-hexanediol dimethacrylate cross-linker in the presence of porogenic solvents was obtained under continuous γ-ray exposure with high conversion yield. The morphology and porous structure of the resulting monoliths have been investigated by Scanning Electron Microscopy (SEM) and 1 H NMR cryoporosimetry. By chromatographic investigation, the new capillary columns attested high kinetic performance (with efficiency larger than 100,000 theoretical plate/m for small molecules at optimum mobile phase linear velocity of about 0.5mm/s) and also excellent mechanical stability and repeatability. The new methacrylate-based monolithic capillary columns have been successfully employed for efficient reversed-phase separation of intact proteins and peptides. Copyright © 2016 Elsevier B.V. All rights reserved.

  10. Monolithic millimeter-wave and picosecond electronic technologies

    International Nuclear Information System (INIS)

    Talley, W.K.; Luhmann, N.C.

    1996-01-01

    Theoretical and experimental studies into monolithic millimeter-wave and picosecond electronic technologies have been undertaken as a collaborative project between the Lawrence Livermore National Laboratory (LLNL) and the University of California Department of Applied Science Coherent Millimeter-Wave Group under the auspices of the Laboratory Directed Research and Development Program at LLNL. The work involves the design and fabrication of monolithic frequency multiplier, beam control, and imaging arrays for millimeter-wave imaging and radar, as well as the development of high speed nonlinear transmission lines for ultra-wideband radar imaging, time domain materials characterization and magnetic fusion plasma applications. In addition, the Coherent Millimeter-Wave Group is involved in the fabrication of a state-of-the-art X-band (∼8-11 GHz) RF photoinjector source aimed at producing psec high brightness electron bunches for advanced accelerator and coherent radiation generation studies

  11. Hydrogenation with monolith reactor under conditions of immiscible liquid phases

    Science.gov (United States)

    Nordquist, Andrew Francis; Wilhelm, Frederick Carl; Waller, Francis Joseph; Machado, Reinaldo Mario

    2002-01-01

    The present invention relates to an improved for the hydrogenation of an immiscible mixture of an organic reactant in water. The immiscible mixture can result from the generation of water by the hydrogenation reaction itself or, by the addition of, water to the reactant prior to contact with the catalyst. The improvement resides in effecting the hydrogenation reaction in a monolith catalytic reactor from 100 to 800 cpi, at a superficial velocity of from 0.1 to 2 m/second in the absence of a cosolvent for the immiscible mixture. In a preferred embodiment, the hydrogenation is carried out using a monolith support which has a polymer network/carbon coating onto which a transition metal is deposited.

  12. Monolithic integration of a plasmonic sensor with CMOS technology

    Science.gov (United States)

    Shakoor, Abdul; Cheah, Boon C.; Hao, Danni; Al-Rawhani, Mohammed; Nagy, Bence; Grant, James; Dale, Carl; Keegan, Neil; McNeil, Calum; Cumming, David R. S.

    2017-02-01

    Monolithic integration of nanophotonic sensors with CMOS detectors can transform the laboratory based nanophotonic sensors into practical devices with a range of applications in everyday life. In this work, by monolithically integrating an array of gold nanodiscs with the CMOS photodiode we have developed a compact and miniaturized nanophotonic sensor system having direct electrical read out. Doing so eliminates the need of expensive and bulky laboratory based optical spectrum analyzers used currently for measurements of nanophotonic sensor chips. The experimental optical sensitivity of the gold nanodiscs is measured to be 275 nm/RIU which translates to an electrical sensitivity of 5.4 V/RIU. This integration of nanophotonic sensors with the CMOS electronics has the potential to revolutionize personalized medical diagnostics similar to the way in which the CMOS technology has revolutionized the electronics industry.

  13. From 1D to 3D - macroscopic nanowire aerogel monoliths

    Science.gov (United States)

    Cheng, Wei; Rechberger, Felix; Niederberger, Markus

    2016-07-01

    Here we present a strategy to assemble one-dimensional nanostructures into a three-dimensional architecture with macroscopic size. With the assistance of centrifugation, we successfully gel ultrathin W18O49 nanowires with diameters of 1 to 2 nm and aspect ratios larger than 100 into 3D networks, which are transformed into monolithic aerogels by supercritical drying.Here we present a strategy to assemble one-dimensional nanostructures into a three-dimensional architecture with macroscopic size. With the assistance of centrifugation, we successfully gel ultrathin W18O49 nanowires with diameters of 1 to 2 nm and aspect ratios larger than 100 into 3D networks, which are transformed into monolithic aerogels by supercritical drying. Electronic supplementary information (ESI) available: Experimental details, SEM and TEM images, and digital photographs. See DOI: 10.1039/c6nr04429h

  14. Coherent optical monolithic phased-array antenna steering system

    Science.gov (United States)

    Hietala, Vincent M.; Kravitz, Stanley H.; Vawter, Gregory A.

    1994-01-01

    An optical-based RF beam steering system for phased-array antennas comprising a photonic integrated circuit (PIC). The system is based on optical heterodyning employed to produce microwave phase shifting by a monolithic PIC constructed entirely of passive components. Microwave power and control signal distribution to the antenna is accomplished by optical fiber, permitting physical separation of the PIC and its control functions from the antenna. The system reduces size, weight, complexity, and cost of phased-array antenna systems.

  15. Monolithic AlGaAs second-harmonic nanoantennas.

    Science.gov (United States)

    Gili, V F; Carletti, L; Locatelli, A; Rocco, D; Finazzi, M; Ghirardini, L; Favero, I; Gomez, C; Lemaître, A; Celebrano, M; De Angelis, C; Leo, G

    2016-07-11

    We demonstrate monolithic aluminum gallium arsenide (AlGaAs) optical nanoantennas. Using a selective oxidation technique, we fabricated epitaxial semiconductor nanocylinders on an aluminum oxide substrate. Second harmonic generation from AlGaAs nanocylinders of 400 nm height and varying radius pumped with femtosecond pulses delivered at 1554-nm wavelength has been measured, revealing a peak conversion efficiency exceeding 10-5 for nanocylinders with an optimized geometry.

  16. Clinical assessment of enamel wear caused by monolithic zirconia crowns.

    Science.gov (United States)

    Stober, T; Bermejo, J L; Schwindling, F S; Schmitter, M

    2016-08-01

    The purpose of this study was to measure enamel wear caused by antagonistic monolithic zirconia crowns and to compare this with enamel wear caused by contralateral natural antagonists. Twenty monolithic zirconia full molar crowns were placed in 20 patients. Patients with high activity of the masseter muscle at night (bruxism) were excluded. For analysis of wear, vinylpolysiloxane impressions were prepared after crown incorporation and at 6-, 12-, and 24-month follow-up. Wear of the occlusal contact areas of the crowns, of their natural antagonists, and of two contralateral natural antagonists (control teeth) was measured by use of plaster replicas and a 3D laser-scanning device. Differences of wear between the zirconia crown antagonists and the control teeth were investigated by means of two-sided paired Student's t-tests and linear regression analysis. After 2 years, mean vertical loss was 46 μm for enamel opposed to zirconia, 19-26 μm for contralateral control teeth and 14 μm for zirconia crowns. Maximum vertical loss was 151 μm for enamel opposed to zirconia, 75-115 μm for control teeth and 60 μm for zirconia crowns. Statistical analysis revealed significant differences between wear of enamel by zirconia-opposed teeth and by control teeth. Gender, which significantly affected wear, was identified as a possible confounder. Monolithic zirconia crowns generated more wear of opposed enamel than did natural teeth. Because of the greater wear caused by other dental ceramics, the use of monolithic zirconia crowns may be justified. © 2016 John Wiley & Sons Ltd.

  17. An Energy Preserving Monolithic Eulerian Fluid-Structure Numerical Scheme *

    OpenAIRE

    Pironneau, Olivier

    2016-01-01

    The conservation laws of continuum mechanic written in an Eulerian frame make no difference between fluids and solids except in the expression of the stress tensors, usually with Newton's hypothesis for the fluids and Helmholtz potentials of energy for hyperelastic solids. By taking the velocities as unknown , monolithic methods for fluid structure interactions (FSI) are built. In this article such a formulation is analyzed when the fluid is compressible and the fluid is incompressible. The i...

  18. An Energy stable Monolithic Eulerian Fluid-Structure Numerical Scheme *

    OpenAIRE

    Pironneau , Olivier

    2017-01-01

    The conservation laws of continuum mechanic written in an Eulerian frame make no difference between fluids and solids except in the expression of the stress tensors, usually with Newton's hypothesis for the fluids and Helmholtz potentials of energy for hyperelastic solids. By taking the velocities as unknown , monolithic methods for fluid structure interactions (FSI) are built. In this article such a formulation is analyzed when the fluid is compressible and the fluid is incompressible. The i...

  19. Fabrication and characterization of nanotemplated carbon monolithic material

    OpenAIRE

    He, Xiaoyun; Nesterenko, Ekaterina; Nesterenko, Pavel; Brabazon, Dermot; Zhou, Lin; Glennon, Jeremy D.; Luong, John H.T.; Paull, Brett

    2013-01-01

    A novel hierarchical nanotemplated carbon monolithic rod (NTCM) was prepared using a novel facile nanotemplating approach. The NTCM was obtained using C60-fullerene modified silica gels as hard templates, which were embedded in a phenolic resin containing a metal catalyst for localized graphitization, followed by bulk carbonization, and template and catalyst removal. TEM, SEM, and BET measurements revealed that NTCM possessed an integrated open hierarchical porous structure, with a trimodal p...

  20. Porous polyacrylamide monoliths in hydrophilic interaction capillary electrochromatography of oligosaccharides

    Czech Academy of Sciences Publication Activity Database

    Guryča, Vilém; Mechref, Y.; Palm, A. K.; Michálek, Jiří; Pacáková, V.; Novotny, M. V.

    2007-01-01

    Roč. 70, č. 1 (2007), s. 3-13 ISSN 0165-022X R&D Projects: GA MŠk 1M0538 Grant - others:U.S. Department of Health and Human Services(US) GM24349 Institutional research plan: CEZ:AV0Z40500505 Keywords : polyacrylamide monoliths * analytical glycobiology * capillary electrochromatography Subject RIV: CD - Macromolecular Chemistry Impact factor: 1.338, year: 2007

  1. Nanoparticle-modified monolithic pipette tips for phosphopeptide enrichment

    Czech Academy of Sciences Publication Activity Database

    Křenková, Jana; Foret, František

    2013-01-01

    Roč. 405, č. 7 (2013), s. 2175-2183 ISSN 1618-2642 R&D Projects: GA ČR(CZ) GAP301/11/2055 Grant - others:Jihomoravský kraj(CZ) 2SGA2721 Program:2SGA Institutional support: RVO:68081715 Keywords : nanoparticles * monolith * phosphopeptide Enrichment Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.578, year: 2013

  2. Distributed or Monolithic? A Computational Architecture Decision Framework

    OpenAIRE

    Mosleh, Mohsen; Dalili, Kia; Heydari, Babak

    2016-01-01

    Distributed architectures have become ubiquitous in many complex technical and socio-technical systems because of their role in improving uncertainty management, accommodating multiple stakeholders, and increasing scalability and evolvability. This departure from monolithic architectures provides a system with more flexibility and robustness in response to uncertainties that it may confront during its lifetime. Distributed architecture does not provide benefits only, as it can increase cost a...

  3. Monolithic GaAs surface acoustic wave chemical microsensor array

    Energy Technology Data Exchange (ETDEWEB)

    HIETALA,VINCENT M.; CASALNUOVO,STEPHEN A.; HELLER,EDWIN J.; WENDT,JOEL R.; FRYE-MASON,GREGORY CHARLES; BACA,ALBERT G.

    2000-03-09

    A four-channel surface acoustic wave (SAW) chemical sensor array with associated RF electronics is monolithically integrated onto one GaAs IC. The sensor operates at 690 MHz from an on-chip SAW based oscillator and provides simple DC voltage outputs by using integrated phase detectors. This sensor array represents a significant advance in microsensor technology offering miniaturization, increased chemical selectivity, simplified system assembly, improved sensitivity, and inherent temperature compensation.

  4. Extended Leach Testing of Simulated LAW Cast Stone Monoliths

    Energy Technology Data Exchange (ETDEWEB)

    Serne, R. Jeffrey [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Lanigan, David C. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Westsik, Joseph H. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Williams, Benjamin D. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Jung, H. B. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Wang, Guohui [Pacific Northwest National Lab. (PNNL), Richland, WA (United States)

    2016-08-12

    This revision to the original report adds two longer term leach sets of data to the report and provides more discussion and graphics on how to interpret the results from long-term laboratory leach tests. The leach tests were performed at Pacific Northwest National Laboratory (PNNL) for Washington River Protection Solutions (WRPS) to evaluate the release of key constituents from monoliths of Cast Stone prepared with four simulated low-activity waste (LAW) liquid waste streams.

  5. Cholesterol-imprinted macroporous monoliths: Preparation and characterization.

    Science.gov (United States)

    Stepanova, Mariia А; Kinziabulatova, Lilia R; Nikitina, Anna A; Korzhikova-Vlakh, Evgenia G; Tennikova, Tatiana B

    2017-11-01

    The development of sorbents for selective binding of cholesterol, which is a risk factor for cardiovascular disease, has a great importance for analytical science and medicine. In this work, two series of macroporous cholesterol-imprinted monolithic sorbents differing in the composition of functional monomers (methacrylic acid, butyl methacrylate, 2-hydroxyethyl methacrylate and ethylene dimethacrylate), amount of a template (4, 6 and 8 mol%) used for molecular imprinting, as well as mean pore size were synthesized by in situ free-radical process in stainless steel housing of 50 mm × 4.6 mm i.d. All prepared materials were characterized regarding to their hydrodynamic permeability and porous properties, as well as examined by BET and SEM methods. Imprinting factors, apparent dynamic dissociation constants, the maximum binding capacity, the number of theoretical plates and the height equivalent to a theoretical palate of MIP monoliths at different mobile phase flow rates were determined. The separation of a mixture of structural analogues, namely, cholesterol and prednisolone, was demonstrated. Additionally, the possibility of using the developed monoliths for cholesterol solid-phase extraction from simulated biological solution was shown. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Monolithic pixels on moderate resistivity substrate and sparsifying readout architecture

    International Nuclear Information System (INIS)

    Giubilato, P.; Battaglia, M.; Bisello, D.; Caselle, M.; Chalmet, P.; Demaria, L.; Ikemoto, Y.; Kloukinas, K.; Mansuy, S.C.; Mattiazzo, S.; Marchioro, A.; Mugnier, H.; Pantano, D.; Potenza, A.; Rivetti, A.; Rousset, J.; Silvestrin, L.; Snoeys, W.

    2013-01-01

    The LePix projects aim realizing a new generation monolithic pixel detectors with improved performances at lesser cost with respect to both current state of the art monolithic and hybrid pixel sensors. The detector is built in a 90 nm CMOS process on a substrate of moderate resistivity. This allows charge collection by drift while maintaining the other advantages usually offered by MAPS, like having a single piece detector and using a standard CMOS production line. The collection by drift mechanism, coupled to the low capacitance design of the collecting node made possible by the monolithic approach, provides an excellent signal to noise ratio straight at the pixel cell together with a radiation tolerance far superior to conventional un-depleted MAPS. The excellent signal-to-noise performance is demonstrated by the device ability to separate the 6 keV 55 Fe double peak at room temperature. To achieve high granularity (10–20 µm pitch pixels) over large detector areas maintaining high readout speed, a completely new compressing architecture has been devised. This architecture departs from the mainstream hybrid pixel sparsification approach, which uses in-pixel logic to reduce data, by using topological compression to minimize pixel area and power consumption

  7. Monolithic pixels on moderate resistivity substrate and sparsifying readout architecture

    CERN Document Server

    Giubilato, P; Snoeys, W; Bisello, D; Marchioro, A; Battaglia, M; Demaria, L; Mansuy, S C; Pantano, D; Rousset, J; Mattiazzo, S; Kloukinas, K; Potenza, A; Ikemoto, Y; Rivetti, A; Chalmet, P; Mugnier, H; Silvestrin, L

    2013-01-01

    The LePix projects aim realizing a new generation monolithic pixel detectors with improved performances at lesser cost with respect to both current state of the art monolithic and hybrid pixel sensors. The detector is built in a 90 nm CMOS process on a substrate of moderate resistivity. This allows charge collection by drift while maintaining the other advantages usually offered by MAPS, like having a single piece detector and using a standard CMOS production line. The collection by drift mechanism, coupled to the low capacitance design of the collecting node made possible by the monolithic approach, provides an excellent signal to noise ratio straight at the pixel cell together with a radiation tolerance far superior to conventional un-depleted MAPS. The excellent signal-to-noise performance is demonstrated by the device ability to separate the 6 keV Fe-55 double peak at room temperature. To achieve high granularity (10-20 mu m pitch pixels) over large detector areas maintaining high readout speed, a complet...

  8. Effect of cements on fracture resistance of monolithic zirconia crowns

    Science.gov (United States)

    Nakamura, Keisuke; Mouhat, Mathieu; Nergård, John Magnus; Lægreid, Solveig Jenssen; Kanno, Taro; Milleding, Percy; Örtengren, Ulf

    2016-01-01

    Abstract Objectives The present study investigated the effect of cements on fracture resistance of monolithic zirconia crowns in relation to their compressive strength. Materials and methods Four different cements were tested: zinc phosphate cement (ZPC), glass-ionomer cement (GIC), self-adhesive resin-based cement (SRC) and resin-based cement (RC). RC was used in both dual cure mode (RC-D) and chemical cure mode (RC-C). First, the compressive strength of each cement was tested according to a standard (ISO 9917-1:2004). Second, load-to-failure test was performed to analyze the crown fracture resistance. CAD/CAM-produced monolithic zirconia crowns with a minimal thickness of 0.5 mm were prepared and cemented to dies with each cement. The crown–die samples were loaded until fracture. Results The compressive strength of SRC, RC-D and RC-C was significantly higher than those of ZPC and GIC (p crown between the groups. Conclusion The values achieved in the load-to-failure test suggest that monolithic zirconia crowns with a minimal thickness of 0.5 mm may have good resistance against fracture regardless of types of cements. PMID:27335900

  9. A Ferrite LTCC-Based Monolithic SIW Phased Antenna Array

    KAUST Repository

    Nafe, Ahmed

    2016-11-17

    In this work, we present a novel configuration for realizing monolithic SIW-based phased antenna arrays using Ferrite LTCC technology. Unlike the current common schemes for realizing SIW phased arrays that rely on surface-mount component (p-i-n diodes, etc) for controlling the phase of the individual antenna elements, here the phase is tuned by biasing of the ferrite filling of the SIW. This approach eliminates the need for mounting of any additional RF components and enables seamless monolithic integration of phase shifters and antennas in SIW technology. As a proof of concept, a two-element slotted SIW-based phased array is designed, fabricated and measured. The prototype exhibits a gain of 4.9 dBi at 13.2 GHz and a maximum E-plane beam-scanning of 28 degrees using external windings for biasing the phase shifters. Moreover, the array can achieve a maximum beam-scanning of 19 degrees when biased with small windings that are embedded in the package. This demonstration marks the first time a fully monolithic SIW-based phased array is realized in Ferrite LTCC technology and paves the way for future larger-size implementations.

  10. Modeling of column apparatus processes

    CERN Document Server

    Boyadjiev, Christo; Boyadjiev, Boyan; Popova-Krumova, Petya

    2016-01-01

    This book presents a new approach for the modeling of chemical and interphase mass transfer processes in industrial column apparatuses, using convection-diffusion and average-concentration models. The convection-diffusion type models are used for a qualitative analysis of the processes and to assess the main, small and slight physical effects, and then reject the slight effects. As a result, the process mechanism can be identified. It also introduces average concentration models for quantitative analysis, which use the average values of the velocity and concentration over the cross-sectional area of the column. The new models are used to analyze different processes (simple and complex chemical reactions, absorption, adsorption and catalytic reactions), and make it possible to model the processes of gas purification with sulfur dioxide, which form the basis of several patents.

  11. Photoinitiated grafting of porous polymer monoliths and thermoplastic polymers for microfluidic devices

    Science.gov (United States)

    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.

  12. Application of Monolithic Zirconia Ceramics in Dental Practice: A Case History Report.

    Science.gov (United States)

    Kim, Hee-Kyung; Kim, Sung-Hun; Lee, Jai-Bong; Han, Jung-Suk; Yeo, In-Sung

    2016-01-01

    Monolithic zirconia restorations increasingly have been used in dental practice in recent years and demonstrate superior mechanical performance compared with porcelain-veneered zirconia restorations. Recent advances in manufacturing technology have made possible the fabrication of translucent monolithic zirconia ceramics. This case report describes three clinical examples of monolithic zirconia fixed dental prostheses being used in the anterior and posterior regions and exhibiting acceptable esthetic results.

  13. Voltage-assisted capillary LC of peptides using monolithic capillary columns prepared by ring-opening metathesis polymerization

    Czech Academy of Sciences Publication Activity Database

    Sedláková, Pavla; Mikšík, Ivan; Gatschelhofer, Ch.; Sinner, F. M.; Buchmeiser, M. R.

    2007-01-01

    Roč. 28, č. 13 (2007), s. 2219-2222 ISSN 0173-0835 R&D Projects: GA ČR GA203/05/2539; GA ČR GA203/06/1044; GA MŠk(CZ) 1M0510 Institutional research plan: CEZ:AV0Z50110509 Keywords : ROMP * voltage-assisted capillary LC Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.609, year: 2007

  14. Development of the trigger algorithm for the MONOLITH experiment

    International Nuclear Information System (INIS)

    Gutsche, O.

    2001-05-01

    The MONOLITH project is proposed to prove atmospheric neutrino oscillations and to improve the corresponding measurements of Super-Kamiokande. The MONOLITH detector consists of a massive (34 kt) magnetized iron tracking calorimeter and is optimized for muon neutrino detection. This diploma thesis presents the development of the trigger algorithm for the MONOLITH experiment and related test measurements. Chapter two gives an introduction to the mechanism of neutrino oscillations. The two flavor approximation and the three flavor mechanism are described and influences of matter on neutrino oscillations are discussed. The principles of neutrino oscillation experiments are discussed and the results of Super-Kamiokande, a neutrino oscillation experiment, are presented. Super-Kamiokande gave the strongest indications for atmospheric neutrino oscillations so far. The third chapter introduces the MONOLITH project in the context of atmospheric neutrino oscillations. The MONOLITH detector is described and the main active component, the glass spark chamber, is presented. Chapter four presents the practical part of this thesis. A test setup of a glass spark chamber is built up including a cosmics trigger and a data acquisition system. Cosmic ray muons are used for the investigation of the chamber. During a long term test, the stability of the efficiency and the noise rate of the chamber are investigated. A status report of the results is given. The results are taken as input for the trigger development. In chapter five, the development of the trigger algorithm is presented. In the beginning, the structural design of the trigger algorithm is described. The efficiency and the rate of the trigger algorithm are investigated using two event sources, a Monte Carlo neutrino event sample and a generated noise sample. For the analysis, the data sources are processed by several processing stages which are visualized by corresponding event displays. In the course of the data processing

  15. Temperature programmable microfabricated gas chromatography column

    Science.gov (United States)

    Manginell, Ronald P.; Frye-Mason, Gregory C.

    2003-12-23

    A temperature programmable microfabricated gas chromatography column enables more efficient chemical separation of chemical analytes in a gas mixture by the integration of a resistive heating element and temperature sensing on the microfabricated column. Additionally, means are provided to thermally isolate the heated column from their surroundings. The small heat capacity and thermal isolation of the microfabricated column improves the thermal time response and power consumption, both important factors for portable microanalytical systems.

  16. 29 CFR 1926.755 - Column anchorage.

    Science.gov (United States)

    2010-07-01

    ... 29 Labor 8 2010-07-01 2010-07-01 false Column anchorage. 1926.755 Section 1926.755 Labor... (CONTINUED) SAFETY AND HEALTH REGULATIONS FOR CONSTRUCTION Steel Erection § 1926.755 Column anchorage. (a) General requirements for erection stability. (1) All columns shall be anchored by a minimum of 4 anchor...

  17. Axisymmetric collapses of granular columns

    Science.gov (United States)

    Lube, Gert; Huppert, Herbert E.; Sparks, R. Stephen J.; Hallworth, Mark A.

    2004-06-01

    Experimental observations of the collapse of initially vertical columns of small grains are presented. The experiments were performed mainly with dry grains of salt or sand, with some additional experiments using couscous, sugar or rice. Some of the experimental flows were analysed using high-speed video. There are three different flow regimes, dependent on the value of the aspect ratio a {=} h_i/r_i, where h_i and r_i are the initial height and radius of the granular column respectively. The differing forms of flow behaviour are described for each regime. In all cases a central, conically sided region of angle approximately 59(°) , corresponding to an aspect ratio of 1.7, remains undisturbed throughout the motion. The main experimental results for the final extent of the deposit and the time for emplacement are systematically collapsed in a quantitative way independent of any friction coefficients. Along with the kinematic data for the rate of spread of the front of the collapsing column, this is interpreted as indicating that frictional effects between individual grains in the bulk of the moving flow only play a role in the last instant of the flow, as it comes to an abrupt halt. For a {reach r_infty is given by t_infty {=} 3(h_i/g)(1/2} {=} 3(r_i/g)({1/2}a^{1/2)) , where g is the gravitational acceleration. The insights and conclusions gained from these experiments can be applied to a wide range of industrial and natural flows of concentrated particles. For example, the observation of the rapid deposition of the grains can help explain details of the emplacement of pyroclastic flows resulting from the explosive eruption of volcanoes.

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

    Science.gov (United States)

    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.

  19. Experimental Investigation for Behavior of Reinforced Hybrid Concrete Corbel-Column System Subjected to Un-Symmetrical Vertical Loading

    Directory of Open Access Journals (Sweden)

    Yasir Ali

    2017-05-01

    Full Text Available In this paper, shear and flexural behavior of reinforced hybrid concrete corbel-column system was experimentally investigated. Fourteen hybrid and homogenous concrete corbel-column systemssubjected to un-symmetrical loading were constructed and tested within two test groups (A, B. The experimental program included several variables such as: type of hybrid concrete;high strength concrete(HSC or steel fiber reinforced concrete(SFRC, shear span to depth ratio (a/d, area of hybridization in corbel - column system.Experimental results showed significant effects of concrete hybridization on structural shear and flexural behavior including: ultimate strength, cracking loads, cracking patterns, failure modes, and ductility. Hybridization process ingroup (A included casting the corbel with HSC or SFRC instated of normal strength concrete (NSC. In shear behavior corbels (a/d= 0.37, this process led to increase the shear capacity of corbel by (26%, 38% and shear cracking loads by (20%, 120% respectively. Furthermore, in flexural behavior corbels (a/d= 0.74 shear capacity increased by (19%, 42%, flexural cracking loads increased by (29%, 143% for HSC and SFRC corbels respectively. In group (B hybridization process included increasing the hybrid area of corbel-column system in group (A to represent a distributed region (D-region or decreasing it to represent hybrid corbel. In both cases shear capacity of corbel increased with a range of (10 to 41 % for specimens hybridized monolithically with HSC, while it increased with a range of (19 to 44 % for specimens hybridized monolithically with SFRC; compared with homogenous NSC specimens having same (a/d ratio.

  20. Alumina column Rb-82 generator

    International Nuclear Information System (INIS)

    Yano, Y.; Roth, E.P.

    1977-10-01

    The use of an alumina column for the adsorption of radioactive Sr for the generator production of 75-sec 82 Rb was evaluated in both batches and column experiments using 85 Sr and cyclotron-produced 82 Sr. Comparisons of alumina, Bio-Rex 70 and Chelex 100 ion exchangers were made to determine Sr adsorption, 82 Rb elution yield and Sr breakthrough. The adsorption of Sr is similar for alumina and Chelex 100 but different for Bio-Rex 70. Alumina and Chelex 100 exhibit a small fraction of poorly bound Sr which appears as higher breakthrough in the early elution volumes. The remaining Sr activity is strongly bound to these ion exchangers and the breakthrough remains stable at a lower breakthrough value through a large number of elutions. Bio-Rex 70 on the other hand does not exhibit the poorly bound Sr fraction and the breakthrough of Sr remains the lowest of the three ion exchangers through a moderate number of elutions and then the Sr breakthrough gradually increases with each additional elution

  1. 10Gbps monolithic silicon FTTH transceiver for PON

    Science.gov (United States)

    Zhang, J.; Liow, T. Y.; Lo, G. Q.; Kwong, D. L.

    2010-05-01

    We propose a new passive optical network (PON) configuration and a novel silicon photonic transceiver architecture for optical network unit (ONU), eliminating the need for an internal laser source in ONU. We adopt dual fiber network configuration. The internal light source in each of the ONUs is eliminated. Instead, an extra seed laser source in the optical line termination (OLT) operates in continuous wave mode to serve the ONUs in the PON as a shared and centralized laser source. λ1 from OLT Tx and λ2 from the seed laser are combined by using a WDM combiner and connected to serve the multiple ONUs through the downstream fibers. The ONUs receive the data in λ1. Meanwhile, the ONUs encode and transmit data in λ2, which are sent back to OLT. The monolithic ONU transceiver contains a wavelength-division-multiplexing (WDM) filter component, a silicon modulator and a Ge photo-detector. The WDM in ONU selectively guides λ1 to the Ge-PD where the data in λ1 are detected and converted to electrical signals, and λ2 to the transmitter where the light is modulated by upstream data. The modulated optical signals in λ2 from ONUs are connected back to OLT through upstream fibers. The monolithic ONU transceiver chip size is only 2mm by 4mm. The crosstalk between the Tx and Rx is measured to be less than -20dB. The transceiver chip is integrated on a SFP+ transceiver board. Both Tx and Rx demonstrated data rate capabilities of up to 10Gbps. By implementing this scheme, the ONU transceiver size can be significantly reduced and the assembly processes will be greatly simplified. The results demonstrate the feasibility of mass manufacturing monolithic silicon ONU transceivers via low cost

  2. Monolithic junction field-effect transistor charge preamplifier for calorimetry at high luminosity hadron colliders

    International Nuclear Information System (INIS)

    Radeka, V.; Rescia, S.; Rehn, L.A.; Manfredi, P.F.; Speziali, V.

    1991-11-01

    The outstanding noise and radiation hardness characteristics of epitaxial-channel junction field-effect transistors (JFET) suggest that a monolithic preamplifier based upon them may be able to meet the strict specifications for calorimetry at high luminosity colliders. Results obtained so far with a buried layer planar technology, among them an entire monolithic charge-sensitive preamplifier, are described

  3. On-line immunoaffinity column-liquid chromatography-tandem mass spectrometry method for trace analysis of diuron in wastewater treatment plant effluent sample.

    Science.gov (United States)

    Zhang, Xiuli; Martens, Dieter; Krämer, Petra M; Kettrup, Antonius A; Liang, Xinmiao

    2006-11-10

    An on-line immunoaffinity column with liquid chromatography/tandem mass spectrometry (IAC-LC-MS/MS) method for the determination of diuron in water matrices was described. This method used a sol-gel immunoaffinity column (20 mm x 4 mm I.D.) for on-line sample cleanup and enrichment, a monolithic analytical column (100 mm x 4.6 mm I.D.) for separation, and a triple quadrupole mass spectrometer for quantitation. The major challenges for the on-line set-up were discussed. The optimized on-line protocol was emphasized by the fact that low limit of quantitation (LOQ) of 1.0 ng/L was achieved with only 2.5-mL sample. In addition, a satisfactory accuracy ( approximately 90% of recovery) and precision (effect, the on-line IAC-LC-MS/MS analysis method can reliably determine diuron in wastewater treatment plant effluent sample.

  4. Monolithic Gyroidal Mesoporous Mixed Titanium–Niobium Nitrides

    Science.gov (United States)

    2015-01-01

    Mesoporous transition metal nitrides are interesting materials for energy conversion and storage applications due to their conductivity and durability. We present ordered mixed titanium–niobium (8:2, 1:1) nitrides with gyroidal network structures synthesized from triblock terpolymer structure-directed mixed oxides. The materials retain both macroscopic integrity and mesoscale ordering despite heat treatment up to 600 °C, without a rigid carbon framework as a support. Furthermore, the gyroidal lattice parameters were varied by changing polymer molar mass. This synthesis strategy may prove useful in generating a variety of monolithic ordered mesoporous mixed oxides and nitrides for electrode and catalyst materials. PMID:25122534

  5. Inherent polarization entanglement generated from a monolithic semiconductor chip

    DEFF Research Database (Denmark)

    Horn, Rolf T.; Kolenderski, Piotr; Kang, Dongpeng

    2013-01-01

    Creating miniature chip scale implementations of optical quantum information protocols is a dream for many in the quantum optics community. This is largely because of the promise of stability and scalability. Here we present a monolithically integratable chip architecture upon which is built...... a photonic device primitive called a Bragg reflection waveguide (BRW). Implemented in gallium arsenide, we show that, via the process of spontaneous parametric down conversion, the BRW is capable of directly producing polarization entangled photons without additional path difference compensation, spectral...... as a serious contender on which to build large scale implementations of optical quantum processing devices....

  6. A monolithic (Si) massively broadband non-reverberant monopole

    International Nuclear Information System (INIS)

    Vilches, Antonio; Michelakis, Kostis; Toumazou, Chris; Hand, Jeff

    2008-01-01

    A novel monolithic implementation of a Wu–King profiled antenna intended for use in critical time-domain/UWB/imaging applications is presented. The simulated device was fabricated on a high-resistivity Si substrate on top of which a layer of GaAs is grown, segmented and patterned to serve as the radiating element. The device's measured return loss indicates a −10 dB BW > 50 GHz and time-domain measurements using a 500 pS input pulse prove that the device is practically non-reverberant in air

  7. Development and characterization of monolithic multilayer Laue lens nanofocusing optics

    Energy Technology Data Exchange (ETDEWEB)

    Nazaretski, E.; Xu, W., E-mail: weihexu@bnl.gov; Bouet, N.; Zhou, J.; Yan, H.; Huang, X.; Chu, Y. S. [Brookhaven National Laboratory, Upton, New York 11973 (United States)

    2016-06-27

    We have developed an experimental approach to bond two independent linear Multilayer Laue Lenses (MLLs) together. A monolithic MLL structure was characterized using ptychography at 12 keV photon energy, and we demonstrated 12 nm and 24 nm focusing in horizontal and vertical directions, respectively. Fabrication of 2D MLL optics allows installation of these focusing elements in more conventional microscopes suitable for x-ray imaging using zone plates, and opens easier access to 2D imaging with high spatial resolution in the hard x-ray regime.

  8. Development and characterization of monolithic multilayer Laue lens nanofocusing optics

    Energy Technology Data Exchange (ETDEWEB)

    Nazaretski, E.; Xu, W.; Bouet, N.; Zhou, J.; Yan, H.; Huang, X.; Chu, Y. S.

    2016-06-27

    We have developed an experimental approach to bond two independent linear Multilayer Laue Lenses (MLLs) together. A monolithic MLL structure was characterized using ptychography at 12 keV photon energy, and we demonstrated 12 nm and 24 nm focusing in horizontal and vertical directions, respectively. Fabrication of 2D MLL optics allows installation of these focusing elements in more conventional microscopes suitable for x-ray imaging using zone plates, and opens easier access to 2D imaging with high spatial resolution in the hard x-ray regime.

  9. Photodetectors and monolithic optical receivers in silicon technologies

    Science.gov (United States)

    Schaub, Jeremy Daniel

    Long-distance, high-performance optical data links operate at 1.55mum to take advantage of the low loss of optical fibers at this wavelength. Shorter distance optical links can be implemented at wavelengths near 850nm to take advantage of low-cost optical devices based on GaAs technology. Since silicon (Si) also detects light at this wavelength, it is possible to use Si-based receivers to further reduce costs and to benefit from the advanced manufacturability and proven reliability of Si technology. In this dissertation, I discuss the design, fabrication and performance characteristics of Si-based photodetectors and monolithically integrated optical receivers. This discussion includes a description of a resonant-cavity-enhanced p-i-n photodiode grown using a selective epitaxial growth technique. The device demonstrated peak quantum efficiencies of 42% at 704nm and 31% at 830nm and a bandwidth exceeding 34GHz at -5V. This is the highest speed reported for a Si p-i-n photodiode and the highest bandwidth-efficiency product for any Si-based photodetector. Two monolithically integrated photoreceivers are also described. The first, a lateral p-i-n photodiode integrated with an NMOS transimpedance amplifier on a high-resistivity Si substrate, achieved a bit error ratio of 10-9 at an incident optical power of -31.8dBm at 622Mb/s and -23.2dBm at 1.0Gb/s. This is the highest reported sensitivity of any Si-based monolithic photoreceiver at these data rates. The slow response of the photodiode, which required a -30V bias, limited the overall speed of the receiver. A similar receiver was fabricated on a 3.0mum-thick silicon-on-insulator (SOI) substrate to improve the speed and lower the operating voltage of the photodiode. This receiver demonstrated a maximum operating speed of 2.0Gb/s with a sensitivity of -12.2dBm. This is the fastest speed reported for a monolithic Si receiver in MOS technology. The sensitivities at 622Mb/s and 1.0Gb/s were -26.2dBm and -20.3d

  10. Evaluation of Packed Distillation Columns I - Atmospheric Pressure

    National Research Council Canada - National Science Library

    Reynolds, Thaine

    1951-01-01

    .... Four column-packing combinations of the glass columns and four column-packing combinations of the steel columns were investigated at atmospheric pressure using a test mixture of methylcyclohexane...

  11. Oscillating water column structural model

    Energy Technology Data Exchange (ETDEWEB)

    Copeland, Guild [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States); Bull, Diana L [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States); Jepsen, Richard Alan [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States); Gordon, Margaret Ellen [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)

    2014-09-01

    An oscillating water column (OWC) wave energy converter is a structure with an opening to the ocean below the free surface, i.e. a structure with a moonpool. Two structural models for a non-axisymmetric terminator design OWC, the Backward Bent Duct Buoy (BBDB) are discussed in this report. The results of this structural model design study are intended to inform experiments and modeling underway in support of the U.S. Department of Energy (DOE) initiated Reference Model Project (RMP). A detailed design developed by Re Vision Consulting used stiffeners and girders to stabilize the structure against the hydrostatic loads experienced by a BBDB device. Additional support plates were added to this structure to account for loads arising from the mooring line attachment points. A simplified structure was designed in a modular fashion. This simplified design allows easy alterations to the buoyancy chambers and uncomplicated analysis of resulting changes in buoyancy.

  12. Less common applications of monoliths: V. Monolithic scaffolds modified with nanostructures for chromatographic separations and tissue engineering

    Czech Academy of Sciences Publication Activity Database

    Křenková, Jana; Foret, František; Švec, F.

    2012-01-01

    Roč. 35, 10-11 (2012), s. 1266-1283 ISSN 1615-9306 R&D Projects: GA ČR(CZ) GBP206/12/G014; GA ČR(CZ) GAP301/11/2055 Grant - others:Jihomoravský kraj(CZ) 2SGA2721 Program:2SGA Institutional research plan: CEZ:AV0Z40310501 Keywords : nanoparticles * monoliths * separation Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 2.591, year: 2012 http://onlinelibrary.wiley.com/doi/10.1002/jssc.201100956/pdf

  13. The preparation method of terahertz monolithic integrated device

    Science.gov (United States)

    Zhang, Cong; Su, Bo; He, Jingsuo; Zhang, Hongfei; Wu, Yaxiong; Zhang, Shengbo; Zhang, Cunlin

    2018-01-01

    The terahertz monolithic integrated device is to integrate the pumping area of the terahertz generation, the detection area of the terahertz receiving and the metal waveguide of terahertz transmission on the same substrate. The terahertz generation and detection device use a photoconductive antenna structure the metal waveguide use a microstrip line structure. The evanescent terahertz-bandwidth electric field extending above the terahertz transmission line interacts with, and is modified by, overlaid dielectric samples, thus enabling the characteristic vibrational absorption resonances in the sample to be probed. In this device structure, since the semiconductor substrate of the photoconductive antenna is located between the strip conductor and the dielectric layer of the microstrip line, and the semiconductor substrate cannot grow on the dielectric layer directly. So how to prepare the semiconductor substrate of the photoconductive antenna and how to bond the semiconductor substrate to the dielectric layer of the microstrip line is a key step in the terahertz monolithic integrated device. In order to solve this critical problem, the epitaxial wafer structure of the two semiconductor substrates is given and transferred to the desired substrate by two methods, respectively.

  14. Seismic waves and earthquakes in a global monolithic model

    Science.gov (United States)

    Roubíček, Tomáš

    2018-03-01

    The philosophy that a single "monolithic" model can "asymptotically" replace and couple in a simple elegant way several specialized models relevant on various Earth layers is presented and, in special situations, also rigorously justified. In particular, global seismicity and tectonics is coupled to capture, e.g., (here by a simplified model) ruptures of lithospheric faults generating seismic waves which then propagate through the solid-like mantle and inner core both as shear (S) or pressure (P) waves, while S-waves are suppressed in the fluidic outer core and also in the oceans. The "monolithic-type" models have the capacity to describe all the mentioned features globally in a unified way together with corresponding interfacial conditions implicitly involved, only when scaling its parameters appropriately in different Earth's layers. Coupling of seismic waves with seismic sources due to tectonic events is thus an automatic side effect. The global ansatz is here based, rather for an illustration, only on a relatively simple Jeffreys' viscoelastic damageable material at small strains whose various scaling (limits) can lead to Boger's viscoelastic fluid or even to purely elastic (inviscid) fluid. Self-induced gravity field, Coriolis, centrifugal, and tidal forces are counted in our global model, as well. The rigorous mathematical analysis as far as the existence of solutions, convergence of the mentioned scalings, and energy conservation is briefly presented.

  15. Transferrable monolithic III-nitride photonic circuit for multifunctional optoelectronics

    Science.gov (United States)

    Shi, Zheng; Gao, Xumin; Yuan, Jialei; Zhang, Shuai; Jiang, Yan; Zhang, Fenghua; Jiang, Yuan; Zhu, Hongbo; Wang, Yongjin

    2017-12-01

    A monolithic III-nitride photonic circuit with integrated functionalities was implemented by integrating multiple components with different functions into a single chip. In particular, the III-nitride-on-silicon platform is used as it integrates a transmitter, a waveguide, and a receiver into a suspended III-nitride membrane via a wafer-level procedure. Here, a 0.8-mm-diameter suspended device architecture is directly transferred from silicon to a foreign substrate by mechanically breaking the support beams. The transferred InGaN/GaN multiple-quantum-well diode (MQW-diode) exhibits a turn-on voltage of 2.8 V with a dominant electroluminescence peak at 453 nm. The transmitter and receiver share an identical InGaN/GaN MQW structure, and the integrated photonic circuit inherently works for on-chip power monitoring and in-plane visible light communication. The wire-bonded monolithic photonic circuit on glass experimentally demonstrates in-plane data transmission at 120 Mb/s, paving the way for diverse applications in intelligent displays, in-plane light communication, flexible optical sensors, and wearable III-nitride optoelectronics.

  16. Monolithic Active Pixel Matrix with Binary Counters (MAMBO) ASIC

    International Nuclear Information System (INIS)

    Khalid, Farah F.; Deptuch, Grzegorz; Shenai, Alpana; Yarema, Raymond J.

    2010-01-01

    Monolithic Active Matrix with Binary Counters (MAMBO) is a counting ASIC designed for detecting and measuring low energy X-rays from 6-12 keV. Each pixel contains analogue functionality implemented with a charge preamplifier, CR-RC 2 shaper and a baseline restorer. It also contains a window comparator which can be trimmed by 4 bit DACs to remove systematic offsets. The hits are registered by a 12 bit ripple counter which is reconfigured as a shift register to serially output the data from the entire ASIC. Each pixel can be tested individually. Two diverse approaches have been used to prevent coupling between the detector and electronics in MAMBO III and MAMBO IV. MAMBO III is a 3D ASIC, the bottom ASIC consists of diodes which are connected to the top ASIC using μ-bump bonds. The detector is decoupled from the electronics by physically separating them on two tiers and using several metal layers as a shield. MAMBO IV is a monolithic structure which uses a nested well approach to isolate the detector from the electronics. The ASICs are being fabricated using the SOI 0.2 (micro)m OKI process, MAMBO III is 3D bonded at T-Micro and MAMBO IV nested well structure was developed in collaboration between OKI and Fermilab.

  17. Monolithic Active Pixel Matrix with Binary Counters (MAMBO) ASIC

    Energy Technology Data Exchange (ETDEWEB)

    Khalid, Farah F.; Deptuch, Grzegorz; Shenai, Alpana; Yarema, Raymond J.; /Fermilab

    2010-11-01

    Monolithic Active Matrix with Binary Counters (MAMBO) is a counting ASIC designed for detecting and measuring low energy X-rays from 6-12 keV. Each pixel contains analogue functionality implemented with a charge preamplifier, CR-RC{sup 2} shaper and a baseline restorer. It also contains a window comparator which can be trimmed by 4 bit DACs to remove systematic offsets. The hits are registered by a 12 bit ripple counter which is reconfigured as a shift register to serially output the data from the entire ASIC. Each pixel can be tested individually. Two diverse approaches have been used to prevent coupling between the detector and electronics in MAMBO III and MAMBO IV. MAMBO III is a 3D ASIC, the bottom ASIC consists of diodes which are connected to the top ASIC using {mu}-bump bonds. The detector is decoupled from the electronics by physically separating them on two tiers and using several metal layers as a shield. MAMBO IV is a monolithic structure which uses a nested well approach to isolate the detector from the electronics. The ASICs are being fabricated using the SOI 0.2 {micro}m OKI process, MAMBO III is 3D bonded at T-Micro and MAMBO IV nested well structure was developed in collaboration between OKI and Fermilab.

  18. Monolithically Integrated High-β Nanowire Lasers on Silicon.

    Science.gov (United States)

    Mayer, B; Janker, L; Loitsch, B; Treu, J; Kostenbader, T; Lichtmannecker, S; Reichert, T; Morkötter, S; Kaniber, M; Abstreiter, G; Gies, C; Koblmüller, G; Finley, J J

    2016-01-13

    Reliable technologies for the monolithic integration of lasers onto silicon represent the holy grail for chip-level optical interconnects. In this context, nanowires (NWs) fabricated using III-V semiconductors are of strong interest since they can be grown site-selectively on silicon using conventional epitaxial approaches. Their unique one-dimensional structure and high refractive index naturally facilitate low loss optical waveguiding and optical recirculation in the active NW-core region. However, lasing from NWs on silicon has not been achieved to date, due to the poor modal reflectivity at the NW-silicon interface. We demonstrate how, by inserting a tailored dielectric interlayer at the NW-Si interface, low-threshold single mode lasing can be achieved in vertical-cavity GaAs-AlGaAs core-shell NW lasers on silicon as measured at low temperature. By exploring the output characteristics along a detection direction parallel to the NW-axis, we measure very high spontaneous emission factors comparable to nanocavity lasers (β = 0.2) and achieve ultralow threshold pump energies ≤11 pJ/pulse. Analysis of the input-output characteristics of the NW lasers and the power dependence of the lasing emission line width demonstrate the potential for high pulsation rates ≥250 GHz. Such highly efficient nanolasers grown monolithically on silicon are highly promising for the realization of chip-level optical interconnects.

  19. The market of huge monolithic mirror substrates for optical astronomy

    Science.gov (United States)

    Döhring, Thorsten

    2013-09-01

    Professional astronomical telescopes are complex optical systems at the limit of technical feasibility. Often monolithic primary mirrors and sometimes even secondary mirrors with huge dimensions are used. Prominent examples are the two reflectors of the Large Binocular Telescope and the giant mirrors of VLT, GEMINI, and SUBARU. The performance of such precision optical components significantly depends on the physical parameters and the quality of their substrate materials. Within this paper selection criteria for mirror substrates will be discussed, thereby considering the important technical parameters as well as commercial points and aspects of project management. Qualities and limitations of classical mirror substrate materials like Zerodur, ULE, Sitall, borosilicate glass and Cervit will be evaluated and compared to new substrate materials like silicon carbide and beryllium. The different suppliers and their production processes are presented. In addition large mirrors of existing observatories and of telescopes under construction will be listed, thereby concentrating on mirrors above three meter in diameter. An outlook on material trends and on future astronomical telescopes closes this overview on the market of huge monolithic mirror substrates for optical astronomy.

  20. Monolithically Integrated Flexible Black Phosphorus Complementary Inverter Circuits.

    Science.gov (United States)

    Liu, Yuanda; Ang, Kah-Wee

    2017-07-25

    Two-dimensional (2D) inverters are a fundamental building block for flexible logic circuits which have previously been realized by heterogeneously wiring transistors with two discrete channel materials. Here, we demonstrate a monolithically integrated complementary inverter made using a homogeneous black phosphorus (BP) nanosheet on flexible substrates. The digital logic inverter circuit is demonstrated via effective threshold voltage tuning within a single BP material, which offers both electron and hole dominated conducting channels with nearly symmetric pinch-off and current saturation. Controllable electron concentration is achieved by accurately modulating the aluminum (Al) donor doping, which realizes BP n-FET with a room-temperature on/off ratio >10 3 . Simultaneously, work function engineering is employed to obtain a low Schottky barrier contact electrode that facilities hole injection, thus enhancing the current density of the BP p-FET by 9.4 times. The flexible inverter circuit shows a clear digital logic voltage inversion operation along with a larger-than-unity direct current voltage gain, while exhibits alternating current dynamic signal switching at a record high frequency up to 100 kHz and remarkable electrical stability upon mechanical bending with a radii as small as 4 mm. Our study demonstrates a practical monolithic integration strategy for achieving functional logic circuits on one material platform, paving the way for future high-density flexible electronic applications.

  1. Macroporous monoliths for trace metal extraction from seawater

    Energy Technology Data Exchange (ETDEWEB)

    Yue, Yanfeng; Mayes, Richard; Gill, Gary A.; Kuo, Li-Jung; Wood, Jordana R.; Binder, Andrew; Brown, Suree; Dai, Sheng

    2015-05-29

    The viability of seawater-based uranium recovery depends on the uranium adsorption rate and capacity, since the concentration of uranium in the oceans is relatively low (3.3 μgL⁻¹). An important consideration for a fast adsorption is to maximize the adsorption properties of adsorbents such as surface areas and pore structures, which can greatly improve the kinetics of uranium extraction and the adsorption capacity simultaneously. Following this consideration, macroporous monolith adsorbents were prepared from the copolymerization of acrylonitrile (AN) and N,N’-methylenebis(acrylamide) (MBAAm) based on a cryogel method using both hydrophobic and hydrophilic monomers. The monolithic sorbents were tested with simulated seawater containing a high uranyl concentration (–6 ppm) and the uranium adsorption results showed that the adsorption capacities are strongly influenced by the ratio of monomer to the crosslinker, i.e., the density of the amidoxime groups. The preliminary seawater testing indicates the high salinity content of seawater does not hinder the adsorption of uranium.

  2. Development of stable monolithic wide-field Michelson interferometers.

    Science.gov (United States)

    Wan, Xiaoke; Ge, Jian; Chen, Zhiping

    2011-07-20

    Bulk wide-field Michelson interferometers are very useful for high precision applications in remote sensing and astronomy. A stable monolithic Michelson interferometer is a key element in high precision radial velocity (RV) measurements for extrasolar planets searching and studies. Thermal stress analysis shows that matching coefficients of thermal expansion (CTEs) is a critical requirement for ensuring interferometer stability. This requirement leads to a novel design using BK7 and LAK7 materials, such that the monolithic interferometer is free from thermal distortion. The processes of design, fabrication, and testing of interferometers are described in detail. In performance evaluations, the field angle is typically 23.8° and thermal sensitivity is typically -2.6×10(-6)/°C near 550 nm, which corresponds to ∼800 m/s/°C in the RV scale. Low-cost interferometer products have been commissioned in multiple RV instruments, and they are producing high stability performance over long term operations. © 2011 Optical Society of America

  3. Immobilization of trypsin on sub-micron skeletal polymer monolith

    Energy Technology Data Exchange (ETDEWEB)

    Yao Chunhe [Beijing National Laboratory for Molecular Sciences, Key Laboratory of Analytical Chemistry for Living Biosystems, Institute of Chemistry, Chinese Academy of Sciences, Beijing 100190 (China); Graduate School, Chinese Academy of Sciences, Beijing 100049 (China); Qi Li, E-mail: qili@iccas.ac.cn [Beijing National Laboratory for Molecular Sciences, Key Laboratory of Analytical Chemistry for Living Biosystems, Institute of Chemistry, Chinese Academy of Sciences, Beijing 100190 (China); Hu Wenbin [Beijing National Laboratory for Molecular Sciences, Key Laboratory of Analytical Chemistry for Living Biosystems, Institute of Chemistry, Chinese Academy of Sciences, Beijing 100190 (China); Graduate School, Chinese Academy of Sciences, Beijing 100049 (China); Wang Fuyi [Beijing National Laboratory for Molecular Sciences, Key Laboratory of Analytical Chemistry for Living Biosystems, Institute of Chemistry, Chinese Academy of Sciences, Beijing 100190 (China); Yang Gengliang [College of Pharmacy, Hebei University, Baoding 071002 (China)

    2011-04-29

    A new kind of immobilized trypsin reactor based on sub-micron skeletal polymer monolith has been developed. Covalent immobilization of trypsin on this support was performed using the epoxide functional groups in either a one- or a multi-step reaction. The proteolytic activity of the immobilized trypsin was measured by monitoring the formation of N-{alpha}-benzoyl-L-arginine (BA) which is the digestion product of a substrate N-{alpha}-benzoyl-L-arginine ethyl ester (BAEE). Results showed that the digestion speed was about 300 times faster than that performed in free solution. The performance of such an enzyme reactor was further demonstrated by digesting protein myoglobin. It has been found that the protein digestion could be achieved in 88 s at 30 deg. C, which is comparable to 24 h digestion in solution at 37 {sup o}C. Furthermore, the immobilized trypsin exhibits increased stability even after continuous use compared to that in free solution. The present monolithic enzyme-reactor provides a promising platform for the proteomic research.

  4. REDISTRIBUTOR FOR LIQUID-LIQUID EXTRACTION COLUMNS

    Science.gov (United States)

    Bradley, J.G.

    1957-10-29

    An improved baffle plate construction to intimately mix immiscible liquid solvents for solvent extraction processes in a liquid-liquid pulse column is described. To prevent the light and heavy liquids from forming separate continuous homogeneous vertical channels through sections of the column, a baffle having radially placed rectangular louvers with deflection plates opening upon alternate sides of the baffle is placed in the column, normal to the axis. This improvement substantially completely reduces strippiig losses due to poor mixing.

  5. Structural design of isolated column footings

    Directory of Open Access Journals (Sweden)

    Fathi Abdrabbo

    2016-09-01

    The study showed that shear span to depth ratio of a footing and distributions of contact stress at footing–soil interface are key factors in the structural design of the footing. ECP203-11, ACI318-08, and EC2-2004 code provisions, underestimate the structural failure loads of isolated column footings, while BS 8110.1-1997 overpredicts the failure loads of isolated column footings, if punching provisions at perimeter of column are pulled out from the code.

  6. Thermally stable dexsil-400 glass capillary columns

    International Nuclear Information System (INIS)

    Maskarinec, M.P.; Olerich, G.

    1980-01-01

    The factors affecting efficiency, thermal stability, and reproducibility of Dexsil-400 glass capillary columns for gas chromatography in general, and for polycyclic aromatic hydrocarbons (PAHs) in particular were investigated. Columns were drawn from Kimble KG-6 (soda-lime) glass or Kimox (borosilicate) glass. All silylation was carried out at 200 0 C. Columns were coated according to the static method. Freshly prepared, degassed solutions of Dexsil-400 in pentane or methylene chloride were used. Thermal stability of the Dexsil 400 columns with respect to gas chromatography/mass spectrometry (GC/MS) were tested. Column-to-column variability is a function of each step in the fabrication of the columns. The degree of etching, extent of silylation, and stationary phase film thickness must be carefully controlled. The variability in two Dexsil-400 capillary column prepared by etching, silylation with solution of hexa methyl disilazone (HMDS), and static coating is shown and also indicates the excellent selectivity of Dexsil-400 for the separation of alkylated aromatic compounds. The wide temperature range of Dexsil-400 and the high efficiency of the capillary columns also allow the analysis of complex mixtures with minimal prefractionation. Direct injection of a coal liquefaction product is given. Analysis by GC/MS indicated the presence of parent PAHs, alkylated PAHs, nitrogen and sulfur heterocycles, and their alkylated derivatives. 4 figures

  7. Miniaturized DNA aptamer-based monolithic sorbent for selective extraction of a target analyte coupled on-line to nanoLC.

    Science.gov (United States)

    Brothier, Fabien; Pichon, Valérie

    2014-12-01

    A complete characterization of a novel target-specific DNA aptamer-based miniaturized solid phase extraction (SPE)-sorbent coupled on-line to nanoLC is presented. A miniaturized oligosorbent (mOS) was prepared via the in situ sol-gel synthesis of a hybrid organic-inorganic monolith in 100 μm i.d. capillary columns using tetraethoxysilane and 3-aminopropyltriethoxysilane as precursors, followed by covalent binding of a 5'-amino-modified DNA aptamer with a C12 spacer arm specific for a molecule of small molecular weight. Ochratoxin A (OTA), one of the most abundant naturally occurring mycotoxins, was chosen as model analyte to demonstrate the principle of such an approach. The mOS was coupled on-line to RP-nanoLC-LIF. Selective extraction of OTA on several mOSs was demonstrated with an average extraction recovery above 80 % when percolating spiked binding buffer and a low recovery on control monoliths grafted with a non-specific aptamer. Reproducibility of mOSs preparation was highlighted by comparing extraction yields. Otherwise, the mOSs demonstrated no cross-reactivity towards an OTA structural analogue, i.e., ochratoxin B. Due to the high specific surface area of the hybrid silica-based monolith, the coverage density of DNA aptamers covalently immobilized in the capillaries was very high and reached 6.27 nmol μL(-1), thus leading to a capacity above 5 ng of OTA. This miniaturized device was then applied to the selective extraction of OTA from beer samples. It revealed to be effective in isolating OTA from this complex matrix, thus improving the reliability of its analysis at the trace level.

  8. Development of molecular imprinted column-on line-two dimensional liquid chromatography for selective determination of clenbuterol residues in biological samples.

    Science.gov (United States)

    Guo, Pengqi; Luo, Zhimin; Xu, Xinya; Zhou, Yulan; Zhang, Bilin; Chang, Ruimiao; Du, Wei; Chang, Chun; Fu, Qiang

    2017-02-15

    A novel method coupling molecular imprinted monolithic column with two-dimensional liquid chromatography was developed and validated for the analysis of clenbuterol in pork liver and swine urine samples. The polymers were characterized by using Fourier transform infrared spectroscopy, nitrogen adsorption desorption analyses, frontal analysis and the adsorption of selectivity. The results indicated that the imprinted columns were well prepared and possessed high selectivity adsorption capacity. Subsequently, the MIMC-2D-LC (molecular imprinted monolithic column-two dimensional liquid chromatography) method was developed for the selective analysis of clenbuterol in practical samples. The accuracy ranged from 94.3% to 99.7% and from 93.7% to 99.6% for liver and urine, respectively. The relative standard deviation (RSD) of repeatability was lower than 8.6% for both analyses. The limit of detections was 16ng·mL(-1) for liver and 25ng·mL(-1) for urine, respectively. Compared with the reported methods, the disturbance of endogenous impurity could be avoided by the 2D-LC method. Copyright © 2016 Elsevier Ltd. All rights reserved.

  9. Nanofiber polymers as novel sorbents for on-line solid phase extraction in chromatographic system: A comparison with monolithic reversed phase C18 sorbent.

    Science.gov (United States)

    Háková, Martina; Havlíková, Lucie Chocholoušová; Chvojka, Jiří; Švec, František; Solich, Petr; Šatínský, Dalibor

    2018-08-14

    A novel application of nanofiber polymers in the wide area of a sample preparation techniques known as solid phase extraction has been studied. We demonstrated application of nanofibers as sorbents for use in a system including on-line extraction coupled with column-switching high performance liquid chromatography. Four types of nanofibers including polyamide 6 with two different surface densities, poly(ε-caprolactone), and polystyrene were tested. We found that three of them were very efficient extraction sorbents sufficiently stable for application in the on-line system. Our results confirmed that the extraction efficiency of the nanofibers depended on the type and chemistry of the spun polymer as well as on the fabrication process of the nanofibrous mats that affected their density, structure, surface density, and mechanical functionality. We also compared performance of all four nanofibers with a conventional monolithic reversed-phase C18 sorbent in terms of extraction efficiency using on-line solid-phase extraction-HPLC system. Polyamide 6 was found to be the best sorbent for lipophilic analytes with a retention and extraction efficiency for the target analytes comparable with that of the C18 monolith. Copyright © 2018 Elsevier B.V. All rights reserved.

  10. PEO-based brush-type amphiphilic macro-RAFT agents and their assembled polyHIPE monolithic structures for applications in separation science.

    Science.gov (United States)

    Khodabandeh, Aminreza; Arrua, R Dario; Mansour, Fotouh R; Thickett, Stuart C; Hilder, Emily F

    2017-08-10

    Polymerized High Internal Phase Emulsions (PolyHIPEs) were prepared using emulsion-templating, stabilized by an amphiphilic diblock copolymer prepared by reversible addition fragmentation chain transfer (RAFT) polymerization. The diblock copolymer consisted of a hydrophilic poly(ethylene glycol) methyl ether acrylate (PEO MA, average Mn 480) segment and a hydrophobic styrene segment, with a trithiocarbonate end-group. These diblock copolymers were the sole emulsifiers used in stabilizing "inverse" (oil-in-water) high internal phase emulsion templates, which upon polymerization resulted in a polyHIPE exhibiting a highly interconnected monolithic structure. The polyHIPEs were characterized by FTIR spectroscopy, BET surface area measurements, SEM, SEM-EDX, and TGA. These materials were subsequently investigated as stationary phase for high-performance liquid chromatography (HPLC) via in situ polymerization in a capillary format as a 'column housing'. Initial separation assessments in reversed-phase (RP) and hydrophilic interaction liquid chromatographic (HILIC) modes have shown that these polyHIPEs are decorated with different microenvironments amongst the voids or domains of the monolithic structure. Chromatographic results suggested the existence of RP/HILIC mixed mode with promising performance for the separation of small molecules.

  11. Sensitive determination of parabens in human urine and serum using methacrylate monoliths and reversed-phase capillary liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Carrasco-Correa, Enrique Javier; Vela-Soria, Fernando; Ballesteros, Oscar; Ramis-Ramos, Guillermo; Herrero-Martínez, José Manuel

    2015-01-30

    A method for the determination of parabens in human urine and serum by capillary liquid chromatography (cLC) with UV-Vis and mass spectrometry (MS) detection using methacrylate ester-based monolithic columns has been developed. The influence of composition of polymerization mixture was studied. The optimum monolith was obtained with butyl methacrylate monomer at 60/40% (wt/wt) butyl methacrylate/ethylene dimethacrylate ratio and 50wt% porogens (composed of 36wt% of 1,4-butanediol, 54wt% 1-propanol and 10wt% water). Baseline resolution of analytes was achieved through a mobile phase of acetonitrile/water in gradient elution mode. Additionally, dispersive liquid-liquid microextraction (DLLME) was combined with both cLC-UV-Vis and cLC-MS to achieve the determination of parabens in human urine and serum samples with very low limits of detection. Satisfactory intra- and inter-day repeatabilities were obtained in UV-Vis and MS detection, although the latter provided lower detection limits (up to 300-fold) than the UV-Vis detection. Recoveries for the target analytes from spiked biological samples ranged from 95.2% to 106.7%. The proposed methodology for the ultra-low determination of parabens in human urine and serum samples is simple and fast, the consumption of reagents is very low, and very small samples can be analyzed. Copyright © 2014 Elsevier B.V. All rights reserved.

  12. Facile preparation of silver nanoparticles homogeneously immobilized in hierarchically monolithic silica using ethylene glycol as reductant.

    Science.gov (United States)

    Yu, Huan; Zhu, Yang; Yang, Hui; Nakanishi, Kazuki; Kanamori, Kazuyoshi; Guo, Xingzhong

    2014-09-07

    A facile and "green" method was proposed to introduce Ag nanoparticles (Ag NPs) into the hierarchically monolithic silica uniformly in the presence of (3-aminopropyl)-triethoxysilane (APTES) and ethylene glycol. APTES is used to modify the monolith by incorporating amino groups onto the surface of meso-macroporous skeletons, while ethylene glycol is employed as the productive reductant. Ag NPs are homogeneously immobilized in hierarchically monolithic silica after reduction and drying at 40 °C for different duration times, and the embedded amount of Ag NPs can reach 15.44 wt% when treated once. The embedment of Ag NPs increases with the repeat treatment and the APTES amount, without uncontrollable crystalline growth. The surface areas of Ag NPs embedded in silica monoliths after heat treatment at 300 and 400 °C are higher than those before heat treatment. The modification via APTES and the embedment of Ag NPs does not spoil the morphology of monolithic silica, while changing the pore structures of the monolith. A tentative formation process and a reduction mechanism are proposed for the modification, reduction and embedment. Ag NPs embedded in monolithic silica is promising for wide applications such as catalysis and separation.

  13. Enthalpy-entropy compensation effect on adsorption of light hydrocarbons on monolithic stationary phases.

    Science.gov (United States)

    Korolev, Alexander A; Shiryaeva, Valeria E; Popova, Tamara P; Kurganov, Alexander A

    2011-08-01

    Enthalpy and entropy of adsorption of light hydrocarbons C1-C4 have been measured for three monoliths of different polarity and for five different carrier gases: helium, hydrogen, nitrogen, carbon dioxide and dinitrogen oxide. Using carrier gas helium the highest values of enthalpy and entropy were observed for monolith based on ethylenedimethacrylate and the lowest values were observed for monolith based on silica, while monolith based on divinylbenzene demonstrated intermediate values. Entropy-enthalpy correlations were observed with carrier gas helium for all thee monoliths and possess similar slope indicating similar adsorption mechanism on all monoliths studied. Comparing different carrier gases entropy-enthalpy correlations within a homological series of solutes were observed for light carrier gases (He, H2 and N2) and were not observed for heavy carrier gases (CO2 and N2O). Instead, entropy-enthalpy correlations for heavy carrier gases were observed with pressure as variable and the higher the carrier gas pressure the lower the values of enthalpy and entropy observed. The observed changes in entropy-enthalpy correlations were explained by competitive adsorption of heavy carrier gas on monoliths. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Synthesis and characterization of hierarchically porous metal, metal oxide, and carbon monoliths with highly ordered nanostructure

    Science.gov (United States)

    Grano, Amy Janine

    Hierarchically porous materials are of great interest in such applications as catalysis, separations, fuel cells, and advanced batteries. One such way of producing these materials is through the process of nanocasting, in which a sacrificial template is replicated and then removed to form a monolithic replica. This replica consists of mesopores, which can be ordered or disordered, and bicontinuous macropores, which allow flow throughout the length of the monolith. Hierarchically porous metal oxide and carbon monoliths with an ordered mesopores system are synthesized for the first time via nanocasting. These replicas were used as supports for the deposition of silver particles and the catalytic efficiency was evaluated. The ordered silica template used in producing these monoliths was also used for an in-situ TEM study involving metal nanocasting, and an observation of the destruction of the silica template during nanocasting made. Two new methods of removing the silica template were developed and applied to the synthesis of copper, nickel oxide, and zinc oxide monoliths. Finally, hollow fiber membrane monoliths were examined via x-ray tomography in an attempt to establish the presence of this structure throughout the monolith.

  15. Peculiarities of Thermal Treatment of Monolithic Reinforced Concrete Structures

    Science.gov (United States)

    Kuchin, V. N.; Shilonosova, N. V.

    2017-11-01

    A mathematical program has been developed that allows one to determine the parameters of heat treatment of monolithic structures. One of the quality indicators of monolithic reinforced concrete structures is the level of temperature stresses arising in the process of heat treatment and further operation of structures. In winter at heat treatment the distribution of temperatures along the cross-section of the structure is uneven. A favorable thermo-stressed state in a concrete massif occurs when using the preheating method, providing the concrete temperature in the center of the structure is greater than at the periphery. In this case, after the strength is set and the temperature is later equalized along the cross-section, the central part of the structure tends to decrease its dimensions more but the extreme zones prevent it. Therefore, the center is in a state of tension, and the extreme zones on the periphery are compressed. In compressed concrete there is a lesser chance of cracks or defects. The temperature gradient over the section of the structure, the stress in the concrete and its strength are determined. When calculating the temperature and strength fields, the stress level was determined - a value equal to the ratio of the tensile stresses in the section under consideration to the tensile strength of the concrete in this section at the same time. The nature of the change in stress level is determined by the massive structure and power of the formwork heaters. It is shown that under unfavorable conditions the stress level is close to the critical value. The greatest temperature gradient occurs in the outer layers adjacent to the heating formwork. A technology for concrete conditioning is proposed which makes it possible to reduce the temperature stresses along the cross-section of the structure. The time for concrete conditioning in the formwork is reduced. In its turn, it further reduces labor costs and the cost of concrete work along with the cost of

  16. Gaseous carbon dioxide absorbing column

    International Nuclear Information System (INIS)

    Harashina, Heihachi.

    1994-01-01

    The absorbing column of the present invention comprises a cyclone to which CO 2 gas and Ca(OH) 2 are blown to form CaCO 3 , a water supply means connected to an upper portion of the cyclone for forming a thin water membrane on the inner wall thereof, and a water processing means connected to a lower portion of the cyclone for draining water incorporating CaCO 3 . If a mixed fluid of CO 2 gas and Ca(OH) 2 is blown in a state where a flowing water membrane is formed on the inner wall of the cyclone, formation of CaCO 3 is promoted also in the inside of the cyclone in addition to the formation of CaCO 3 in the course of blowing. Then, formed CaCO 3 is discharged from the lower portion of the cyclone together with downwardly flowing water. With such procedures, solid contents such as CaCO 3 separated at the inner circumferential wall are sent into the thin water membrane, adsorbed and captured, and the solid contents are successively washed out, so that a phenomenon that the solid contents deposit and grow on the inner wall of the cyclone can be prevented effectively. (T.M.)

  17. Column: Factors Affecting Data Decay

    Directory of Open Access Journals (Sweden)

    Kevin Fairbanks

    2012-06-01

    Full Text Available In nuclear physics, the phrase decay rate is used to denote the rate that atoms and other particles spontaneously decompose. Uranium-235 famously decays into a variety of daughter isotopes including Thorium and Neptunium, which themselves decay to others. Decay rates are widely observed and wildly different depending on many factors, both internal and external. U-235 has a half-life of 703,800,000 years, for example, while free neutrons have a half-life of 611 seconds and neutrons in an atomic nucleus are stable.We posit that data in computer systems also experiences some kind of statistical decay process and thus also has a discernible decay rate. Like atomic decay, data decay fluctuates wildly. But unlike atomic decay, data decay rates are the result of so many different interplaying processes that we currently do not understand them well enough to come up with quantifiable numbers. Nevertheless, we believe that it is useful to discuss some of the factors that impact the data decay rate, for these factors frequently determine whether useful data about a subject can be recovered by forensic investigation.(see PDF for full column

  18. Monolitni katalizatori i reaktori: osnovne značajke, priprava i primjena (Monolith catalysts and reactors: preparation and applications

    Directory of Open Access Journals (Sweden)

    Tomašić, V.

    2004-12-01

    Full Text Available Monolithic (honeycomb catalysts are continuous unitary structures containing many narrow, parallel and usually straight channels (or passages. Catalytically active components are dispersed uniformly over the whole porous ceramic monolith structure (so-called incorporated monolithic catalysts or are in a layer of porous material that is deposited on the walls of channels in the monolith's structure (washcoated monolithic catalysts. The material of the main monolithic construction is not limited to ceramics but includes metals, as well. Monolithic catalysts are commonly used in gas phase catalytic processes, such as treatment of automotive exhaust gases, selective catalytic reduction of nitrogen oxides, catalytic removal of volatile organic compounds from industrial processes, etc. Monoliths continue to be the preferred support for environmental applications due to their high geometric surface area, different design options, low pressure drop, high temperature durability, mechanical strength, ease of orientation in a reactor and effectiveness as a support for a catalytic washcoat. As known, monolithic catalysts belong to the class of the structured catalysts and/or reactors (in some cases the distinction between "catalyst" and "reactor" has vanished. Structured catalysts can greatly intensify chemical processes, resulting in smaller, safer, cleaner and more energy efficient technologies. Monolith reactors can be considered as multifunctional reactors, in which chemical conversion is advantageously integrated with another unit operation, such as separation, heat exchange, a secondary reaction, etc. Finally, structured catalysts and/or reactors appear to be one of the most significant and promising developments in the field of heterogeneous catalysis and chemical engineering of the recent years. This paper gives a description of the background and perspectives for application and development of monolithic materials. Different methods and techniques

  19. Rasch models with exchangeable rows and columns

    DEFF Research Database (Denmark)

    Lauritzen, Steffen Lilholt

    The article studies distributions of doubly infinite binary matrices with exchangeable rows and columns which satify the further property that the probability of any $m \\times n$ submatrix is a function of the row- and column sums of that matrix. We show that any such distribution is a (unique...

  20. The general packed column : an analytical solution

    NARCIS (Netherlands)

    Gielen, J.L.W.

    2000-01-01

    The transient behaviour of a packed column is considered. The column, uniformly packed on a macroscopic scale, is multi-structured on the microscopic level: the solid phase consists of particles, which may differ in incidence, shape or size, and other relevant physical properties. Transport in the