Comparison of twin-cell centrifugal partition chromatographic columns with different cell volume.

PubMed

Goll, Johannes; Audo, Gregoire; Minceva, Mirjana

2015-08-07

Two twin-cell centrifugal partition chromatographic columns (SCPC 250 and SCPE-250-BIO, Armen Instrument, France) with the same column volume but different cell size and number were compared in terms of stationary phase retention and column efficiency. The columns were tested with two types of solvent systems: a commonly used organic solvent based biphasic system from the ARIZONA solvent system family and a polymer/salt based aqueous two phase system (ATPS). The efficiency of the columns was evaluated by pulse injection experiments of two benzenediols (pyrocatechol and hydroquinone) in the case of the ARIZONA system and a protein mixture (myoglobin and lysozyme) in the case of the ATPS. As result of high stationary phase retention, the column with the lower number of larger twin-cells (SCPE-250-BIO) is suitable for protein separations using ATPS. On the other hand, due to higher column efficiency, the column with the greater number of smaller cells (SCPC 250) is superior for batch elution separations performed with standard liquid-liquid chromatography organic solvent based biphasic systems. Copyright © 2015 Elsevier B.V. All rights reserved.

Enhancing Photon Utilization Efficiency for Astaxanthin Production from Haematococcus lacustris Using a Split-Column Photobioreactor.

PubMed

Kim, Z-Hun; Park, Hanwool; Lee, Ho-Sang; Lee, Choul-Gyun

2016-07-28

A split-column photobioreactor (SC-PBR), consisting of two bubble columns with different sizes, was developed to enhance the photon utilization efficiency in an astaxanthin production process from Haematococcus lacustris. Among the two columns, only the smaller column of SC-PBR was illuminated. Astaxanthin productivities and photon efficiencies of the SC-PBRs were compared with a standard bubble-column PBR (BC-PBR). Astaxanthin productivity of SC-PBR was improved by 28%, and the photon utilization efficiencies were 28-366% higher than the original BC-PBR. The results clearly show that the effective light regime of SC-PBR could enhance the production of astaxanthin.

Efficient control system for low-concentration inorganic gases from a process vent stream: application of surfactants in spray and packed columns.

PubMed

Chein, Hungmin; Aggarwal, Shankar G; Wu, Hsin-Hsien

2004-11-01

Control of low-concentration pollutants from a semiconductor process vent stream using a wet-scrubbing technique is a challenging task to meet Taiwan environmental emission standards. An efficient wet-scrubber is designed on a pilot scale and tested to control low concentration acid and base waste-gas emission. The scrubber system consisted of two columns, i.e., a fine spray column [cutoff diameter (based on volume), Dv(50) = 15.63 microm; Sauter mean diameter (SMD) = 7.62 microm], which is especially efficient for NH3 removal as the pH of the spraying liquid is approximately 7 followed by a packed column with a scrubbing liquid pH approximately 9.0 mainly for acids removal. It is observed that use of the surfactants in low concentration about 10(-4) M and 10(-7) M in the spray liquid and in the scrubbing liquid, respectively, remarkably enhances the removal efficiency of the system. A traditional packed column (without the spray column and the surfactant) showed that the removal efficiencies of NH3, HF, and HCl for the inlet concentration range 0.2 to 3 ppm were (n = 5) 22.6+/-3.4%, 43.4+/-5.5%, and 40.4+/-7.4%, respectively. The overall efficiencies of the proposed system (the spray column and the packed column) in the presence of the surfactant in the spray liquid and in the scrubbing liquid forthese three species were found to increase significantly (n = 5) from 60.3+/-3.6 to 82.8+/-6.8%, 59.1+/-2.7 to 83.4+/-4.2%, and 56.2+/-7.3 to 81.0+/-6.7%, respectively. In this work, development of charge on the gas-liquid interface due to the surfactants has been measured and discussed. It is concluded that the presence of charge on the gas-liquid interface is the responsible factor for enhancement of the removal efficiency (mass-transfer in liquid phase). The effects of the type of surfactants, their chain length, concentration in liquid, etc. on the removal efficiency are discussed. Since the pilot tests were performed under the operating conditions similar to most of the wet-scrubbers operated in semiconductors manufacturing facilities for inorganic pollutants, this study can be applied to modify the existing wet-scrubbers to enhance the removal efficiencies, especially for low-concentration pollutants.

Innovation of Iron Reinforcing Column of Partical From Frame of Light Steel

NASA Astrophysics Data System (ADS)

Ramadhan, M. R.; Faslih, A.; Umar, M. Z.

2018-05-01

Almost half of houses in Indonesia are using lightweight steel roof truss today. The phenomenon in the field is that lightweight steel roof truss can blend with mortar mixture. Thus this phenomenon is captured for later applied dynamically, creatively, and innovatively with new idioms such as reinforcement for columns. This research aims to investigate the comparison of the way of making and the price of the materials between the column material made of the light steel and the column material made of the iron reinforcement which is the most efficient. Type of research is qualitative with a comparative causal approach. This research is divided into several stages, namely; Literature study, column creation, and validation. This study concluds that the manufacture of column material from reinforcement is more efficient, than the lightweight steel column material. The reinforcement column material is more efficient because of the more effective way of making and the price of the working materials more economical than the lightweight steel column material. Lightweight steel columns can be used for public housing on condition made by experienced craftsmen to make the process faster, and the dimensions of lightweight steel can be scaled down to make it more economical.

Combination of COFRADIC and high temperature-extended column length conventional liquid chromatography: a very efficient way to tackle complex protein samples, such as serum.

PubMed

Sandra, Koen; Verleysen, Katleen; Labeur, Christine; Vanneste, Lies; D'Hondt, Filip; Thomas, Grégoire; Kas, Koen; Gevaert, Kris; Vandekerckhove, Joël; Sandra, Pat

2007-03-01

The previously reported COmbined FRActional DIagonal Chromatography (COFRA-DIC) methodology, in which a subset of peptides representative for their parent proteins are sorted, is particularly powerful for whole proteome analysis. This peptide-centric technology is built around diagonal chromatography, where peptide separations are crucial. This paper presents high efficiency peptide separations, in which four 250 x 2.1 mm, 5 microm Zorbax 300SB-C18 columns (total length 1 m) were coupled at operating temperatures of 60'C using a dedicated LC oven and conventional LC equipment. The high efficiency separations were combined with the COFRADIC procedure. This extremely powerful combination resulted, for the analysis of serum, in an increase in the uniquely identified peptide sequences by a factor of 2.6, compared to the COFRADIC procedure on a 25 cm column. This is a reflection of the increased peak capacity obtained on the 1 m column, which was calculated to be a factor 2.7 higher than on the 25 cm column. Besides more efficient sorting, less ion suppression was noticed.

Influence of mass transfer on the ozonation of wastewater from the glass fiber industry.

PubMed

Byun, S; Cho, S H; Yoon, J; Geissen, S U; Vogelpohl, A; Kim, S M

2004-01-01

The mass transfer rate (kLa) is one of the most important parameters in the ozonation of wastewater, because it frequently constitutes the rate-determining step. This study investigated the influence of kLa on the ozonation of glass fiber wastewater using a high-performance jet loop reactor (HJLR), which is well known for its high mass transfer property, and compared the results of this investigation with those obtained using the bubble column reactor. It was found that the higher kLa achieved by increasing the energy input did not lead to higher ozonation efficiency, since the reaction involving the OH radical was greatly hindered at the low pH produced as a result of ozonation. By maintaining the pH at a value greater than 8.0, the higher kLa in the HJLR reactor contributed to increasing not only the TOC removal of wastewater, but also the ozone consumption efficiency, as expressed by the specific ozone consumption. The specific ozone consumption in the HJLR reactor (7.1 g ozone/ g TOC) was 20% better than that in the bubble column reactor.

Particle size distribution and column efficiency. An ongoing debate revived with 1.9μm Titan-C18 particles.

PubMed

Gritti, Fabrice; Bell, David S; Guiochon, Georges

2014-08-15

The mass transfer mechanism in four prototype columns (2.1 and 3.0×50mm, 2.1 and 3.0×100mm) packed with 1.9μm fully porous Titan-C18 particles was investigated by using two previously reported home-made protocols. The first one was used to measure the eddy dispersion HETP of these new columns, the second one to estimate their intrinsic (corrected for HPLC system contribution) HETPs. Titan particles are fully porous particles with a narrow particle size distribution (RSD of 9.2%). The mean Sauter diameter (dSauter=2.04μm) was determined from Coulter counter measurements on the raw silica material (before C18 derivatization) and in the absence of a dispersant agent (Triton X-100) in a 2% NaCl electrolyte solution. The results show that these RPLC Titan columns have intrinsic minimum reduced HETPs ranging from 1.7 to 1.9 and generate up to 290,000 plates per meter. The 3.0mm i.d. columns are more efficient than the 2.1mm i.d. ones and short columns are preferred to minimize efficiency losses due to frictional heating at high speeds. This work also revealed that (1) the lowest h values of the Titan columns are observed at low reduced velocities (νopt=5); (2) this is due to the unusually small diffusivity of analytes across the porous Titan-C18 particles; and (3) the Titan columns are not packed more uniformly than conventional columns packed with fully porous particles. Earlier and recent findings showing that the PSD has no direct physical impact on eddy dispersion and column efficiency are confirmed by these results. Copyright © 2014 Elsevier B.V. All rights reserved.

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

PubMed

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

2016-10-01

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

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

PubMed

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

2011-08-15

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

Colloidal aspects and packing behaviour of charged microparticulates in high efficiency ion chromatography.

PubMed

Wahab, M Farooq; Pohl, Christopher A; Lucy, Charles A

2012-12-28

The development of small particles in ion chromatography (IC) is a recent phenomenon. Very few studies are available on packing polymeric particles bearing ionizable functional groups. This study explores the colloidal and rheological properties that govern slurry packing to form high efficiency IC columns. The polymeric substrate used was non-porous 4.4 μm sulfonated ethylvinylbenzene–divinylbenzene (1.4 mequiv. SO(3)H/g resin) with 55% crosslink. We developed simple tests optical microscopy and sedimentation tests for predicting the quality of packed columns. The negatively charged particles (zeta potential: −52 mV in water) behave like colloids. The influence of counter-ion charge (Al(3+), Mg(2+), Na(+)) and ionic strength on column efficiency followed the Schulze–Hardy rule. Highly flocculating slurries give poorly packed columns with N ~ 900 whereas under non-agglomerating slurry conditions efficiencies up to N > 10,000 can be achieved. A non-agglomerating slurry also shows non-Newtonian behaviour, specifically shear thickening. Packing at lower flow rate (<1 mL/min) or higher temperature (>50 °C) reduces the shear thickening and produces higher efficiency columns. The packed sulfonated resin column is coated with 72 nm quaternary ammonium bearing latex (AS4A) and used in the separation of F(−), Cl(−), NO(2)(−), Br(−), and NO(3)(−) yielding a reduced plate height of 1.9 under optimum conditions.

Efficient production of Trastuzumab Fab antibody fragments in Brevibacillus choshinensis expression system.

PubMed

Mizukami, Makoto; Onishi, Hiromasa; Hanagata, Hiroshi; Miyauchi, Akira; Ito, Yuji; Tokunaga, Hiroko; Ishibashi, Matsujiro; Arakawa, Tsutomu; Tokunaga, Masao

2018-10-01

The Brevibacillus expression system has been successfully employed for the efficient productions of a variety of recombinant proteins, including enzymes, cytokines, antigens and antibody fragments. Here, we succeeded in secretory expression of Trastuzumab Fab antibody fragments using B. choshinensis/BIC (Brevibacillus in vivocloning) expression system. In the fed-batch high-density cell culture, recombinant Trastuzumab Fab with amino-terminal His-tag (His-BcFab) was secreted at high level, 1.25 g/liter, and Fab without His-tag (BcFab) at ∼145 mg/L of culture supernatant. His-BcFab and BcFab were purified to homogeneity using combination of conventional column chromatographies with a yield of 10-13%. This BcFab preparation exhibited native structure and functions evaluated by enzyme-linked immunosorbent assay, surface plasmon resonance, circular dichroism measurements and size exclusion chromatography. To our knowledge, this is the highest production of Fab antibody fragments in gram-positive bacterial expression/secretion systems. Copyright © 2018 Elsevier Inc. All rights reserved.

Sub-to super-ambient temperature programmable microfabricated gas chromatography column

DOEpatents

Robinson, Alex L.; Anderson, Lawrence F.

2004-03-16

A sub- to super-ambient temperature programmable microfabricated gas chromatography column enables more efficient chemical separation of chemical analytes in a gas mixture by combining a thermoelectric cooler and temperature sensing on the microfabricated column. Sub-ambient temperature programming enables the efficient separation of volatile organic compounds and super-ambient temperature programming enables the elution of less volatile analytes within a reasonable time. 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.

An on-line coupling of nanofibrous extraction with column-switching high performance liquid chromatography - A case study on the determination of bisphenol A in environmental water samples.

PubMed

Háková, Martina; Chocholoušová Havlíková, Lucie; Chvojka, Jiří; Solich, Petr; Šatínský, Dalibor

2018-02-01

Polyamide 6 nanofiber polymers were used as modern sorbents for on-line solid phase extraction (SPE) coupled with liquid chromatography. The on-line SPE system was tested for the determination of bisphenol A in river water samples. Polyamide nanofibers were prepared using needleless electrospinning, inserted into a mini-column cartridge (5 × 4.6mm) and coupled with HPLC. The effect of column packing and the amount of polyamide 6 on extraction efficiency was tested and the packing process was optimized. The proposed method was performed using a 50-µL sample injection followed by an on-line nanofibrous extraction procedure. The influence of the washing mobile phase on the retention of bisphenol A during the extraction procedure was evaluated. Ascentis ® Express C18 (10cm × 4.6mm) core-shell column was used as an analytical column. Fluorescence detection wavelengths (λ ex = 225nm and λ em = 320nm) were used for identification and quantification of Bisphenol A in river waters. The linearity was tested in the range from 2 to 500µgL -1 (using nine calibration points). The limits of detection and quantification were 0.6 and 2µgL -1 , respectively. The developed method was successfully used for the determination of bisphenol A in various samples of river waters in the Czech Republic (The Ohře, Labe, Nisa, Úpa, and Opava Rivers). Copyright © 2017 Elsevier B.V. All rights reserved.

Microengineered open tubular columns for GC analysis

NASA Astrophysics Data System (ADS)

Wiranto, Goib; Haskard, Malcolm R.; Mulcahy, Dennis E.; Davey, David E.; Dawes, Ernest F.

1999-09-01

Microengineered open tubular (MOT) columns with semi rectangular cross-sections have been designed and fabricated using microengineering techniques. The creation of 100-micrometers wide, 20-micrometers deep, and 125-cm long columns employed isotropic etching on (100) silicon and anodic bonding with a Pyrex 7740 glass cover plate. Column geometry has been optimized to achieve maximum efficiency and allow extreme operating conditions. The walls of the microcolumns were coated with a non-polar liquid stationary phase. Performances of the MOT columns have been demonstrated by their ability to completely separate a series of hydrocarbon mixture in less than 1.25 min under isothermal condition of 150 degrees C. The achievable column efficiencies as measured in terms of theoretical plate height ranged from 0.57 to 1.45 mm, which agreed well with theoretical predictions.

The importance of system band broadening in modern size exclusion chromatography.

PubMed

Goyon, Alexandre; Guillarme, Davy; Fekete, Szabolcs

2017-02-20

In the last few years, highly efficient UHP-SEC columns packed with sub-3μm particles were commercialized by several providers. Besides the particle size reduction, the dimensions of modern SEC stationary phases (150×4.6mm) was also modified compared to regular SEC columns (300×6 or 300×8mm). Because the analytes are excluded from the pores in SEC, the retention factors are very low, ranging from -1

Bed morphological features associated with an optimal slurry concentration for reproducible preparation of efficient capillary ultrahigh pressure liquid chromatography columns.

PubMed

Reising, Arved E; Godinho, Justin M; Jorgenson, James W; Tallarek, Ulrich

2017-06-30

Column wall effects and the formation of larger voids in the bed during column packing are factors limiting the achievement of highly efficient columns. Systematic variation of packing conditions, combined with three-dimensional bed reconstruction and detailed morphological analysis of column beds, provide valuable insights into the packing process. Here, we study a set of sixteen 75μm i.d. fused-silica capillary columns packed with 1.9μm, C18-modified, bridged-ethyl hybrid silica particles slurried in acetone to concentrations ranging from 5 to 200mg/mL. Bed reconstructions for three of these columns (representing low, optimal, and high slurry concentrations), based on confocal laser scanning microscopy, reveal morphological features associated with the implemented slurry concentration, that lead to differences in column efficiency. At a low slurry concentration, the bed microstructure includes systematic radial heterogeneities such as particle size-segregation and local deviations from bulk packing density near the wall. These effects are suppressed (or at least reduced) with higher slurry concentrations. Concomitantly, larger voids (relative to the mean particle diameter) begin to form in the packing and increase in size and number with the slurry concentration. The most efficient columns are packed at slurry concentrations that balance these counteracting effects. Videos are taken at low and high slurry concentration to elucidate the bed formation process. At low slurry concentrations, particles arrive and settle individually, allowing for rearrangements. At high slurry concentrations, they arrive and pack as large patches (reflecting particle aggregation in the slurry). These processes are discussed with respect to column packing, chromatographic performance, and bed microstructure to help reinforce general trends previously described. Conclusions based on this comprehensive analysis guide us towards further improvement of the packing process. Copyright © 2017 Elsevier B.V. All rights reserved.

ENTRAINMENT AND EFFICIENCY STUDIES IN A SMALL DIAMETER BUBBLECAP PLATE COLUMN

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

Chrones, J.

1952-07-01

Efficiency and entrainment studies were made in a 4inch diameter bubblecap plate column using a plate spacing of 4 inches. The plates contained one bubblecap each, and were designed so taat they could be easily inserted in a single length of 4 inch OD stainless steel tubing. An entrainment of 10% was obtained for the water-steam system at a column vapor velocity of 1.9 fps or a vapor mass rate of 255 pounds of steam per hour per square foot. This entraimnent value is gener ally accepted as the maximum allowable without impairing the plate efficiency appreciably. This low entrainmentmore » may be partly due to the small column diameter with the walls acting as entrainanent separators. The Murphree vapor plate efficiency, as measured for alcohol-water, was found to depend on the slope of the equilibrium line and the mass velocity factor V / sub v//sup 0.5/. An empirical equation was developed relating these factors. Fow low values of the slope of the equilibrium line (2 or less it was noted, that for practical purposes, the actual point efficiency on the plates was equal to the measured Murphree vapor plate efficiency regardless of the degree of mixing on the plate. (auth)« less

The Joule-Thomson coefficient as a criterion for efficient operating conditions in supercritical fluid chromatography.

PubMed

Poe, Donald P; Helmueller, Shawn; Kobany, Stephanie; Feldhacker, Hannah; Kaczmarski, Krzysztof

2017-01-27

When an SFC column is operated in a traditional oven with forced air at low pressures near the critical temperature, severe efficiency losses can occur. The mobile phase cools as it expands along the column, forming axial and radial temperature gradients. In this study we present a simple model based on a virtual fluid to predict the conditions which lead to the onset of efficiency loss. The model shows that the Joule-Thomson coefficient is an important factor leading to efficiency loss in packed columns under forced air conditions. The model was tested experimentally for elution of n-alkylbenzenes on 250×4.6-mm ID columns packed with 5-μm Luna-C18 (fully porous) and Kinetex-C18 (superficially porous) particles at optimum flow rates in a forced air oven at 20-80°C and outlet pressures from 90 to 250bar, with CO 2 mobile phase containing 5, 10 and 20% methanol (v/v). For simplicity, we used a formal J-T coefficient corresponding to the inlet temperature and the outlet pressure to characterize the chromatographic conditions. For 5% methanol, there was no significant loss of efficiency for elution of n-octadecylbenzene as long as the formal J-T coefficient was less than 0.11K/bar for Luna or 0.15K/bar for Kinetex, with minimum reduced plate heights equal to 1.82 and 1.55, respectively, at an average apparent retention factor of approximately 4.0 for both columns. The Kinetex column provided superior efficiency in general, and at 10-20bar lower outlet pressures relative to the Luna column due to the higher thermal conductivity of the packing. Results for 10 and 20% methanol showed similar trends but were less predictable. Copyright © 2016 Elsevier B.V. All rights reserved.

Influence of detergent formulation on nutrient movement through sand columns simulating mound and conventional septic system drainfields

NASA Astrophysics Data System (ADS)

Alhajjar, Bashar J.; Linn Gould, C.; Chesters, Gordon; Harkin, John M.

1990-12-01

The effects of phosphate (P) and zeolite (Z) -built detergents on leaching of N and P through sand columns simulating septic system drainfields were examined in laboratory columns. To simulate mound septic system drainfields, paired sets of columns were dosed intermittently with septic tank effluent from households using P- or Z-built detergent. Two other paired sets of columns were flooded with P- or Z-effluent to simulate new conventional septic system drainfields; after clogging mats or "crusts" developed at infiltration surface, the subsurfaces of the columns were aerated to simulate mature (crusted) conventional septic system drainfields. NO 3 loading in leachate was 1.1 times higher and ortho-P loading was 4.3 times lower when columns were dosed with Z- than with P-effluent. Dosed columns removed P poorly; total phosphorus (TP) loading in leachate was 81 and 19 g m -2 yr -1 with P- and Z-effluent, respectively. In flooded columns 1.3, 2.0 and 1.8 times more NH 4, organic nitrogen (ON) and total nitrogen (TN) respectively, were leached with Z- than with P-effluent; NO 3 leaching was similar. Flooded columns removed P efficiently; TP leached through flooded systems was 2.5 and 1.4 g m -2 yr -1 with P- and Z effluent, respectively. Crusted columns fed Z-effluent leached 1.2, 2.6, 1.4 and 2.1 times more NH 4, NO 3, ON and TN, respectively, than those with P-effluent but 1.8 times less TP. Crusted columns removed P satisfactorily: 8.2 and 4.6 g m -2 yr -1 TP with P- and Z-effluent, respectively. The P-built detergent substantially improves the efficiency of N removal with satisfactory P removal in columns simulating conventional septic system drainfield. Simultaneous removal of N and P under flooded conditions might be explained by precipitation of struvite-type minerals. Dosed system drainfields were less efficient in removing N and P compared to flooded and crusted system drainfelds.

Temperature programmable microfabricated gas chromatography column

DOEpatents

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.

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

PubMed

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

2017-03-01

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

Efficient concepts for large erectable space structures

NASA Technical Reports Server (NTRS)

Card, M. F.; Bush, H. G.; Heard, W. L., Jr.; Mikulas, M. M., Jr.

1978-01-01

The status of Langley Research Center development of the nestable column concept is reviewed including results of member and truss component tests, and planned assembly studies. In addition, more recent studies of alternative member concepts are presented. Preliminary results on relative efficiency of several types of truss-type columns are compared and future test plans discussed.

An improved Pearson's correlation proximity-based hierarchical clustering for mining biological association between genes.

PubMed

Booma, P M; Prabhakaran, S; Dhanalakshmi, R

2014-01-01

Microarray gene expression datasets has concerned great awareness among molecular biologist, statisticians, and computer scientists. Data mining that extracts the hidden and usual information from datasets fails to identify the most significant biological associations between genes. A search made with heuristic for standard biological process measures only the gene expression level, threshold, and response time. Heuristic search identifies and mines the best biological solution, but the association process was not efficiently addressed. To monitor higher rate of expression levels between genes, a hierarchical clustering model was proposed, where the biological association between genes is measured simultaneously using proximity measure of improved Pearson's correlation (PCPHC). Additionally, the Seed Augment algorithm adopts average linkage methods on rows and columns in order to expand a seed PCPHC model into a maximal global PCPHC (GL-PCPHC) model and to identify association between the clusters. Moreover, a GL-PCPHC applies pattern growing method to mine the PCPHC patterns. Compared to existing gene expression analysis, the PCPHC model achieves better performance. Experimental evaluations are conducted for GL-PCPHC model with standard benchmark gene expression datasets extracted from UCI repository and GenBank database in terms of execution time, size of pattern, significance level, biological association efficiency, and pattern quality.

An Improved Pearson's Correlation Proximity-Based Hierarchical Clustering for Mining Biological Association between Genes

PubMed Central

Booma, P. M.; Prabhakaran, S.; Dhanalakshmi, R.

2014-01-01

Microarray gene expression datasets has concerned great awareness among molecular biologist, statisticians, and computer scientists. Data mining that extracts the hidden and usual information from datasets fails to identify the most significant biological associations between genes. A search made with heuristic for standard biological process measures only the gene expression level, threshold, and response time. Heuristic search identifies and mines the best biological solution, but the association process was not efficiently addressed. To monitor higher rate of expression levels between genes, a hierarchical clustering model was proposed, where the biological association between genes is measured simultaneously using proximity measure of improved Pearson's correlation (PCPHC). Additionally, the Seed Augment algorithm adopts average linkage methods on rows and columns in order to expand a seed PCPHC model into a maximal global PCPHC (GL-PCPHC) model and to identify association between the clusters. Moreover, a GL-PCPHC applies pattern growing method to mine the PCPHC patterns. Compared to existing gene expression analysis, the PCPHC model achieves better performance. Experimental evaluations are conducted for GL-PCPHC model with standard benchmark gene expression datasets extracted from UCI repository and GenBank database in terms of execution time, size of pattern, significance level, biological association efficiency, and pattern quality. PMID:25136661

Radial distribution of the flow velocity, efficiency and concentration in a wide HPLC column

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

Farkas, T.; Sepaniak, M.J.; Guiochon, G.

1997-08-01

The use of optical fibers in a fluorescence-detection scheme permits the accurate determination of the radial distribution of the transit time, the column efficiency, and the analyte concentration at the exit of a chromatographic axial-compression column (50 mmID). The results obtained demonstrate that the column is not homogeneous, but suggest a nearly cylindrical distribution of the packing density. The average velocity close to the column wall is 7% lower than along its axis and the HETP 25% higher. The lack of homogeneity of the column packing is another source of band broadening not taken into account in chromatography so far.more » It causes the apparent HETP derived from the conventional elution chromatogram recorded on the bulk eluent to be larger than the local HETP and the band profile to be unsymmetrical with a slight tail reminiscent of kinetic tailing.« less

Comparison between the intra-particle diffusivity in the hydrophilic interaction chromatography and reversed phase liquid chromatography modes. Impact on the column efficiency.

PubMed

Gritti, Fabrice; Guiochon, Georges

2013-07-05

The effective diffusion coefficients of five low molecular weigh compounds (naphthalene, uracil, uridine, adenosine, and cytosine) were measured at room temperature in a 4.6mm×100mm column packed with 3.5μm XBridge HILIC particles. The mobile phase was an acetonitrile-water mixture (92.5/7.5, v/v) containing 10mM ammonium acetate and 0.02% acetic acid. Using a physically reliable model of effective diffusion in binary composite media (Torquato's model), accurate estimates of the intra-particle diffusivities in the HILIC particles were obtained as a function of the retention of these analytes. The HILIC diffusion coefficients were compared to those previously obtained for endcapped RPLC-C18 particles (5.0μm Gemini-C18). The experimental results confirm that adsorption sites are not localized in RPLC whereas they are so in the HILIC mode. In contrast to RPLC columns, HILIC columns provide longitudinal diffusion B/u terms that increase very little with increasing retention factors. This confirms the absence of surface diffusion in HILIC. The impact of intra-particle diffusivity on the column efficiency was projected in HILIC and RPLC on the basis of the measured intra-particle diffusivities and on the well established theory of band broadening in particulate columns. Accordingly, RPLC columns generate short-range eddy dispersion and solid-liquid mass transfer resistance Cu terms that increase less than do HILIC column with increasing retention factors. The HETP contribution caused by the trans-column structure heterogeneity is smaller in the HILIC than in the RPLC modes because the transverse excursion length is smaller in HILIC. Even though the overall column efficiencies are comparable in HILIC and RPLC, this study shows that the individual mass transfer phenomena are inherently different in the HILIC and the RPLC retention modes. Copyright © 2013 Elsevier B.V. All rights reserved.

Comparison of high-performance liquid chromatography separation of red wine anthocyanins on a mixed-mode ion-exchange reversed-phase and on a reversed-phase column.

PubMed

Vergara, Carola; Mardones, Claudia; Hermosín-Gutiérrez, Isidro; von Baer, Dietrich

2010-09-03

Anthocyanins, which confer the characteristic color to red wine, can be used as markers to classify wines according to the grape variety. It is a complex separation that requires very high chromatographic efficiency, especially in the case of aged red wines, due to the formation of pyranoanthocyanins. A coelution between these kinds of compounds can affect the R(ac/coum) ratio of aged wines, and might lead to false results when classifying the wine variety. In 2007, the use of a novel mixed-mode ion-exchange reversed-phase column was reported to separate anthocyanins extracted from grapes of Vitis labrusca with different selectivity than C-18 columns. In the present work, the separation of anthocyanins including pyranoanthocyanins in young and aged Cabernet Sauvignon wines and other varieties is evaluated. The most interesting contributions of this research are the different elution order and selectivity obtained for anthocyanins and pyranoanthocyanins (only formed in wine), compared with those observed in C-18 stationary phases. Also interesting is the separation of the polymeric fraction, which elutes as a clearly separated peak at the chromatogram's end. However, a comparison with a high efficiency C-18 column with the same dimensions and particle size demonstrated that the tested mixed-mode column shows broader peaks with a theoretical plate number below 8000, for malvidin-3-glucoside peak, while it can be up to 10 times higher for a high efficiency C-18 column, depending on the column manufacturer. Under the tested conditions, in mixed-mode phase, the analysis time is almost twice that of a C-18 column with the same dimensions and particle size. A mixed-mode phase with increased efficiency should provide an interesting perspective for separation of anthocyanins in wine, due to its improved selectivity, combined with a useful role in a second-dimension separation in preparative anthocyanin chromatography. 2010 Elsevier B.V. All rights reserved.

An experiment for determining the Euler load by direct computation

NASA Technical Reports Server (NTRS)

Thurston, Gaylen A.; Stein, Peter A.

1986-01-01

A direct algorithm is presented for computing the Euler load of a column from experimental data. The method is based on exact inextensional theory for imperfect columns, which predicts two distinct deflected shapes at loads near the Euler load. The bending stiffness of the column appears in the expression for the Euler load along with the column length, therefore the experimental data allows a direct computation of bending stiffness. Experiments on graphite-epoxy columns of rectangular cross-section are reported in the paper. The bending stiffness of each composite column computed from experiment is compared with predictions from laminated plate theory.

Chromatographic efficiency of polar capillary columns applied for the analysis of fatty acid methyl esters by gas chromatography.

PubMed

Waktola, Habtewold D; Mjøs, Svein A

2018-04-01

The chromatographic efficiency that could be achieved in temperature-programmed gas chromatography was compared for four capillary columns that are typically applied for analysis of fatty acid methyl esters (FAME). Three different carrier gases, hydrogen, helium and nitrogen, were applied. For each experiment, the carrier gas velocities and the temperature rates were varied with a full 9 × 3 design, with nine levels on the carrier gas velocity and temperature rates of 1, 2 or 3°C/min. Response surface methodology was used to create models of chromatographic efficiency as a function of temperature rate and carrier gas velocity. The chromatographic efficiency was defined as the inverse of peak widths measured in retention index units. The final results were standardized so that the efficiencies that could be achieved within a certain time frame, defined by the retention time of the last compound in the chromatogram, could be compared. The results show that there were clear differences in the efficiencies that could be achieved with the different columns and that the efficiency decreased with increasing polarity of the stationary phase. The differences can be explained by higher resistance to mass transfer in the stationary phase in the most polar columns. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Implementation of high slurry concentration and sonication to pack high-efficiency, meter-long capillary ultrahigh pressure liquid chromatography columns.

PubMed

Godinho, Justin M; Reising, Arved E; Tallarek, Ulrich; Jorgenson, James W

2016-09-02

Slurry packing capillary columns for ultrahigh pressure liquid chromatography is complicated by many interdependent experimental variables. Previous results have suggested that combination of high slurry concentration and sonication during packing would create homogeneous bed microstructures and yield highly efficient capillary columns. Herein, the effect of sonication while packing very high slurry concentrations is presented. A series of six, 1m×75μm internal diameter columns were packed with 200mg/mL slurries of 2.02μm bridged-ethyl hybrid silica particles. Three of the columns underwent sonication during packing and yielded highly efficient separations with reduced plate heights as low as 1.05. Copyright © 2016 Elsevier B.V. All rights reserved.

Distillation Column Flooding Predictor

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

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 distillationmore » 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/vapor traffic that produce increased contact area and lead to substantial increases in separation efficiency – which translates to a 10% increase in energy efficiency on a BTU/bbl basis. The Flooding Predictor™ operates on the principle that between five to sixty minutes in advance of a flooding event, certain column variables experience an oscillation, a pre-flood pattern. The pattern recognition system of the Flooding Predictor™ utilizes the mathematical first derivative of certain column variables to identify the column’s pre-flood pattern(s). This pattern is a very brief, highly repeatable, simultaneous movement among the derivative values of certain column variables. While all column variables experience negligible random noise generated from the natural frequency of the process, subtle pre-flood patterns are revealed among sub-sets of the derivative values of column variables as the column approaches its hydraulic limit. The sub-set of column variables that comprise the pre-flood pattern is identified empirically through in a two-step process. First, 2ndpoint’s proprietary off-line analysis tool is used to mine historical data for pre-flood patterns. Second, the column is flood-tested to fine-tune the pattern recognition for commissioning. Then the Flooding Predictor™ is implemented as closed-loop advanced control strategy on the plant’s distributed control system (DCS), thus automating control of the column at its hydraulic limit.« less

Monodisperse CNT Microspheres for High Permeability and Efficiency Flow-Through Filtration Applications.

PubMed

Copic, Davor; Maggini, Laura; De Volder, Michael

2018-03-01

Carbon nanotube (CNT)-based filters have the potential to revolutionize water treatment because of their high capacity and fast kinetics in sorption of organic, inorganic, and biological pollutants. To date, CNT filters either rely on CNTs dispersed in liquids, which are difficult to recover and cause safety concerns, or on CNT buckypaper, which offers high efficiency, but suffers from an intrinsic trade-off between filter permeability and capacity. Here, a new approach is presented that bypasses this trade-off and achieves buckypaper-like efficiency combined with filter-column-like permeability and capacity. For this, CNTs are first assembled into porous microspheres and then are packed into microfluidic column filters. These microcolumns exhibit large flow-through filtration efficiencies, while maintaining membrane permeabilities an order of magnitude larger then CNT buckypaper and specific permeabilities double that of activated carbon for similar flowrates (232 000 L m -2 h -1 bar -1 , 1.23 × 10 -12 m 2 ). Moreover, in a test to remove sodium dodecyl sulfate (SDS) from water, these microstructured CNT columns outperform activated carbon columns. This improved filtration efficiency and permeability is an important step toward a broader implementation of CNT-based filtration devices. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

An efficient procedure for the expression and purification of HIV-1 protease from inclusion bodies.

PubMed

Nguyen, Hong-Loan Thi; Nguyen, Thuy Thi; Vu, Quy Thi; Le, Hang Thi; Pham, Yen; Trinh, Phuong Le; Bui, Thuan Phuong; Phan, Tuan-Nghia

2015-12-01

Several studies have focused on HIV-1 protease for developing drugs for treating AIDS. Recombinant HIV-1 protease is used to screen new drugs from synthetic compounds or natural substances. However, large-scale expression and purification of this enzyme is difficult mainly because of its low expression and solubility. In this study, we constructed 9 recombinant plasmids containing a sequence encoding HIV-1 protease along with different fusion tags and examined the expression of the enzyme from these plasmids. Of the 9 plasmids, pET32a(+) plasmid containing the HIV-1 protease-encoding sequence along with sequences encoding an autocleavage site GTVSFNF at the N-terminus and TEV plus 6× His tag at the C-terminus showed the highest expression of the enzyme and was selected for further analysis. The recombinant protein was isolated from inclusion bodies by using 2 tandem Q- and Ni-Sepharose columns. SDS-PAGE of the obtained HIV-1 protease produced a single band of approximately 13 kDa. The enzyme was recovered efficiently (4 mg protein/L of cell culture) and had high specific activity of 1190 nmol min(-1) mg(-1) at an optimal pH of 4.7 and optimal temperature of 37 °C. This procedure for expressing and purifying HIV-1 protease is now being scaled up to produce the enzyme on a large scale for its application. Copyright © 2015 Elsevier Inc. All rights reserved.

Numerical study on xenon positive column discharges of mercury-free lamp

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

Ouyang, Jiting; He, Feng; Miao, Jinsong

2007-02-15

In this paper, the numerical study has been performed on the xenon positive column discharges of mercury-free fluorescent lamp. The plasma discharge characteristics are analyzed by numerical simulation based on two-dimensional fluid model. The effects of cell geometry, such as the dielectric layer, the electrode width, the electrode gap, and the cell height, and the filling gas including the pressure and the xenon percentage are investigated in terms of discharge current and discharge efficiency. The results show that a long transient positive column will form in the xenon lamp when applying ac sinusoidal power and the lamp can operate inmore » a large range of voltage and frequency. The front dielectric layer of the cell plays an important role in the xenon lamp while the back layer has little effect. The ratio of electrode gap to cell height should be large to achieve a long positive column xenon lamp and higher efficiency. Increase of pressure or xenon concentration results in an increase of discharge efficiency and voltage. The discussions will be helpful for the design of commercial xenon lamp cells.« less

High Strength Concrete Columns under Axial Compression Load: Hybrid Confinement Efficiency of High Strength Transverse Reinforcement and Steel Fibers

PubMed Central

Perceka, Wisena; Liao, Wen-Cheng; Wang, Yo-de

2016-01-01

Addition of steel fibers to high strength concrete (HSC) improves its post-peak behavior and energy absorbing capability, which can be described well in term of toughness. This paper attempts to obtain both analytically and experimentally the efficiency of steel fibers in HSC columns with hybrid confinement of transverse reinforcement and steel fibers. Toughness ratio (TR) to quantify the confinement efficiency of HSC columns with hybrid confinement is proposed through a regression analysis by involving sixty-nine TRs of HSC without steel fibers and twenty-seven TRs of HSC with hybrid of transverse reinforcement and steel fibers. The proposed TR equation was further verified by compression tests of seventeen HSC columns conducted in this study, where twelve specimens were reinforced by high strength rebars in longitudinal and transverse directions. The results show that the efficiency of steel fibers in concrete depends on transverse reinforcement spacing, where the steel fibers are more effective if the spacing transverse reinforcement becomes larger in the range of 0.25–1 effective depth of the section column. Furthermore, the axial load–strain curves were developed by employing finite element software (OpenSees) for simulating the response of the structural system. Comparisons between numerical and experimental axial load–strain curves were carried out. PMID:28773391

The effect of column purification on cDNA indirect labelling for microarrays

PubMed Central

Molas, M Lia; Kiss, John Z

2007-01-01

Background The success of the microarray reproducibility is dependent upon the performance of standardized procedures. Since the introduction of microarray technology for the analysis of global gene expression, reproducibility of results among different laboratories has been a major problem. Two of the main contributors to this variability are the use of different microarray platforms and different laboratory practices. In this paper, we address the latter question in terms of how variation in one of the steps of a labelling procedure affects the cDNA product prior to microarray hybridization. Results We used a standard procedure to label cDNA for microarray hybridization and employed different types of column chromatography for cDNA purification. After purifying labelled cDNA, we used the Agilent 2100 Bioanalyzer and agarose gel electrophoresis to assess the quality of the labelled cDNA before its hybridization onto a microarray platform. There were major differences in the cDNA profile (i.e. cDNA fragment lengths and abundance) as a result of using four different columns for purification. In addition, different columns have different efficiencies to remove rRNA contamination. This study indicates that the appropriate column to use in this type of protocol has to be experimentally determined. Finally, we present new evidence establishing the importance of testing the method of purification used during an indirect labelling procedure. Our results confirm the importance of assessing the quality of the sample in the labelling procedure prior to hybridization onto a microarray platform. Conclusion Standardization of column purification systems to be used in labelling procedures will improve the reproducibility of microarray results among different laboratories. In addition, implementation of a quality control check point of the labelled samples prior to microarray hybridization will prevent hybridizing a poor quality sample to expensive micorarrays. PMID:17597522

The effect of column purification on cDNA indirect labelling for microarrays.

PubMed

Molas, M Lia; Kiss, John Z

2007-06-27

The success of the microarray reproducibility is dependent upon the performance of standardized procedures. Since the introduction of microarray technology for the analysis of global gene expression, reproducibility of results among different laboratories has been a major problem. Two of the main contributors to this variability are the use of different microarray platforms and different laboratory practices. In this paper, we address the latter question in terms of how variation in one of the steps of a labelling procedure affects the cDNA product prior to microarray hybridization. We used a standard procedure to label cDNA for microarray hybridization and employed different types of column chromatography for cDNA purification. After purifying labelled cDNA, we used the Agilent 2100 Bioanalyzer and agarose gel electrophoresis to assess the quality of the labelled cDNA before its hybridization onto a microarray platform. There were major differences in the cDNA profile (i.e. cDNA fragment lengths and abundance) as a result of using four different columns for purification. In addition, different columns have different efficiencies to remove rRNA contamination. This study indicates that the appropriate column to use in this type of protocol has to be experimentally determined. Finally, we present new evidence establishing the importance of testing the method of purification used during an indirect labelling procedure. Our results confirm the importance of assessing the quality of the sample in the labelling procedure prior to hybridization onto a microarray platform. Standardization of column purification systems to be used in labelling procedures will improve the reproducibility of microarray results among different laboratories. In addition, implementation of a quality control check point of the labelled samples prior to microarray hybridization will prevent hybridizing a poor quality sample to expensive micorarrays.

Beyond Scale-Free Small-World Networks: Cortical Columns for Quick Brains

NASA Astrophysics Data System (ADS)

Stoop, Ralph; Saase, Victor; Wagner, Clemens; Stoop, Britta; Stoop, Ruedi

2013-03-01

We study to what extent cortical columns with their particular wiring boost neural computation. Upon a vast survey of columnar networks performing various real-world cognitive tasks, we detect no signs of enhancement. It is on a mesoscopic—intercolumnar—scale that the existence of columns, largely irrespective of their inner organization, enhances the speed of information transfer and minimizes the total wiring length required to bind distributed columnar computations towards spatiotemporally coherent results. We suggest that brain efficiency may be related to a doubly fractal connectivity law, resulting in networks with efficiency properties beyond those by scale-free networks.

A design procedure for a tension-wire stiffened truss-column

NASA Technical Reports Server (NTRS)

Greene, W. H.

1980-01-01

A deployable, tension wire stiffened, truss column configuration was considered for space structure applications. An analytical procedure, developed for design of the truss column and exercised in numerical studies, was based on equivalent beam stiffness coefficients in the classical analysis for an initially imperfect beam column. Failure constraints were formulated to be used in a combined weight/strength and nonlinear mathematical programming automated design procedure to determine the minimum mass column for a particular combination of design load and length. Numerical studies gave the mass characteristics of the truss column for broad ranges of load and length. Comparisons of the truss column with a baseline tubular column used a special structural efficiency parameter for this class of columns.

Characterization of new types of stationary phases for fast and ultra-fast liquid chromatography by signal processing based on AutoCovariance Function: a case study of application to Passiflora incarnata L. extract separations.

PubMed

Pietrogrande, Maria Chiara; Dondi, Francesco; Ciogli, Alessia; Gasparrini, Francesco; Piccin, Antonella; Serafini, Mauro

2010-06-25

In this study, a comparative investigation was performed of HPLC Ascentis (2.7 microm particles) columns based on fused-core particle technology and Acquity (1.7 microm particles) columns requiring UPLC instruments, in comparison with Chromolith RP-18e columns. The study was carried out on mother and vegetal tinctures of Passiflora incarnata L. on one single or two coupled columns. The fundamental attributions of the chromatographic profiles are evaluated using a chemometric procedure, based on the AutoCovariance Function (ACVF). Different chromatographic systems are compared in terms of their separation parameters, i.e., number of total chemical components (m(tot)), separation efficiency (sigma), peak capacity (n(c)), overlap degree of peaks and peak purity. The obtained results show the improvements achieved by HPLC columns with narrow size particles in terms of total analysis time and chromatographic efficiency: comparable performance are achieved by Ascentis (2.7 microm particle) column and Acquity (1.7 microm particle) column requiring UPLC instruments. The ACVF plot is proposed as a simplified tool describing the chromatographic fingerprint to be used for evaluating and comparing chemical composition of plant extracts by using the parameters D% - relative abundance of the deterministic component - and c(EACF) - similarity index computed on ACVF. Copyright 2010 Elsevier B.V. All rights reserved.

Semi-industrial experimental study on bauxite separation using a cell-column integration process

NASA Astrophysics Data System (ADS)

Zhang, Ning-ning; Zhou, Chang-chun; Cong, Long-fei; Cao, Wen-long; Zhou, You

2016-01-01

The cyclonic-static micro-bubble flotation column (FCSMC) is a highly efficient mineral processing equipment. In this study, a cell-column (FCSMC) integration process was investigated for the separation of bauxite and its feasibility was analyzed on a theoretical basis. The properties of low-grade bauxite ore from Henan Province, China were analyzed. Parameters such as reagent dosage, scraping bubble time, and pressure of the circulating pump during the sorting process were investigated and optimized to improve the flotation efficiency. On the basis of these parameters, continuous separation experiments were conducted. Bauxite concentrate with an aluminum-to-silicon (A/S) mass ratio of 6.37 and a 77.63wt% recovery rate were achieved via a flow sheet consisting of "fast flotation using a flotation cell, one roughing flotation and one cleaning flotation using flotation columns". Compared with the full-flotation-cells process, the cell-column integration process resulted in an increase of the A/S ratio by 0.41 and the recovery rate by 17.58wt%. Cell-column integration separation technology represents a new approach for the separation of middle-to-low-grade bauxite ore.

Adsorption of water from aqueous acetonitrile on silica-based stationary phases in aqueous normal-phase liquid chromatography.

PubMed

Soukup, Jan; Jandera, Pavel

2014-12-29

Excess adsorption of water from aqueous acetonitrile mobile phases was investigated on 16 stationary phases using the frontal analysis method and coulometric Karl-Fischer titration. The stationary phases include silica gel and silica-bonded phases with different polarities, octadecyl and cholesterol, phenyl, nitrile, pentafluorophenylpropyl, diol and zwitterionic sulfobetaine and phosphorylcholine ligands bonded on silica, hybrid organic-silica and hydrosilated matrices. Both fully porous and core-shell column types were included. Preferential uptake of water by the columns can be described by Langmuir isotherms. Even though a diffuse rather than a compact adsorbed discrete layer of water on the adsorbent surface can be formed because of the unlimited miscibility of water with acetonitrile, for convenience, the preferentially adsorbed water was expressed in terms of a hypothetical monomolecular water layer equivalent in the inner pores. The uptake of water strongly depends on the polarity and type of the column. Less than one monomolecular water layer equivalent was adsorbed on moderate polar silica hydride-based stationary phases, Ascentis Express F5 and Ascentis Express CN column at the saturation capacity, while on more polar stationary phases, several water layer equivalents were up-taken from the mobile phase. The strongest affinity to water was observed on the ZIC cHILIC stationary phases, where more than nine water layer equivalents were adsorbed onto its surface at its saturation capacity. Columns with bonded hydroxyl and diol ligands show stronger water adsorption in comparison to bare silica. Columns based on hydrosilated silica generally show significantly decreased water uptake in comparison to stationary phases bonded on ordinary silica. Significant correlations were found between the water uptake and the separation selectivity for compounds with strong polarity differences. Copyright © 2014 Elsevier B.V. All rights reserved.

Intraganglionic AAV6 results in efficient and long-term gene transfer to peripheral sensory nervous system in adult rats.

PubMed

Yu, Hongwei; Fischer, Gregory; Ferhatovic, Lejla; Fan, Fan; Light, Alan R; Weihrauch, Dorothee; Sapunar, Damir; Nakai, Hiroyuki; Park, Frank; Hogan, Quinn H

2013-01-01

We previously demonstrated safe and reliable gene transfer to the dorsal root ganglion (DRG) using a direct microinjection procedure to deliver recombinant adeno-associated virus (AAV) vector. In this study, we proceed to compare the in vivo transduction patterns of self-complementary (sc) AAV6 and AAV8 in the peripheral sensory pathway. A single, direct microinjection of either AAV6 or AAV8 expressing EGFP, at the adjusted titer of 2×10(9) viral particle per DRG, into the lumbar (L) 4 and L5 DRGs of adult rats resulted in efficient EGFP expression (48±20% for AAV6 and 25±4% for AAV8, mean ± SD) selectively in sensory neurons and their axonal projections 3 weeks after injection, which remained stable for up to 3 months. AAV6 efficiently transfers EGFP to all neuronal size groups without differential neurotropism, while AAV8 predominantly targets large-sized neurons. Neurons transduced with AAV6 penetrate into the spinal dorsal horn (DH) and terminate predominantly in superficial DH laminae, as well as in the dorsal columns and deeper laminae III-V. Only few AAV8-transduced afferents were evident in the superficial laminae, and spinal EGFP was mostly present in the deeper dorsal horn (lamina III-V) and dorsal columns, with substantial projections to the ventral horn. AAV6-mediated EGFP-positive nerve fibers were widely observed in the medial plantar skin of ipsilateral hindpaws. No apparent inflammation, tissue damage, or major pain behaviors were observed for either AAV serotype. Taken together, both AAV6 and AAV8 are efficient and safe vectors for transgene delivery to primary sensory neurons, but they exhibit distinct functional features. Intraganglionic delivery of AAV6 is more uniform and efficient compared to AAV8 in gene transfer to peripheral sensory neurons and their axonal processes.

Bacterial Adhesion under Static and Dynamic Conditions

PubMed Central

Rijnaarts, Huub H. M.; Norde, Willem; Bouwer, Edward J.; Lyklema, Johannes; Zehnder, Alexander J. B.

1993-01-01

The deposition of various pseudomonads and coryneform bacteria with different hydrophobicities (water contact angles) and negative cell surface charges on negatively charged Teflon and glass surfaces was investigated. The levels of deposition varied between 5.0 × 104 and 1.6 × 107 cells cm-2 and between 5.0 × 104 and 3.6 × 107 cells cm-2 for dynamic column and static batch systems, respectively, indicating that there was a wide variation in physicochemical interactions. Batch and column results were compared in order to better distinguish between hydrodynamic and other system-dependent influences and method-independent physicochemical interactions. Despite the shorter suspension-solid contact time in columns (1 h) than in batch systems (4 h), the level of deposition (expressed as the number of cells that adhered) divided by the applied ambient cell concentration was 4.12 ± 1.63 times higher in columns than in batch sytems for 15 of 22 strain-surface combinations studied. This demonstrates that transport of microbial particles from bulk liquid to surfaces is more efficient in dynamic columns (transport dominated by convection and diffusion) than in static batch systems (transport by diffusion only). The relative constancy of this ratio for the 15 combinations shows that physicochemical interactions affect adhesion similarly in the two systems. The deviating deposition behavior of the other seven strain-surface combinations could be attributed to method-dependent effects resulting from specific cell characteristics (e.g., to the presence of capsular polymers, to an ability to aggregate, to large cell sizes, or to a tendency to desorb after passage through an air-liquid interface). Images PMID:16349063

HPLC column-switching technique for sample preparation and fluorescence determination of propranolol in urine using fused-core columns in both dimensions.

PubMed

Satínský, Dalibor; Havlíková, Lucie; Solich, Petr

2013-08-01

A new and fast high-performance liquid chromatography (HPLC) column-switching method using fused-core columns in both dimensions for sample preconcentration and determination of propranolol in human urine has been developed. On-line sample pretreatment and propranolol preconcentration were performed on an Ascentis Express RP-C-18 guard column (5 × 4.6 mm), particle size, 2.7 μm, with mobile phase acetonitrile/water (5:95, v/v) at a flow rate of 2.0 mL min(-1) and at a temperature of 50 °C. Valve switch from pretreatment column to analytical column was set at 4.0 min in a back-flush mode. Separation of propranolol from other endogenous urine compounds was achieved on the fused-core column Ascentis Express RP-Amide (100 × 4.6 mm), particle size, 2.7 μm, with mobile phase acetonitrile/water solution of 0.5% triethylamine, pH adjusted to 4.5 by means of glacial acetic acid (25:75, v/v), at a flow rate of 1.0 mL min(-1) and at a temperature of 50 °C. Fluorescence excitation/emission detection wavelengths were set at 229/338 nm. A volume of 1,500 μL of filtered urine sample solution was injected directly into the column-switching HPLC system. The total analysis time including on-line sample pretreatment was less than 8 min. The experimentally determined limit of detection of the method was found to be 0.015 ng mL(-1).

Comparison in partition efficiency of protein separation between four different tubing modifications in spiral high-speed countercurrent chromatography

PubMed Central

Ito, Yoichiro; Clary, Robert

2016-01-01

High-speed countercurrent chromatography with a spiral tube assembly can retain a satisfactory amount of stationary phase of polymer phase systems used for protein separation. In order to improve the partition efficiency a simple tool to modify the tubing shapes was fabricated, and the following four different tubing modifications were made: intermittently pressed at 10 mm width, flat, flat-wave, and flat-twist. Partition efficiencies of the separation column made from these modified tubing were examined in protein separation with an aqueous-aqueous polymer phase system at flow rates of 1–2 ml/min under 800 rpm. The results indicated that the column with all modified tubing improved the partition efficiency at a flow rate of 1 ml/min, but at a higher flow rate of 2 ml/min the columns made of flattened tubing showed lowered partition efficiency apparently due to the loss of the retained stationary phase. Among all the modified columns, the column with intermittently pressed tubing gave the best peak resolution. It may be concluded that the intermittently pressed and flat-twist improve the partition efficiency in a semi-preparative separation while other modified tubing of flat and flat-wave configurations may be used for analytical separations with a low flow rate. PMID:27790621

Comparison in partition efficiency of protein separation between four different tubing modifications in spiral high-speed countercurrent chromatography.

PubMed

Ito, Yoichiro; Clary, Robert

2016-12-01

High-speed countercurrent chromatography with a spiral tube assembly can retain a satisfactory amount of stationary phase of polymer phase systems used for protein separation. In order to improve the partition efficiency a simple tool to modify the tubing shapes was fabricated, and the following four different tubing modifications were made: intermittently pressed at 10 mm width, flat, flat-wave, and flat-twist. Partition efficiencies of the separation column made from these modified tubing were examined in protein separation with an aqueous-aqueous polymer phase system at flow rates of 1-2 ml/min under 800 rpm. The results indicated that the column with all modified tubing improved the partition efficiency at a flow rate of 1 ml/min, but at a higher flow rate of 2 ml/min the columns made of flattened tubing showed lowered partition efficiency apparently due to the loss of the retained stationary phase. Among all the modified columns, the column with intermittently pressed tubing gave the best peak resolution. It may be concluded that the intermittently pressed and flat-twist improve the partition efficiency in a semi-preparative separation while other modified tubing of flat and flat-wave configurations may be used for analytical separations with a low flow rate.

Purification and immunogenicity of hemagglutinin from highly pathogenic avian influenza virus H5N1 expressed in Nicotiana benthamiana

PubMed Central

Pua, Teen-Lee; Chan, Xiao Ying; Loh, Hwei-San; Omar, Abdul Rahman; Yusibov, Vidadi; Musiychuk, Konstantin; Hall, Alexandra C.; Coffin, Megan V.; Shoji, Yoko; Chichester, Jessica A.; Bi, Hong; Streatfield, Stephen J.

2017-01-01

ABSTRACT Highly pathogenic avian influenza (HPAI) H5N1 is an ongoing global health concern due to its severe sporadic outbreaks in Asia, Africa and Europe, which poses a potential pandemic threat. The development of safe and cost-effective vaccine candidates for HPAI is considered the best strategy for managing the disease and addressing the pandemic preparedness. The most potential vaccine candidate is the antigenic determinant of influenza A virus, hemagglutinin (HA). The present research was aimed at developing optimized expression in Nicotiana benthamiana and protein purification process for HA from the Malaysian isolate of H5N1 as a vaccine antigen for HPAI H5N1. Expression of HA from the Malaysian isolate of HPAI in N. benthamiana was confirmed, and more soluble protein was expressed as truncated HA, the HA1 domain over the entire ectodomain of HA. Two different purification processes were evaluated for efficiency in terms of purity and yield. Due to the reduced yield, protein degradation and length of the 3-column purification process, the 2-column method was chosen for target purification. Purified HA1 was found immunogenic in mice inducing H5 HA-specific IgG and a hemagglutination inhibition antibody. This paper offers an alternative production system of a vaccine candidate against a locally circulating HPAI, which has a regional significance. PMID:27929750

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

PubMed

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

2013-10-01

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

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

PubMed

Laaniste, Asko; Kruve, Anneli; Leito, Ivo

2013-08-01

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

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

PubMed

Gritti, Fabrice; McDonald, Thomas; Gilar, Martin

2016-06-17

250μm×100mm fused silica glass capillaries were packed with 1.8μm high-strength silica (HSS) fully porous particles. They were prepared without bulky stainless steel endfittings and metal frits, which both generate significant sample dispersion. The isocratic efficiencies and gradient peak capacities of these prototype capillary columns were measured for small molecules (n-alkanophenones) using a home-made ultra-low dispersive micro-HPLC instrument. Their resolution power was compared to that of standard 2.1mm×100mm very high-pressure liquid chromatography (vHPLC) narrow-bore columns packed with the same particles. The results show that, for the same column efficiency (25000 plates) and gradient steepness (0.04min(-1)), the peak capacity of the 250μm i.d. capillary columns is systematically 15-20% higher than that of the 2.1mm i.d. narrow-bore columns. A validated model of gradient chromatography enabled one to predict accurately the observed peak capacities of the capillary columns for non-linear solvation strength retention behavior and under isothermal conditions. Thermodynamics applied to the eluent quantified the temperature difference for the thermal gradients in both capillary and narrow-bore columns. Experimental data revealed that the gradient peak capacity is more affected by viscous heating than the column efficiency. Unlike across 2.1mm i.d. columns, the changes in eluent composition across the 250μm i.d. columns during the gradient is rapidly relaxed by transverse dispersion. The combination of (1) the absence of viscous heating and (2) the high uniformity of the eluent composition across the diameter of capillary columns explains the intrinsic advantage of capillary over narrow-bore columns in gradient vHPLC. Copyright © 2016 Elsevier B.V. All rights reserved.

Buckling analysis of non-prismatic columns based on modified vibration modes

NASA Astrophysics Data System (ADS)

Rahai, A. R.; Kazemi, S.

2008-10-01

In this paper, a new procedure is formulated for the buckling analysis of tapered column members. The calculation of the buckling loads was carried out by using modified vibrational mode shape (MVM) and energy method. The change of stiffness within a column is characterized by introducing a tapering index. It is shown that, the changes in the vibrational mode shapes of a tapered column can be represented by considering a linear combination of various modes of uniform-section columns. As a result, by making use of these modified mode shapes (MVM) and applying the principle of stationary total potential energy, the buckling load of tapered columns can be obtained. Several numerical examples on tapered columns demonstrate the accuracy and efficiency of the proposed analytical method.

Ideal versus real automated twin column recycling chromatography process.

PubMed

Gritti, Fabrice; Leal, Mike; McDonald, Thomas; Gilar, Martin

2017-07-28

The full baseline separation of two compounds (selectivity factors α<1.03) is either impractical (too long analysis times) or even impossible when using a single column of any length given the pressure limitations of current LC instruments. The maximum efficiency is that of an infinitely long column operated at infinitely small flow rates. It is determined by the maximum allowable system pressure, the column permeability (particle size), the viscosity of the eluent, and the intensity of the effective diffusivity of the analytes along the column. Alternatively, the twin-column recycling separation process (TCRSP) can overcome the efficiency limit of the single-column approach. In the TCRSP, the sample mixture may be transferred from one to a second (twin) column until its band has spread over one column length. Basic theory of chromatography is used to confirm that the speed-resolution performance of the TCRSP is intrinsically superior to that of the single-column process. This advantage is illustrated in this work by developing an automated TCRSP for the challenging separation of two polycyclic aromatic hydrocarbon (PAH) isomers (benzo[a]anthracene and chrysene) in the reversed-phase retention mode at pressure smaller than 5000psi. The columns used are the 3.0mm×150mm column packed with 3.5μm XBridge BEH-C 18 material (α=1.010) and the 3.0mm or 4.6mm×150mm columns packed with the same 3.5μm XSelect HSST 3 material (α=1.025). The isocratic mobile phase is an acetonitrile-water mixture (80/20, v/v). Remarkably, significant differences are observed between the predicted retention times and efficiencies of the ideal TCRSP (given by the number of cycles multiplied by the retention time and efficiency of one column) and those of the real TCRSP. The fundamental explanation lies in the pressure-dependent retention of these PAHs or in the change of their partial molar volume as they are transferred from the mobile to the stationary phase. A revisited retention and efficiency model is then built to predict the actual performance of real TCRSPs. The experimental and calculated resolution data are found in very good agreement for a change, Δv m =-10cm 3 /mol, of the partial molar volume of the two PAH isomers upon transfer from the acetonitrile-water eluent mixture to the silica-C 18 stationary phase. Copyright © 2017 Elsevier B.V. All rights reserved.

Simulation of a Novel Single-column Cryogenic Air Separation Process Using LNG Cold Energy

NASA Astrophysics Data System (ADS)

Jieyu, Zheng; Yanzhong, Li; Guangpeng, Li; Biao, Si

In this paper, a novel single-column air separation process is proposed with the implementation of heat pump technique and introduction of LNG coldenergy. The proposed process is verifiedand optimized through simulation on the Aspen Hysys® platform. Simulation results reveal that thepower consumption per unit mass of liquid productis around 0.218 kWh/kg, and the total exergy efficiency of the systemis 0.575. According to the latest literatures, an energy saving of 39.1% is achieved compared with those using conventional double-column air separation units.The introduction of LNG cold energy is an effective way to increase the system efficiency.

Compact sieve-tray distillation column for ammonia-water absorption heat pump: Part 1 -- Design methodology

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

Anand, G.; Erickson, D.C.

1999-07-01

The distillation column is a key component of ammonia-water absorption units including advanced generator-absorber heat exchange (GAX) cycle heat pumps. The design of the distillation column is critical to unit performance, size, and cost. The distillation column can be designed with random packing, structured packing, or various tray configurations. A sieve-tray distillation column is the least complicated tray design and is less costly than high-efficiency packing. Substantial literature is available on sieve tray design and performance. However, most of the correlations and design recommendations were developed for large industrial hydrocarbon systems and are generally not directly applicable to the compactmore » ammonia-water column discussed here. The correlations were reviewed and modified as appropriate for this application, and a sieve-tray design model was developed. This paper presents the sieve-tray design methodology for highly compact ammonia-water columns. A conceptual design of the distillation column for an 8 ton vapor exchange (VX) GAX heat pump is presented, illustrating relevant design parameters and trends. The design process revealed several issues that have to be investigated experimentally to design the final optimized rectifier. Validation of flooding and weeping limits and tray/point efficiencies are of primary importance.« less

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

PubMed

Broeckhoven, Ken; Desmet, Gert

2007-11-16

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

Relative importance of column and adsorption parameters on the productivity in preparative liquid chromatography II: Investigation of separation systems with competitive Langmuir adsorption isotherms.

PubMed

Forssén, Patrik; Samuelsson, Jörgen; Fornstedt, Torgny

2014-06-20

In this study we investigated how the maximum productivity for commonly used, realistic separation system with a competitive Langmuir adsorption isotherm is affected by changes in column length, packing particle size, mobile phase viscosity, maximum allowed column pressure, column efficiency, sample concentration/solubility, selectivity, monolayer saturation capacity and retention factor of the first eluting compound. The study was performed by generating 1000 random separation systems whose optimal injection volume was determined, i.e., the injection volume that gives the largest achievable productivity. The relative changes in largest achievable productivity when one of the parameters above changes was then studied for each system and the productivity changes for all systems were presented as distributions. We found that it is almost always beneficial to use shorter columns with high pressure drops over the column and that the selectivity should be greater than 2. However, the sample concentration and column efficiency have very limited effect on the maximum productivity. The effect of packing particle size depends on the flow rate limiting factor. If the pumps maximum flow rate is the limiting factor use smaller packing, but if the pressure of the system is the limiting factor use larger packing up to about 40μm. Copyright © 2014 Elsevier B.V. All rights reserved.

The Modulation of Crustal Magmatic Systems by Tectonic Forcing

NASA Astrophysics Data System (ADS)

Karakas, O.; Dufek, J.

2010-12-01

The amount, location and residence time of melt in the crust significantly impacts crustal structure and influences the composition, frequency, and volume of eruptive products. In this study, we develop a two dimensional model that simulates the response of the crust to prolonged mantle-derived intrusions in arc environments. The domain includes the entire crustal section and upper mantle and focuses on the evolving thermal structure due to intrusions and external tectonic forcing. Magmatic intrusion into the crust can be accommodated by extension or thickening of the crust or some combination of both mechanisms. Additionally, external tectonic forcing can generate thicker crustal sections, while tectonic extension can significantly thin the crust. We monitor the thermal response, melt fraction and surface heat flux for different tectonic conditions and melt flux from the mantle. The amount of crustal melt versus fractionated primary mantle melts present in the crustal column helps determine crustal structure and growth through time. We express the amount of crustal melting in terms of an efficiency; we define the melting efficiency as the ratio of the melted volume of crustal material to the volume of melt expected from a strict enthalpy balance as explained by Dufek and Bergantz (2005). Melting efficiencies are less than 1 in real systems because heat diffuses to sections of the crust that never melt. In general, thick crust and crust experiencing extended compressional regimes results in an increased melting efficiency; and thin crust and crust with high extension rates have lower efficiency. In most settings, maximum efficiencies are less than 0.05-0.10. We also observe that with a geophysically estimated flux, the mantle-derived magma bodies build up isolated magma pods that are distributed in the crust. One of the aspects of this work is to monitor the location and size of these magma chambers in the crustal column. We further investigate the rheological, stress and pre-existing structure control on the longevity of the individual magmatic systems.

Mynodbcsv: lightweight zero-config database solution for handling very large CSV files.

PubMed

Adaszewski, Stanisław

2014-01-01

Volumes of data used in science and industry are growing rapidly. When researchers face the challenge of analyzing them, their format is often the first obstacle. Lack of standardized ways of exploring different data layouts requires an effort each time to solve the problem from scratch. Possibility to access data in a rich, uniform manner, e.g. using Structured Query Language (SQL) would offer expressiveness and user-friendliness. Comma-separated values (CSV) are one of the most common data storage formats. Despite its simplicity, with growing file size handling it becomes non-trivial. Importing CSVs into existing databases is time-consuming and troublesome, or even impossible if its horizontal dimension reaches thousands of columns. Most databases are optimized for handling large number of rows rather than columns, therefore, performance for datasets with non-typical layouts is often unacceptable. Other challenges include schema creation, updates and repeated data imports. To address the above-mentioned problems, I present a system for accessing very large CSV-based datasets by means of SQL. It's characterized by: "no copy" approach--data stay mostly in the CSV files; "zero configuration"--no need to specify database schema; written in C++, with boost [1], SQLite [2] and Qt [3], doesn't require installation and has very small size; query rewriting, dynamic creation of indices for appropriate columns and static data retrieval directly from CSV files ensure efficient plan execution; effortless support for millions of columns; due to per-value typing, using mixed text/numbers data is easy; very simple network protocol provides efficient interface for MATLAB and reduces implementation time for other languages. The software is available as freeware along with educational videos on its website [4]. It doesn't need any prerequisites to run, as all of the libraries are included in the distribution package. I test it against existing database solutions using a battery of benchmarks and discuss the results.

Mynodbcsv: Lightweight Zero-Config Database Solution for Handling Very Large CSV Files

PubMed Central

Adaszewski, Stanisław

2014-01-01

Volumes of data used in science and industry are growing rapidly. When researchers face the challenge of analyzing them, their format is often the first obstacle. Lack of standardized ways of exploring different data layouts requires an effort each time to solve the problem from scratch. Possibility to access data in a rich, uniform manner, e.g. using Structured Query Language (SQL) would offer expressiveness and user-friendliness. Comma-separated values (CSV) are one of the most common data storage formats. Despite its simplicity, with growing file size handling it becomes non-trivial. Importing CSVs into existing databases is time-consuming and troublesome, or even impossible if its horizontal dimension reaches thousands of columns. Most databases are optimized for handling large number of rows rather than columns, therefore, performance for datasets with non-typical layouts is often unacceptable. Other challenges include schema creation, updates and repeated data imports. To address the above-mentioned problems, I present a system for accessing very large CSV-based datasets by means of SQL. It's characterized by: “no copy” approach – data stay mostly in the CSV files; “zero configuration” – no need to specify database schema; written in C++, with boost [1], SQLite [2] and Qt [3], doesn't require installation and has very small size; query rewriting, dynamic creation of indices for appropriate columns and static data retrieval directly from CSV files ensure efficient plan execution; effortless support for millions of columns; due to per-value typing, using mixed text/numbers data is easy; very simple network protocol provides efficient interface for MATLAB and reduces implementation time for other languages. The software is available as freeware along with educational videos on its website [4]. It doesn't need any prerequisites to run, as all of the libraries are included in the distribution package. I test it against existing database solutions using a battery of benchmarks and discuss the results. PMID:25068261

Evaluation of 1.0 mm i.d. column performances on ultra high pressure liquid chromatography instrumentation.

PubMed

Lestremau, François; Wu, Di; Szücs, Roman

2010-07-23

The present study focuses on the evaluation of 1.0 mm i.d. (internal diameter) columns on a commercial Ultra-High Pressure system. These systems have been developed specifically to operate columns with small volumes, typically 2.1 mm i.d., by reducing extra-column volume dispersion. The use of columns with smaller i.d. results in a reduced solvent consumption and required sample volume. The evaluation of the columns was carried out with samples containing neutral and pharmaceutical compounds. In isocratic mode, the extra-column volume produced additional band broadening leading to poor performances compared to equivalent 2.1 mm i.d. columns. By increasing the length of the column, the influence of the extra-column bandspreading could be reduced and 75,000 plates were obtained when four columns were coupled. In gradient mode, the effect of the extra-column contribution on efficiency was limited and about 80% of the performance of the 2.1 mm i.d. columns was obtained. Optimum conditions in gradient mode were further investigated by changing flow rate, gradient time and column length. A different approach of the calculation of peak capacity was also considered for the comparison of the influence of these different parameters. Copyright (c) 2010 Elsevier B.V. All rights reserved.

The design of a new concept chromatography column.

PubMed

Camenzuli, Michelle; Ritchie, Harald J; Ladine, James R; Shalliker, R Andrew

2011-12-21

Active Flow Management is a new separation technique whereby the flow of mobile phase and the injection of sample are introduced to the column in a manner that allows migration according to the principles of the infinite diameter column. A segmented flow outlet fitting allows for the separation of solvent or solute that elutes along the central radial section of the column from that of the sample or solvent that elutes along the wall region of the column. Separation efficiency on the analytical scale is increased by 25% with an increase in sensitivity by as much as 52% compared to conventional separations.

Fabrication and characterization of microelectromechanical systems-based gas chromatography column with embedded micro-posts for separation of environmental carcinogens.

PubMed

Sun, Jianhai; Cui, Dafu; Chen, Xing; Zhang, Lulu; Cai, Haoyuan; Li, Hui

2013-05-24

In this paper, a micro gas chromatography (μGC) column with embedded micro-posts was developed for increasing overall surface area of the columns which is able to support more of the stationary phase and reducing the effective width of the column, leading to higher separation efficiency. The proposed columns have a higher sample capacity as the overall surface area is about 3 times larger than that of open columns with the same dimensions. In order to achieve an even flow velocity in the channels, the location of the micro-posts in the linear channels and the configuration of curved channels were optimized by numerical simulation. The results have indicated that the proposed column separated 5 environmental carcinogens in less than 50s, achieved a separation efficiency of about 9500plates/m and eluted highly symmetrical Gaussian peaks. Copyright © 2013 Elsevier B.V. All rights reserved.

An on-line SPE-HPLC method for effective sample preconcentration and determination of fenoxycarb and cis, trans-permethrin in surface waters.

PubMed

Šatínský, Dalibor; Naibrtová, Linda; Fernández-Ramos, Carolina; Solich, Petr

2015-09-01

A new on-line SPE-HPLC method using fused-core columns for on-line solid phase extraction and large volume sample injection for increasing the sensitivity of detection was developed for the determination of insecticides fenoxycarb and cis-, trans-permethrin in surface waters. The separation was carried out on fused-core column Phenyl-Hexyl (100×4.6 mm), particle size 2.7 µm with mobile phase acetonitrile:water in gradient mode at flow rate 1.0 mL min(-1), column temperature 45°C. Large volume sample injection (1500 µL) to the extraction dimension using short precolumn Ascentis Express RP C-18 (5×4.6 mm); fused-core particle size 2.7 µm allowed effective sample preconcentration and efficient ballast sample matrix removal. The washing mobile phase consisting of a mixture of acetonitrile:water; 30:70, (v/v) was pumped at flow rate of 0.5 mL min(-1) through the extraction precolumn to the waste. Time of the valve switch for transferring the preconcentrated sample zone from the extraction to the separation column was set at 3rd min. Elution of preconcentrated insecticides from the extraction precolumn and separation on the analytical column was performed in gradient mode. Linear gradient elution started from 40% of acetonitrile at time of valve switch from SPE column (3rd min) to 95% of acetonitrile at 7th min. Synthetic dye sudan I was chosen as an internal standard. UV detection at wavelength 225 nm was used and the method reached the limits of detection (LOD) at ng mL(-1) levels for both insecticides. The method showing on-line sample pretreatment and preconcentration with highly sensitive determination of insecticides was applied for monitoring of fenoxycarb and both permethrin isomers in different surface water samples in Czech Republic. The time of whole analysis including on-line extraction, interferences removal, chromatography separation and system equilibration was less than 8 min. Copyright © 2015 Elsevier B.V. All rights reserved.

High-efficiency liquid chromatography on conventional columns and instrumentation by using temperature as a variable I. Experiments with 25 cm x 4.6 mm I.D., 5 microm ODS columns.

PubMed

Lestremau, François; Cooper, Andrew; Szucs, Roman; David, Frank; Sandra, Pat

2006-03-24

High plate numbers were obtained in conventional LC by coupling columns and by using temperature to reduce the viscosity of the mobile phase. At 80 degrees C up to eight columns of 25 cm x 4.6 mm I.D. packed with 5 microm ODS particles could be coupled generating 180,000 effective plates while the pressure drop was only 350bar. For routine work, a set of four columns is preferred. The analysis times on one column operated at 30 degrees C and 1 mL/min flow rate and on four columns at 80 degrees C and 2 mL/min flow rate are the same in isoeluotropic conditions while the resolution is doubled. Multicolumn systems were successfully applied in isocratic and gradient mode for the analysis of pharmaceutical and environmental samples.

Repeatability of the efficiency of columns packed with sub-3μm core-shell particles: Part III. 2.7μm Poroshell 120 EC-C18 particles in 4.6mm and 2.1mm × 100mm column formats.

PubMed

Gritti, Fabrice; Guiochon, Georges

2012-08-24

As part of an investigation of the column-to-column repeatability of the efficiency of columns packed with sub-3μm shell particles, the parameters of the mass transfer kinetics of twelve columns packed with the same batch of 2.7μm Poroshell 120 EC-C(18) particles (Agilent Technologies, Little Fall, DE, USA) were sequentially measured, using columns provided by the manufacturers that were representative of the efficiency distribution given by the quality test control. The reduced longitudinal diffusion term (B) was measured using the peak parking (PP) method; the reduced solid-liquid mass transfer resistance term (C) was given by a combination of the PP results and the most accurate model of effective diffusion in ternary composite materials. The overall eddy diffusion term (A) was obtained by subtraction of these two HETP terms from the overall reduced HETP derived from the peak moments measured by numerical integration of the entire peak profiles. The results demonstrate that the dispersion of the column efficiencies is a result of the random nature of the packing process and the eddy diffusion term resulting from the lack of homogeneity of the column bed. At the highest reduced velocity achieved for small analytes, the relative standard deviations (RSD) of the eddy diffusion term for the 2.1mm I.D. columns were ca. 3 and 11% (with average values h(eddy)= 2.5 and 13.5) for naphthalene (k=3) and uracil (k=0), respectively. For the 4.6mm I.D. columns, these RSDs were 5 and 13%, respectively, with average values h(eddy)= 1.4 and 2.9. For insulin at reduced velocities as high as 160, the RSDs of the total reduced plate heights were 3 and 8% for the 2.1 and 4.6mm I.D. columns, respectively. Copyright © 2012 Elsevier B.V. All rights reserved.

Theoretical study of the accuracy of the elution by characteristic points method for bi-langmuir isotherms.

PubMed

Ravald, L; Fornstedt, T

2001-01-26

The bi-Langmuir equation has recently been proven essential to describe chiral chromatographic surfaces and we therefore investigated the accuracy of the elution by characteristic points method (ECP) for estimation of bi-Langmuir isotherm parameters. The ECP calculations was done on elution profiles generated by the equilibrium-dispersive model of chromatography for five different sets of bi-Langmuir parameters. The ECP method generates two different errors; (i) the error of the ECP calculated isotherm and (ii) the model error of the fitting to the ECP isotherm. Both errors decreased with increasing column efficiency. Moreover, the model error was strongly affected by the weight of the bi-Langmuir function fitted. For some bi-Langmuir compositions the error of the ECP calculated isotherm is too large even at high column efficiencies. Guidelines will be given on surface types to be avoided and on column efficiencies and loading factors required for adequate parameter estimations with ECP.

E-beam column monitoring for improved CD SEM stability and tool matching

NASA Astrophysics Data System (ADS)

Hayes, Timothy S.; Henninger, Randall S.

2000-06-01

Tool matching is an important metric for in-line semiconductor metrology systems. The ability to obtain the same measurement results on two or more systems allows a semiconductor fabrication facility (fab) to deploy product in an efficient manner improving overall equipment efficiency (OEE). Many parameters on the critical dimension scanning electron microscopes (CDSEMs) can affect the long-term precision component to the tool-matching metric. One such class of parameters is related to the electron beam column stability. The alignment and condition of the gun and apertures, as well as astigmatism correction, have all been found to affect the overall measurements of the CDSEM. These effects are now becoming dominant factors in sub-3nm tool-matching criteria. This paper discusses the methodologies of column parameter monitoring and actions and controls for improving overall stability. Results have shown that column instabilities caused by contamination, gun fluctuations, component failures, detector efficiency, and external issues can be identified through parameter monitoring. The Applied Materials (AMAT) 7830 Series CDSEMs evaluated at IBM's Burlington, Vermont manufacturing facility have demonstrated 5 nm tool matching across 11 systems, which has resulted in non-dedicated product deployment and has significantly reduced cost of ownership.

Importance of the accuracy of experimental data in the nonlinear chromatographic determination of adsorption energy distributions

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

Stanley, B.J.; Guiochon, G.

1994-11-01

Adsorption energy distributions (AEDs) are calculated from the classical, fundamental integral equation of adsorption using adsorption isotherms and the expectation-maximization method of parameter estimation. The adsorption isotherms are calculated from nonlinear elution profiles obtained from gas chromatographic data using the characteristic points method of finite concentration chromatography. Porous layer open tubular capillary columns are used to support the adsorbent. The performance of these columns is compared to that of packed columns in terms of their ability to supply accurate isotherm data and AEDs. The effect of the finite column efficiency and the limited loading factor on the accuracy of themore » estimated energy distributions is presented. This accuracy decreases with decreasing efficiency, and approximately 5000 theoretical plates are needed when the loading factor, L[sub f], equals 0.56 for sampling of a unimodal Gaussian distribution. Increasing L[sub f] further increases the contribution of finite efficiency to the AED and causes a divergence at the low-energy endpoint if too high. This occurs as the retention time approaches the holdup time. Data are presented for diethyl ether adsorption on porous silica and its C-18-bonded derivative. 36 refs., 8 figs., 2 tabs.« less

The rayleigh: interpretation of the unit in terms of column emission rate or apparent radiance expressed in SI units.

PubMed

Baker, D J; Romick, G J

1976-08-01

The rayleigh, originally defined as a unit to express the total column light emission rate [10(10) photons sec(-1) (m(2)column) (-1)] can equivalently be defined as a unit for apparent photon radiance ((1/4)pi 10(10) photons sec(-1) m(-2) sr(-1)). The selection of the appropriate definition will depend upon the physical situation and the interests of the user. The applicability of the unit for expressing the quantitative measurement of all extended light sources, including optically thick media, is both handy and valid.

A novel in situ strategy for the preparation of a β-cyclodextrin/polydopamine-coated capillary column for capillary electrochromatography enantioseparations.

PubMed

Guo, Heying; Niu, Xiaoying; Pan, Congjie; Yi, Tao; Chen, Hongli; Chen, Xingguo

2017-06-01

Inspired by the chiral recognition ability of β-cyclodextrin and the natural adhesive properties of polydopamine under alkaline conditions, in this study, a rapid and in situ modification strategy was developed to fabricate β-cyclodextrin/polydopamine composite material coated-capillary columns for open tubular capillary electrochromatography. The results of scanning electron microscopy, FTIR spectroscopy, streaming potential, and electro-osmotic flow studies indicated that β-cyclodextrin/polydopamine was successfully fixed on the inner wall of the capillary column. This coating can be achieved within 1 h affording a greatly reduced capillary preparation time. The performance of the β-cyclodextrin/polydopamine-coated capillary was validated by the analysis of seven pairs of chiral analytes, namely epinephrine, norepinephrine, isoprenaline, terbutaline, verapamil, tryptophane, carvedilol. Good enantioseparation efficiencies were achieved for all. For three consecutive runs, the relative standard deviations for the migration times of the analytes for intraday, interday, and column-to-column repeatability were in the range of 0.41-1.74, 1.03-4.18, and 1.66-8.24%, respectively. Moreover, the separation efficiency of the β-cyclodextrin/polydopamine-coated capillary column did not decrease obviously over 90 runs. The strategy should also be feasible to introduce and immobilize other chiral selectors on the inner walls surface of capillary columns. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Chemical factors influencing colloid-facilitated transport of contaminants in porous media

USGS Publications Warehouse

Roy, Sujoy B.; Dzombak, David A.

1997-01-01

The effects of colloids on the transport of two strongly sorbing solutesa hydrophobic organic compound, phenanthrene, and a metal ion, Ni2+were studied in sand-packed laboratory columns under different pH and ionic strength conditions. Two types of column experiments were performed as follows:  (i) sorption/mobilization experiments where the contaminant was first sorbed in the column under conditions where no colloids were released and mobilized under conditions where colloids were released as a result of ionic strength reduction in the influent; and (ii) transport experiments where the contaminant, dissolved or sorbed on colloids, was injected into columns packed with a strongly sorbing porous medium. In the first type of experiment, contaminant mobilization was significant only when all releasable colloids were flushed from the column. In all other cases, although high colloid particle concentrations were encountered, there was no marked effect on total contaminant concentrations. In the second type of experiment, colloid deposition efficiencies were shown to control the enhancement of transport. The deposition efficiency was a function of the pH (for a high organic content sand) and of the contaminant concentration (for a charged species such as Ni2+).

Deflection of natural oil droplets through the water column in deep-water environments: The case of the Lower Congo Basin

NASA Astrophysics Data System (ADS)

Jatiault, Romain; Dhont, Damien; Loncke, Lies; de Madron, Xavier Durrieu; Dubucq, Dominique; Channelliere, Claire; Bourrin, François

2018-06-01

Numerous recurrent seep sites were identified in the deep-water environment of the Lower Congo Basin from the analysis of an extensive dataset of satellite-based synthetic-aperture radar images. The integration of current data was used to link natural oil slicks with active seep-related seafloor features. Acoustic Doppler current profiler measurements across the water column provided an efficient means to evaluate the horizontal deflection of oil droplets rising through the water column. Eulerian propagation model based on a range of potential ascension velocities helped to approximate the path for rising oil plume through the water column using two complementary methods. The first method consisted in simulating the reversed trajectory of oil droplets between sea-surface oil slick locations observed during current measurements and seep-related seafloor features while considering a range of ascension velocities. The second method compared the spatial spreading of natural oil slicks from 21 years of satellite monitoring observations for water depths ranging from 1200 to 2700 m against the modeled deflections during the current measurement period. The mapped oil slick origins are restricted to a 2.5 km radius circle from associated seep-related seafloor features. The two methods converge towards a range of ascension velocities for oil droplets through the water column, estimated between 3 and 8 cm s-1. The low deflection values validate that the sub-vertical projection of the average surface area of oil slicks at the sea surface can be used to identify the origin of expelled hydrocarbon from the seafloor, which expresses as specific seafloor disturbances (i.e. pockmarks or mounds) known to expel fluids.

Recent advances in monolithic columns for protein and peptide separation by capillary liquid chromatography.

PubMed

Liang, Yu; Zhang, Lihua; Zhang, Yukui

2013-03-01

Capillary liquid chromatography (cLC) has great potential for protein and peptide separation, with advantages of high efficiency, high resolution, low sample consumption, and high sensitivity when coupled with mass spectrometry. In recent years, monoliths have been widely used as the stationary phases for capillary columns, owing to easy preparation, high permeability, fast mass transfer, and low backpressure. This review summarizes recent advances (2007-2012) in monolithic columns for protein and peptide separation by cLC. After a brief introduction on the preparation of monolithic capillary columns, the emphasis of this review is focused on the recent application of such columns for protein and peptide separation by cLC. Furthermore, the challenges and potential hot points of monolithic capillary columns in the future are discussed.

One-pot preparation of a sulfamethoxazole functionalized affinity monolithic column for selective isolation and purification of trypsin.

PubMed

Xiao, Yuan; Guo, Jialiang; Ran, Danni; Duan, Qianqian; Crommen, Jacques; Jiang, Zhengjin

2015-06-26

A facile and efficient "one-pot" copolymerization strategy was used for the preparation of sulfonamide drug (SA) functionalized monolithic columns. Two novel SA-immobilized methacrylate monolithic columns, i.e. poly(GMA-SMX-co-EDMA) and poly(GMA-SAA-co-EDMA) were prepared by one-pot in situ copolymerization of the drug ligand (sulfamethoxazole (SMX) or sulfanilamide (SAA)), the monomer (glycidyl methacrylate, GMA) and the cross-linker (ethylene dimethacrylate, EDMA) within 100 μm i.d. capillaries under optimized polymerization conditions. The physicochemical properties and column performance of the fabricated monolithic columns were characterized by elemental analysis, scanning electron microscopy and micro-HPLC. Satisfactory column permeability, efficiency and separation performance were obtained on the optimized poly(GMA-SMX-co-EDMA) monolithic column for small molecules, such as a standard test mixture and eight aromatic ketones. Notably, it was found that the poly(GMA-SMX-co-EDMA) monolith showed a selective affinity to trypsin, while the poly(GMA-SAA-co-EDMA) monolith containing sulfanilamide did not exhibit such affinity at all. This research not only provides a novel monolith for the selective isolation and purification of trypsin, but it also offers the possibility to easily prepare novel drug functionalized methacrylate monoliths through a one-pot copolymerization strategy. Copyright © 2015 Elsevier B.V. All rights reserved.

Long-chain alkylimidazolium ionic liquids, a new class of cationic surfactants coated on ODS columns for anion-exchange chromatography.

PubMed

Qiu, Hongdeng; Zhang, Qinghua; Chen, Limei; Liu, Xia; Jiang, Shengxiang

2008-08-01

Separations of common inorganic anions were carried out on ODS columns coated with two long-chain alkylimidazolium ionic liquids ([C(12)MIm]Br and [C(14)MIm]Br) as new cationic surfactants for ion chromatography. With phthalate buffer solution as the mobile phases and non-suppressed conductivity detection, high column efficiencies and excellent selectivity were obtained in the separation of inorganic anions. Chromatographic parameters are calculated and the results show that the coated column possesses significant potential for the analysis of some inorganic anions such as CH(3)COO(-), IO(3)(-), Cl(-), BrO(3)(-), NO(2)(-), Br(-), NO(3)(-), SO(4)(2-), I(-), BF(4)(-), and SCN(-). The effect of eluent pH values on the separation of anions has been studied on the column coated with [C(12)MIm]Br. The stability of the coated columns was also examined.

StatSTEM: An efficient approach for accurate and precise model-based quantification of atomic resolution electron microscopy images.

PubMed

De Backer, A; van den Bos, K H W; Van den Broek, W; Sijbers, J; Van Aert, S

2016-12-01

An efficient model-based estimation algorithm is introduced to quantify the atomic column positions and intensities from atomic resolution (scanning) transmission electron microscopy ((S)TEM) images. This algorithm uses the least squares estimator on image segments containing individual columns fully accounting for overlap between neighbouring columns, enabling the analysis of a large field of view. For this algorithm, the accuracy and precision with which measurements for the atomic column positions and scattering cross-sections from annular dark field (ADF) STEM images can be estimated, has been investigated. The highest attainable precision is reached even for low dose images. Furthermore, the advantages of the model-based approach taking into account overlap between neighbouring columns are highlighted. This is done for the estimation of the distance between two neighbouring columns as a function of their distance and for the estimation of the scattering cross-section which is compared to the integrated intensity from a Voronoi cell. To provide end-users this well-established quantification method, a user friendly program, StatSTEM, is developed which is freely available under a GNU public license. Copyright © 2016 Elsevier B.V. All rights reserved.

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

PubMed

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

2015-01-30

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

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

PubMed

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

2014-07-18

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

Efficiency for unretained solutes in packed column supercritical fluid chromatography. I. Theory for isothermal conditions and correction factors for carbon dioxide.

PubMed

Poe, Donald P

2005-06-17

A general theory for efficiency of nonuniform columns with compressible mobile phase fluids is applied to the elution of an unretained solute in packed-column supercritical fluid chromatography (pSFC). The theoretical apparent plate height under isothermal conditions is given by the Knox equation multiplied by a compressibility correction factor f1, which is equal to the ratio of the temporal-to-spatial average densities of the mobile phase. If isothermal conditions are maintained, large pressure drops in pSFC should not result in excessive efficiency losses for elution of unretained solutes.

Fused-core particle technology as an alternative to sub-2-microm particles to achieve high separation efficiency with low backpressure.

PubMed

Cunliffe, Jennifer M; Maloney, Todd D

2007-12-01

Fused-Core particles have recently been introduced as an alternative to using sub-2-microm particles in chromatographic separations. Fused-Core particles are composed of a 1.7 microm solid core surrounded by a 0.5 microm porous silica layer (d(p) = 2.7 microm) to reduce mass transfer and increase peak efficiency. The performance of two commercially available Fused-Core particles (Advanced Materials Technology Halo C18 and Supelco Ascentis Express C18) was compared with sub-2-microm particles from Waters, Agilent, and Thermo Scientific. Although the peak efficiencies were only approximately 80% of those obtained by the Waters Acquity particles, the 50% lower backpressure allowed columns to be coupled in series to increase peak efficiency to 92,750 plates. The low backpressure and high efficiencies of the Fused-Core particles offer a viable alternative to using sub-2-microm particles and very-high-pressure LC instrumentation.

Chlorophenol degradation in soil columns inoculated with Anthracophyllum discolor immobilized on wheat grains.

PubMed

Diez, M C; Gallardo, F; Tortella, G; Rubilar, O; Navia, R; Bornhardt, C

2012-03-01

The white-rot fungus Anthracophyllum discolor immobilized on wheat grains was evaluated for chlorophenol (2,4-dichlorophenol, 2,4,6-trichlorophenol and pentachlorophenol) degradation in allophanic soil columns activated by acidification. Columns without inoculation were used as the control to evaluate the adsorption capacity of the soil columns. The chlorophenols were removed efficiently in soil columns by both adsorption and degradation processes. In inoculated soil columns, 2,4-dichlorophenol was highly degraded and this degradation is associated with a high production of manganese peroxidase. 2,4,6-trichlorophenol was degraded to a lesser extent compared with 2,4-dichlorophenol. Pentachlorophenol was first removed by adsorption and then through degradation by the fungus. Manganese peroxidase activity was lowest when the column was fed with pentachlorophenol and highest when the column was fed with 2,4-dichlorophenol. Laccase was also produced by the fungus but to a lesser degree. Copyright © 2010 Elsevier Ltd. All rights reserved.

Controlled irrigation of a structured packing as a method for increasing the efficiency of liquid mixture separation in the distillation column

NASA Astrophysics Data System (ADS)

Pavlenko, A. N.; Zhukov, V. E.; Pecherkin, N. I.; Nazarov, A. D.; Li, X.; Li, H.; Gao, X.; Sui, H.

2017-09-01

The use of modern structured packing in the distillation columns allows much more even distribution of the liquid film over the packing surface, but it does not completely solve the problem of uniform distribution of flow parameters over the entire height of the packing. Negative stratification of vapor along the packing height caused by different densities of vapor mixture components and higher temperature in the lower part of the column leads to formation of large-scale maldistributions of temperature and mixture composition over the column cross-section even under the conditions of uniform irrigation of packing with liquid. In these experiments, the idea of compensatory action of liquid distributor on the large-scale maldistribution of mixture composition over the column cross-section was implemented. The experiments were carried out in the distillation column with the diameter of 0.9 m on 10 layers of the Mellapak 350Y packing with the total height of 2.1 m. The mixture of R-21 and R-114 was used as the working mixture. To irrigate the packing, the liquid distributorr with 126 independently controlled solenoid valves overlapping the holes with the diameter of 5 mm, specially designed by the authors, was used. Response of the column to the action of liquid distributor was observed in real time according to the indications of 3 groups of thermometers mounted in 3 different cross-sections of the column. The experiments showed that the minimal correction of the drip point pattern in the controlled liquid distributor can significantly affect the pattern of flow parameter distribution over the cross-section and height of the mass transfer surface and increase separation efficiency of the column within 20%.

Water column particulate matter: A key contributor to phosphorus regeneration in a coastal eutrophic environment, the Chesapeake Bay: Particulate phosphorus in the Chesapeake Bay

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

Li, Jiying; Reardon, Patrick; McKinley, James P.

Particulate phosphorus (PP) in the water column is an essential component of phosphorus (P) cycling in aquatic ecosystems yet its composition and transformations remain largely uncharacterized. To understand the roles of suspended particulates on regeneration of inorganic P (Pi) into the water column as well as sequestration into more stable mineral precipitates, we studied seasonal variation in both organic and inorganic P speciation in suspended particles in three sites in the Chesapeake Bay using sequential P extraction, 1D (31P) and 2D (1H-31P) nuclear magnetic resonance (NMR) spectroscopies, and electron microprobe analyses (EMPA). Remineralization efficiency of particulate P average 8% andmore » 56% in shallow and deep sites respectively, suggesting the importance of PP remineralization is in resupplying water column Pi. Strong temporal and spatial variability of organic P composition, distributions, and remineralization efficiency were observed relating to water column parameters such as temperature and redox conditions: concentration of orthophosphate monoesters and diesters, and diester-to-monoester (D/M) ratios decreased with depth. Both esters and the D/M ratios were lower in the hypoxic July and September. In contrast, pyrophosphate and orthophosphate increased with depth, and polyphosphates was high in the anoxic water column. Sequential extraction and EMPA analyses of the suspended particles suggest presence of Ca-bound phosphate in the water column. We hypothesize authigenic precipitation of carbonate fluorapatite and/or its precursor mineral(s) in Pi rich water column, supported by our thermodynamic calculations. Our results, overall, reveal the important role suspended particles play in P remineralization and P sequestration in the Chesapeake Bay water column, provide important implications on P bioavailability and P sinks in similar eutrophic coastal environments.« less

High performance liquid chromatography column efficiency enhancement by zero dead volume recycling and practical approach using park and recycle arrangement.

PubMed

Minarik, Marek; Franc, Martin; Minarik, Milan

2018-06-15

A new instrumental approach to recycling HPLC is described. The concept is based on fast reintroduction of incremental peak sections back onto the separation column. The re-circulation is performed within a closed loop containing only the column and two synchronized switching valves. By having HPLC pump out of the cycle, the method minimizes peak broadening due to dead volume. As a result the efficiency is dramatically increased allowing for the most demanding analytical applications. In addition, a parking loop is employed for temporary storage of analytes from the middle section of the separated mixture prior to their recycling. Copyright © 2018 Elsevier B.V. All rights reserved.

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

PubMed

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

2018-02-23

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

Reset noise suppression in two-dimensional CMOS photodiode pixels through column-based feedback-reset

NASA Technical Reports Server (NTRS)

Pain, B.; Cunningham, T. J.; Hancock, B.; Yang, G.; Seshadri, S.; Ortiz, M.

2002-01-01

We present new CMOS photodiode imager pixel with ultra-low read noise through on-chip suppression of reset noise via column-based feedback circuitry. The noise reduction is achieved without introducing any image lag, and with insignificant reduction in quantum efficiency and full well.

Hybrid Sargassum-sand sorbent: a novel adsorbent in packed column to treat metal-bearing wastewaters from inductively coupled plasma-optical emission spectrometry.

PubMed

Vijayaraghavan, K; Joshi, U M

2013-01-01

Laboratory batch and column experiments were carried out to examine the efficiency of algal-based treatment technique to clean-up wastewaters emanating from inductively coupled plasma-optical emission spectrometry (ICP-OES). Chemical characterization revealed the extreme complexity of the wastewater, with the presence of 14 different metals under very low pH (pH = 1.1), high conductivity (6.98 mS/cm), total dissolved solid (4.46 g/L) and salinity (3.77). Batch experiments using Sargassum biomass indicated that it was possible to attain high removal efficiencies at optimum pH of 4.0. Efforts were also made to continuously treat ICP-OES wastewater using up-flow packed column. However, swelling of Sargassum biomass leads to stoppage of column. To address the problem, Sargassum was mixed with sand at a ratio of 40: 60 on volume basis. Remarkably, the hybrid Sargassum-sand sorbent showed very high removal efficiency towards multiple metal ions with the column able to operate for 11 h at a flow rate of 10 mL/min. Metal ions such as Cu, Cd, and Pb were only under trace levels in the treated water until 11 h. The results of the treatment process were compared with trade effluent discharge standards. Further the process evaluation and cost analysis were presented.

Fabrication and investigation of electrochromatographic columns with a simplex configuration.

PubMed

Liu, Qing; Yang, Lijun; Wang, Qiuquan; Zhang, Bo

2014-07-04

Duplex capillary columns with a packed and an open section are widely used in electrochromatography (CEC). The duplex column configuration leads to non-uniform voltage drop, electrical field distribution and separation performance. It also adds to the complexity in understanding and optimizing electrochromatographic process. In this study, we introduced a simplex column configuration based on single particle fritting technology. The new column configuration has an essentially uniform packed bed through the entire column length, with only 1mm length left unpacked serving as the optical detection window. The study shows that a simplex column has higher separation efficiency than a duplex column, especially at the high voltage range, due to the consistent distribution of electrical field over the column length. In comparison to the duplex column, the simplex column presented a lower flow rate at the same applied voltage, suggesting that an open section may support a higher speed than a packed section. In practice, the long and short ends of the simplex column could be used as independent CEC columns respectively. This "two-in-one" bi-functional column configuration provided extra flexibilities in selecting and optimizing electrochromatographic conditions. Copyright © 2014 Elsevier B.V. All rights reserved.

Mass transfer resistance in narrow-bore columns packed with 1.7 microm particles in very high pressure liquid chromatography.

PubMed

Gritti, Fabrice; Guiochon, Georges

2010-07-30

Surprisingly, the mass transfer kinetic properties of columns packed with superficially porous particles are markedly different from those of columns packed with fully porous particles. The performances of 2.1mmx150mm columns packed with a new type of sub-2microm particles, the superficially porous 1.7microm Kinetex-C(18), and with the classical 1.7microm BEH-C(18) fully porous particles were measured and are discussed. The sample was naphtho[2,3-a]pyrene; the use of different mobile phase compositions allowed a comparison between data measured with retention factors of k(') approximately 2 and k(') approximately 20. The minimum reduced height equivalent to a theoretical plate (HETP) of the two columns were similar, at h(min)=2.0. However, this minimum HETP was observed at a markedly shorter reduced linear velocity for the column packed with totally porous particles, between 5 and 7 for BEH, than for the one packed with shell particles, between 8 and 10 for Kinetex. This result is explained by the combination of (1) a 35% smaller B term for the Kinetex column than for the BEH column, due to the 37% lower porous volume of the former; (2) a larger reduced A term for the Kinetex column (1.6), showing a relatively poorly packed column with significant trans-column velocity biases than for the BEH column (ca. 1.0); and (3) a much lesser dependance of the efficiency on the mobile phase velocity at high velocities for the Kinetex than for the BEH column, when these columns are placed in the oven of the instrument under still-air conditions. The heat friction affects significantly more the efficiency of the BEH column than that of the Kinetex column. This unexpected result is accounted for by the three times smaller heat conductivity of the BEH bed (lambda(BEH) approximately 0.25 W/m/K) than that of the Kinetex bed (lambda(Kinetex) approximately 0.75W/m/K).

Stiffening of short small-size circular composite steel–concrete columns with shear connectors

PubMed Central

Younes, Sherif M.; Ramadan, Hazem M.; Mourad, Sherif A.

2015-01-01

An experimental program was conducted to investigate the effect of shear connectors’ distribution and method of load application on load–displacement relationship and behavior of thin-walled short concrete-filled steel tube (CFT) columns when subjected to axial load. The study focused on the compressive strength of the CFT columns and the efficiency of the shear stud in distribution of the load between the concrete core and steel tube. The study showed that the use of shear connectors enhanced slightly the axial capacity of CFT columns. It is also shown that shear connectors have a great effect on load distribution between the concrete and steel tubes. PMID:27222757

Efficiency gain limits of the parallel segmented inlet and outlet flow concept in analytical liquid chromatography columns suffering from radial transcolumn packing density gradients.

PubMed

Broeckhoven, Ken; Desmet, Gert

2012-10-05

The maximal gain in efficiency that can be expected from the use of the segmented column end fittings that were recently introduced to alleviate the effect of transcolumn packing density gradients has been quantified and generalized using numerical computations of the band broadening process. It was found that, for an unretained compound in a column with a parabolic packing density gradient, the use of a segmented inlet or a segmented outlet allows to eliminate about 60-100% of the plate height contribution (H(tc)) originating from a parabolic transcolumn velocity gradient in a d(c)=4.6 mm column. In a d(c)=2.1 mm column, these percentages change from 10 to 100%. Using a combined segmented in- and outlet, H(tc) can be reduced by about 90-100% (d(c)=4.6 mm column) or 20-100% (d(c)=2.1 mm column). The strong variation of these gain percentages is due to fact that they depend very strongly on the column length and the flow rate. Dimensionless graphs have been established that allow to directly quantify the effect for each specific case. It was also found that, in agreement with one's physical intuition, trans-column velocity profiles that are more flat in the central region benefit more from the concept than sharp, parabolic-like profiles. The gain margins furthermore tend to become smaller with increasing retention and increasing diffusion coefficient. Copyright © 2012 Elsevier B.V. All rights reserved.

Accurate measurements of the true column efficiency and of the instrument band broadening contributions in the presence of a chromatographic column.

PubMed

Gritti, Fabrice; Guiochon, Georges

2014-01-31

A rapid and simple validated experimental protocol is proposed for the accurate determination of the true intrinsic column efficiency and for that of the variance of the extra-column volume of the instrument used, the latter being obtained without requiring the removal of the chromatographic column from the HPLC system. This protocol was applied to 2.1mm×100mm columns packed with sub-3 (2.7μm Halo Peptide ES-C18) and sub-2μm (1.6μm prototype) core-shell particles. It was validated by observing the linear behavior of the plot of the apparent column plate height versus the reciprocal of (1+k')(2) for at least three homologous compounds, with a linear regression coefficient R(2) larger than 0.999. Irrespective of the contribution of the several, different instruments used to the total band broadening, the same column HETP value was obtained within 5%. This new protocol outperform the classical one in which the chromatographic column is replaced with a zero dead volume (ZDV) union connector to measure the extra-column volume variance, which is subtracted from the variance measured with the column to measure the intrinsic HETP. This protocol fails because it significantly underestimates the system volume variance. Copyright © 2013 Elsevier B.V. All rights reserved.

Controlling the column spacing in isothermal magnetic advection to enable tunable heat and mass transfer.

DOE PAGES

Solis, Kyle Jameson; Martin, James E.

2012-11-01

Isothermal magnetic advection is a recently discovered method of inducing highly organized, non-contact flow lattices in suspensions of magnetic particles, using only uniform ac magnetic fields of modest strength. The initiation of these vigorous flows requires neither a thermal gradient nor a gravitational field and so can be used to transfer heat and mass in circumstances where natural convection does not occur. These advection lattices are comprised of a square lattice of antiparallel flow columns. If the column spacing is sufficiently large compared to the column length, and the flow rate within the columns is sufficiently large, then one wouldmore » expect efficient transfer of both heat and mass. Otherwise, the flow lattice could act as a countercurrent heat exchanger and only mass will be efficiently transferred. Although this latter case might be useful for feeding a reaction front without extracting heat, it is likely that most interest will be focused on using IMA for heat transfer. In this paper we explore the various experimental parameters of IMA to determine which of these can be used to control the column spacing. These parameters include the field frequency, strength, and phase relation between the two field components, the liquid viscosity and particle volume fraction. We find that the column spacing can easily be tuned over a wide range, to enable the careful control of heat and mass transfer.« less

Converter slag-coal cinder columns for the removal of phosphorous and other pollutants.

PubMed

Yang, Jian; Wang, Su; Lu, Zhibo; Yang, Jian; Lou, Shanjie

2009-08-30

A mixture of converter slag and coal cinder as adsorbent for the removal of phosphorous and other pollutants was studied in the paper. The maximum P adsorption capacity, pH of solution, contact time and initial phosphate concentration were evaluated in batch experiments for the two materials firstly. The data of P sorption were best fitted to Langumir equation, and the maximum adsorption capacities of converter slag and coal cinder were 2.417 and 0.398 mg P/g, respectively. The pH of solutions with converter slag and coal cinder changed dramatically with time and closed to 8 in 8h, and the influence of initial pH on phosphate removal by coal cinder was more significant than by converter slag. Phosphate removal rate by converter slag decreased with increase of initial phosphate concentrations. Subsequently, two flow-through columns (Column 1#, V(converter slag):V(coal cinder)=1:5; Column 2#, V(converter slag):V(coal cinder)=1:3) were operated for the removal of phosphorous and other pollutants from the effluents of a vermifilter for nearly eleven months. Results indicated the average removal efficiency of total phosphorus, dissolved phosphorus, COD and NH(4)(+)-N by Column 1# were 44%, 56%, 31% and 67%, and by Column 2# were 42%, 54%, 24% and 57%, respectively. Column 1# had higher removal efficiency for P and other pollutants.

The impact analysis of the connecting pipe length and diameter on the operation of a piston hybrid power machine of positive displacement with gas suction capacity

NASA Astrophysics Data System (ADS)

Shcherba, V. E.; Grigoriev, A. V.; Averyanov, G. S.; Surikov, V. I.; Vedruchenko, V. P.; Galdin, N. S.; Trukhanova, D. A.

2017-08-01

The article analyzes the impact of the connecting liquid pipe length and diameter on consumables and power characteristics of the piston hybrid power machine with gas suction capacity. The following operating characteristics of the machine were constructed and analyzed: the average height of the liquid column in the jacket space; instantaneous velocity and height of the liquid column in the jacket space; the relative height of the liquid column in the jacket space; volumetric efficiency; indicator isothermal efficiency; flowrate in the pump section; relative pressure losses during suction; relative flowrate. The dependence of the instantaneous pressure in the work space and the suction space of the compressor section on the rotation angle of the crankshaft is determined for different values of the length and diameter of the connecting pipeline.

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

PubMed

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

2015-05-22

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

Repeatability of the efficiency of columns packed with sub-3μm core-shell particles: Part I. 2.6μm Kinetex-C(18) particles in 4.6mm and 2.1mm×100mm column formats.

PubMed

Gritti, Fabrice; Guiochon, Georges

2012-08-24

The column-to-column repeatability of the mass transfer mechanism in columns packed with sub-3μm shell particles was investigated. The parameters of this mechanism were measured for twelve columns (six 2.1mm×100mm and six 4.6mm×100mm) packed with the same batch of 2.6μm Kinetex-C(18) particles (Phenomenex, CA, USA). For both series, the manufacturer provided columns at different positions in the efficiency distribution given by the quality test control. Three compounds were used, uracil, naphthalene and insulin. The reduced longitudinal diffusion term was measured with the peak parking (PP) method, the reduced solid-liquid mass transfer resistance term was given by a combination of the PP results and a model of effective diffusion in ternary composite materials (non-porous cores, concentric porous shell, and eluent matrix), validated previously. The overall eddy diffusion term was obtained by subtraction of these two HETP terms from the overall reduced HETP measured by numerical integration of the entire peak profiles. The results demonstrate that the dispersion of the column efficiencies is only due to the random nature of the packing process. At the highest reduced velocity achieved, the relative standard deviations (RSDs) of the eddy diffusion term for the 2.1mm I.D. columns were ca. 7% and 3% for the low molecular weight compounds and for insulin, respectively. For the 4.6mm I.D. columns, these RSDs were 15% and 5%, respectively. The larger RSDs for the 4.6mm I.D. columns is explained by the exceptionally low value of the eddy diffusion term. Copyright © 2012 Elsevier B.V. All rights reserved.

Effect of Non-laminar Regime on the Efficiency of a Thermal Diffusion Column. Report No. 26; INFLUENCIA DEL REGIMEN NO LAMINAR SOBRE LA EFICIENCIA DE UNA COLUMNA DE DIFUSION TERMICA. Informe No. 26

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

Espanol, C.E.

1960-01-01

The effect of the appearance of localized perturbations on the separation factor and operation time of a thermal diffusion column is studied. The separation factor of a column was obtained experimentally and the enrichment was recorded continuously as a function of time by measurement of the thermal conductivity of the gaseous mixture at the foot and head of the column. A mixture of Ar and CO/sub 2/ was used as it behaves as an isotopic mixture. The results showed the linear decrease of the separation factor with the number of stages and the operation time practically does not vary. Themore » introduction of localized turbulences in a thermal diffusion column reduces the column yield. (J.S.R.)« less

Stability and dynamic analysis of a slender column with curved longitudinal stiffeners

NASA Technical Reports Server (NTRS)

Lake, Mark S.

1989-01-01

The results of a stability design study are presented for a slender column with curved longitudinal stiffeners for large space structure applications. Linear stability analyses are performed using a link-plate representation of the stiffeners to determine stiffener local buckling stresses. Results from a set of parametric analyses are used to determine an approximate explicit expression for stiffener local buckling in terms of its geometric parameters. This expression along with other equations governing column stability and mass are assembled into a determinate system describing minimum mass stiffened column design. An iterative solution is determined to solve this system and a computer program incorporating this routine is presented. Example design problems are presented which verify the solution accuracy and illustrate the implementation of the solution routine. Also, observations are made which lead to a greatly simplified first iteration design equation relating the percent increase in column mass to the percent increase in column buckling load. From this, generalizations are drawn as to the mass savings offered by the stiffened column concept. Finally, the percent increase in fundamental column vibration frequency due to the addition of deployable stiffeners is studied.

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

PubMed

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.

A cross-species bi-clustering approach to identifying conserved co-regulated genes.

PubMed

Sun, Jiangwen; Jiang, Zongliang; Tian, Xiuchun; Bi, Jinbo

2016-06-15

A growing number of studies have explored the process of pre-implantation embryonic development of multiple mammalian species. However, the conservation and variation among different species in their developmental programming are poorly defined due to the lack of effective computational methods for detecting co-regularized genes that are conserved across species. The most sophisticated method to date for identifying conserved co-regulated genes is a two-step approach. This approach first identifies gene clusters for each species by a cluster analysis of gene expression data, and subsequently computes the overlaps of clusters identified from different species to reveal common subgroups. This approach is ineffective to deal with the noise in the expression data introduced by the complicated procedures in quantifying gene expression. Furthermore, due to the sequential nature of the approach, the gene clusters identified in the first step may have little overlap among different species in the second step, thus difficult to detect conserved co-regulated genes. We propose a cross-species bi-clustering approach which first denoises the gene expression data of each species into a data matrix. The rows of the data matrices of different species represent the same set of genes that are characterized by their expression patterns over the developmental stages of each species as columns. A novel bi-clustering method is then developed to cluster genes into subgroups by a joint sparse rank-one factorization of all the data matrices. This method decomposes a data matrix into a product of a column vector and a row vector where the column vector is a consistent indicator across the matrices (species) to identify the same gene cluster and the row vector specifies for each species the developmental stages that the clustered genes co-regulate. Efficient optimization algorithm has been developed with convergence analysis. This approach was first validated on synthetic data and compared to the two-step method and several recent joint clustering methods. We then applied this approach to two real world datasets of gene expression during the pre-implantation embryonic development of the human and mouse. Co-regulated genes consistent between the human and mouse were identified, offering insights into conserved functions, as well as similarities and differences in genome activation timing between the human and mouse embryos. The R package containing the implementation of the proposed method in C ++ is available at: https://github.com/JavonSun/mvbc.git and also at the R platform https://www.r-project.org/ jinbo@engr.uconn.edu. © The Author 2016. Published by Oxford University Press.

PAR and UV effects on vertical migration and photosynthesis in Euglena gracilis.

PubMed

Richter, Peter; Helbling, Walter; Streb, Christine; Häder, Donat-P

2007-01-01

Recently it was shown that the unicellular flagellate Euglena gracilis changes the sign of gravitaxis from negative to positive upon excessive radiation. This sign change persists in a cell culture for hours even if subsequently transferred to dim light. To test the ecological relevance of this behavior, a vertical column experiment was performed (max. depth 65 cm) to test distribution, photosynthetic efficiency and motility in different horizons of the column (surface, 20, 40 and 65 cm). One column was covered with a UV cut-off filter, which transmits photosynthetically active radiation (PAR) only, the other with a filter which transmits PAR and UV. The columns were irradiated with a solar simulator (PAR 162 W m(-2), UV-A 32.6 W m(-2), UV-B 1.9 W m(-2)). The experiment was conducted for 10 days, normally with a light/dim light cycle of 12 h:12 h, but in some cases the light regime was changed (dim light instead of full radiation). Under irradiation the largest fraction of cells was found at the bottom of the column. The cell density decreased toward the surface. Photosynthetic efficiency, determined with a pulse amplitude modulated fluorometer, was negligible at the surface and increased toward the bottom. While the cell suspension showed a positive gravitaxis at the bottom, the cells in the 40 cm horizon were bimodally oriented (about the same percentage of cells swimming upward and downward, respectively). At 20 cm and at the surface the cells showed negative gravitaxis. Positive gravitaxis was more pronounced in the UV + PAR samples. At the surface and in the 20 and 40 cm horizons photosynthetic efficiency was better in the PAR-only samples than in the PAR + UV samples. At the bottom photosynthetic efficiency was similar in both light treatments. The data suggest that high light reverses gravitaxis of the cells, so that they move downward in the water column. At the bottom the light intensity is lower (attenuation of the water column and self shading of the cells) and the cells recover. After recovery the cells swim upward again until the negative gravitaxis is reversed again.

[Complex program for the recovery of the vertebral column motor function].

PubMed

Kukareko, V P; Furmanov, A G

2011-01-01

This paper addresses the problems pertinent to the improvement of the efficacy of restoration of the vertebral column motor function based on the implementation of a comprehensive therapeutic program including massage, thermal procedures, and physical exercises. The program was realized in three phases, viz. preparatory, basic, and consolidating. The results of integral estimation of the whole body and vertebral column condition were taken into consideration. The experiment lasted 6 months and confirmed high efficiency of the comprehensive program.

Evaluating two process scale chromatography column header designs using CFD.

PubMed

Johnson, Chris; Natarajan, Venkatesh; Antoniou, Chris

2014-01-01

Chromatography is an indispensable unit operation in the downstream processing of biomolecules. Scaling of chromatographic operations typically involves a significant increase in the column diameter. At this scale, the flow distribution within a packed bed could be severely affected by the distributor design in process scale columns. Different vendors offer process scale columns with varying design features. The effect of these design features on the flow distribution in packed beds and the resultant effect on column efficiency and cleanability needs to be properly understood in order to prevent unpleasant surprises on scale-up. Computational Fluid Dynamics (CFD) provides a cost-effective means to explore the effect of various distributor designs on process scale performance. In this work, we present a CFD tool that was developed and validated against experimental dye traces and tracer injections. Subsequently, the tool was employed to compare and contrast two commercially available header designs. © 2014 American Institute of Chemical Engineers.

Cross flow cyclonic flotation column for coal and minerals beneficiation

DOEpatents

Lai, Ralph W.; Patton, Robert A.

2000-01-01

An apparatus and process for the separation of coal from pyritic impurities using a modified froth flotation system. The froth flotation column incorporates a helical track about the inner wall of the column in a region intermediate between the top and base of the column. A standard impeller located about the central axis of the column is used to generate a centrifugal force thereby increasing the separation efficiency of coal from the pyritic particles and hydrophillic tailings.

Application of EDTA decontamination on soils affected by mining activities and impact of treatment on the geochemical partition of metal contaminants.

PubMed

Xia, Wenbin; Gao, Hui; Wang, Xianhai; Zhou, Chunhua; Liu, Yunguo; Fan, Ting; Wang, Xin

2009-05-30

Two soil samples were collected at mining areas located in southern Hunan Province, China. EDTA extraction of Pb, Zn, Cu and Cd from these two tailing soils was studied using column leaching experiments. The redistributions of heavy metals (HMs) were determined using the modified BCR (Community Bureau of Reference) sequential extraction procedure, before and after EDTA extraction. The results indicated that EDTA was an effective extractant because of its strong chelating ability for various HMs. The proportions of Pb, Zn, Cu and Cd in the four fractions varied largely after EDTA extraction. The extraction efficiency of EDTA of the acid-extractable fraction (AEX) was significant in shallow soil column, while in deeper soil column, decrease of the extraction efficiency of reduced (RED), oxidizable (OX) and residual fractions (RES) was obtained, which was mainly due to the decrease of EDTA concentration.

Bioremoval of heavy metals from industrial effluent by fixed-bed column of red macroalgae.

PubMed

Ibrahim, Wael M; Mutawie, Hawazin H

2013-02-01

Three different species of nonliving red algal biomass Laurancia obtusa, Geldiella acerosa and Hypnea sp. were used to build three types of fixed-bed column for the removal of toxic heavy metal ions such as Cu(2+), Zn(2+), Mn(2+) and Ni(2+) from industrial effluent. In general, the highest efficiency of metal ion bioremoval was recorded for algal column of L. obtusa followed by G. acerosa and the lowest one was recorded for Hypnea sp., with mean removal values of 94%, 85% and 71%, respectively. The obtained results showed that biological treatments of industrial effluents with these algal columns, using standard algal biotest, Pseudokirchneriella subcapitata, were capable of reducing effluent toxicities from 75% to 15%, respectively. Red algal column may be considered as an inexpensive and efficient alternative treatment for conventional removal technology, for sequestering heavy metal ions from industrial effluents.

Repeatability of the efficiency of columns packed with sub-3μm core-shell particles: Part II. 2.7 μm Halo-ES-Peptide-C18 particles in 4.6mm and 2.1mm×100mm column formats.

PubMed

Gritti, Fabrice; Guiochon, Georges

2012-08-24

The column-to-column repeatability of the mass transfer kinetics in columns packed with sub-3μm shell particles was investigated. The parameters of this kinetics were measured for twelve columns (six 2.1mm×100mm and six 4.6mm×100mm) packed with the same batch of 2.7μm Halo-ES-Peptide-C(18) particles (Advanced Material Technologies, Wilmington, DE, USA). For both series, the manufacturer provided columns at different positions in the efficiency distribution given by the quality test control. Three compounds were used, uracil, naphthalene and insulin. The reduced longitudinal diffusion term was measured with the peak parking (PP) method; the reduced solid-liquid mass transfer resistance term was given by a combination of the PP results and the most accurate model of effective diffusion in ternary composite materials (non-porous cores, concentric porous shell, and eluent matrix), validated previously. The overall eddy diffusion term was obtained by subtraction of these two HETP terms from the overall reduced HETP measured by numerical integration of the entire peak profiles. The results demonstrate that the dispersion of the column efficiencies is mostly due to the random nature of the packing process and the associated eddy diffusion term. At the highest reduced velocity achieved, the relative standard deviations (RSDs) of the eddy diffusion term for the 2.1mm I.D. columns were ca. 5 and 10% (with average values A(ν)=2.3 and 8.5) for naphthalene and uracil, respectively. For the 4.6mm I.D. columns, these RSDs were 3 and 5%, respectively, with average values A(ν)=1.5 and 2.7. Copyright © 2012 Elsevier B.V. All rights reserved.

Parasagittal compartmentation of cerebellar mossy fibers as revealed by the patterned expression of vesicular glutamate transporters VGLUT1 and VGLUT2.

PubMed

Gebre, Samrawit A; Reeber, Stacey L; Sillitoe, Roy V

2012-04-01

The cerebellum receives sensory signals from spinocerebellar (lower limbs) and dorsal column nuclei (upper limbs) mossy fibers. In the cerebellum, mossy fibers terminate in bands that are topographically aligned with stripes of Purkinje cells. While much is known about the molecular heterogeneity of Purkinje cell stripes, little is known about whether mossy fiber compartments have distinct molecular profiles. Here, we show that the vesicular glutamate transporters VGLUT1 and VGLUT2, which mediate glutamate uptake into synaptic vesicles of excitatory neurons, are expressed in complementary bands of mossy fibers in the adult mouse cerebellum. Using a combination of immunohistochemistry and anterograde tracing, we found heavy VGLUT2 and weak VGLUT1 expression in bands of spinocerebellar mossy fibers. The adjacent bands, which are in part comprised of dorsal column nuclei mossy fibers, strongly express VGLUT1 and weakly express VGLUT2. Simultaneous injections of fluorescent tracers into the dorsal column nuclei and lower thoracic-upper lumbar spinal cord revealed that upper and lower limb sensory pathways innervate adjacent VGLUT1/VGLUT2 parasagittal bands. In summary, we demonstrate that VGLUT1 and VGLUT2 are differentially expressed by dorsal column nuclei and spinocerebellar mossy fibers, which project to complementary cerebellar bands and respect common compartmental boundaries in the adult mouse cerebellum.

Preliminary kinetic evaluation of an immobilized polysaccharide sub-2μm column using a low dispersion supercritical fluid chromatograph.

PubMed

Berger, Terry A

2017-08-11

The performance of a 3×50mm, 1.6μm d p column with an immobilized polysaccharide stationary phase (ChiralPak IA-U) was evaluated for efficiency, and pressure drop, with respect to flow rate and modifier concentration using supercritical fluid chromatography (SFC). This appears to be the first such report using such a column in SFC. A unique low dispersion (ultra-high performance) SFC was used for the evaluation. The minimum reduced plate height of 2.78, indicates that the maximum efficiency was similar to or better than coated polysaccharide columns. Selectivity was different from ChiralPak AD, with the same chiral selector, as reported by many others. At high flows and high methanol concentrations, pump pressures sometimes approached 600bar. With 5% methanol, pressure vs. flow rate was non-linear suggesting turbulent flow in the connector tubing. The optimum flow rate (F opt ) at 40% methanol was ≈0.8mL/min, where the column efficiency was highest. At 5% methanol, F opt increased to ≈1.6mL/min, but efficiency degraded noticeably. The differences in F opt suggests that the solute diffusion coefficients are a strong function of modifier concentration. Several sub-1min separations, including a 7.5s separation, are presented. Copyright © 2017 Elsevier B.V. All rights reserved.

Chromatographic properties PLOT multicapillary columns.

PubMed

Nikolaeva, O A; Patrushev, Y V; Sidelnikov, V N

2017-03-10

Multicapillary columns (MCCs) for gas chromatography make it possible to perform high-speed analysis of the mixtures of gaseous and volatile substances at a relatively large amount of the loaded sample. The study was performed using PLOT MCCs for gas-solid chromatography (GSC) with different stationary phases (SP) based on alumina, silica and poly-(1-trimethylsilyl-1-propyne) (PTMSP) polymer as well as porous polymers divinylbenzene-styrene (DVB-St), divinylbenzene-vinylimidazole (DVB-VIm) and divinylbenzene-ethylene glycol dimethacrylate (DVB-EGD). These MCCs have the efficiency of 4000-10000 theoretical plates per meter (TP/m) and at a column length of 25-30cm can separate within 10-20s multicomponent mixtures of substances belonging to different classes of chemical compounds. The sample amount not overloading the column is 0.03-1μg and depends on the features of a porous layer. Examples of separations on some of the studied columns are considered. Copyright © 2017 Elsevier B.V. All rights reserved.

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

PubMed

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.

Twist functions in vertebral column formation in medaka, Oryzias latipes.

PubMed

Yasutake, Junichi; Inohaya, Keiji; Kudo, Akira

2004-07-01

Medaka twist, a basic helix-loop-helix (bHLH) transcription factor, is expressed in the sclerotome during embryogenesis. We previously established a line of twist-EGFP transgenic medaka, whose EGFP expression is regulated by the twist promoter; therefore, we could observe the behavior of sclerotomal cells in vivo. In the transgenic medaka embryos, EGFP-positive sclerotomal cells migrated dorsally around the notochord and the neural tube, where at a later stage the vertebral column would be formed. This finding strongly suggests that twist-expressing sclerotomal cells participate in vertebral column formation in medaka. To clarify the function of twist gene in the sclerotome, we performed knockdown analysis of twist by using two kinds of morpholino antisense oligonucleotides targeted against twist (MO1 and MO2). Both the MO1 and MO2 morphants exhibited absence of neural arches, which are bilaterally paired, dorsomedially oriented bones on the dorsal aspect of the centrum. In addition, MO2, which blocks translation of only endogenous twist mRNA in the twist-EGFP transgenic medaka, did not affect the migration pattern of EGFP-positive cells, revealing that the migration of sclerotome-derived cells were normal in the absence of twist gene function. These results demonstrate that medaka twist functions in vertebral column formation by regulating the sclerotomal cell differentiation.

Process development and economic evaluation of recombinant human lactoferrin expressed in rice grain.

PubMed

Nandi, Somen; Yalda, Dorice; Lu, Stephen; Nikolov, Zivko; Misaki, Ryo; Fujiyama, Kazuhito; Huang, Ning

2005-06-01

In this paper, we show that recombinant human lactoferrin (rhLF) has been stably expressed at 0.5% brown rice flour weight for nine generations. Process development indicates that rhLF can be efficiently extracted from rice flour in 20 mM phosphate buffer (pH 7.0) containing up to 0.5 M NaCl and at a ratio of 1 kg flour to 10 L buffer. After solid/liquid separation, the extract can then be loaded directly onto an ion-exchange column and rhLF can be eluted using 0.8 M NaCl. The resulting rhLF is about 95% pure. A range of biochemical and biophysical analyses were carried out and results indicated that the purified rhLF was identical to its native human counterpart other than its glycosylation. Economic analysis shows that at 600 kg/year scale, the cash cost to produce 1 g of rhLF of pharmaceutical grade is US$ 5.90. Analysis also indicates that the expression level has profound impact on costs related to planting, milling, extraction and purification, thus high level expression of recombinant protein in plants is one of the key parameters for the success of plant made pharmaceuticals.

Influence of soil moisture on sunflower oil extraction of polycyclic aromatic hydrocarbons from a manufactured gas plant soil.

PubMed

Gong, Zongqiang; Wilke, B-M; Alef, Kassem; Li, Peijun

2005-05-01

The influence of soil moisture on efficiency of sunflower oil extraction of polycyclic aromatic hydrocarbons (PAHs) from contaminated soil was investigated. The PAH-contaminated soil was collected from a manufactured gas plant (MGP) site in Berlin, Germany. Half of the soil was air-dried, and the other half was kept as field-moist soil. Batch experiments were performed using air-dried and field-moist soils, and sunflower oil was used as extractant at oil/soil ratios of 2:1 and 1:1 (v/m). The experimental data were fitted to a first-order empirical model to describe mass-transfer profiles of the PAHs. Column extraction experiments were also conducted. Field-moist and air-dried soils in the column were extracted using sunflower oil at an oil/soil ratio of 2:1. In the batch experiments, PAHs were more rapidly extracted from air-dried soil than from field-moist soil. Removal rate of total PAH increased 23% at oil/soil ratio of 1:1 and 15.5% at oil/soil ratio of 2:1 after the soil was air dried. The most favorable conditions for batch extraction were air-dried soil, with an oil/soil ratio of 2:1. In the column experiments, the removal rate of total PAH from air-dried soil was 30.7% higher than that from field-moist soil. For field-moist soil, extraction efficiencies of the batch extraction (67.2% and 81.5%) were better than that for column extraction (65.6%). However, this difference between the two methods became less significant for the air-dried soil, with a total removal rate of 96.3% for column extraction and 90.2% and 97% for batch extractions. A mass-balance test was carried out for analytical quality assurance. The results of both batch and column experiments indicated that drying the soil increased efficiency of extraction of PAHs from the MGP soil.

Fixed Bed Column Study for Adsolubilization of 2,4-D Herbicide on Surfactant Modified Silica Gel Waste

NASA Astrophysics Data System (ADS)

Koner, S.; Adak, A.

2012-09-01

The fixed bed column study was conducted for the removal of 2,4-dichlorophenoxyacetic acid (2,4-D), a widely used herbicide from synthetically prepared wastewater using surfactant modified silica gel waste (SMSGW) as an adsorbing media. The adsorbing media was prepared by treating silica gel waste (SGW) with cationic surfactant. The removal was due to adsolubilization of 2,4-D molecules within the admicelles formed on the surface of SGW. The column having 2.5 cm diameter, with different bed heights such as 20, 30 and 40 cm were used in the study. The different column design parameters like depth of exchange zone, time required for exchange zone to move its own height, adsorption rate constant, adsorption capacity constant were calculated using BDST model. The SMSGW was found to be a very efficient media for the removal of 2,4-D from wastewater. Column design parameters were modeled for different field conditions to predict the duration of column run for practical application.

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

PubMed

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.

Gas chromatographic column for the Viking 1975 molecular analysis experiment

NASA Technical Reports Server (NTRS)

Novotny, M.; Hayes, J. M.; Bruner, F.; Simmonds, P. G.

1975-01-01

A gas chromatographic column has been developed for use in the remote analysis of the Martian surface. The column, which utilizes a liquid-modified organic adsorbent (Tenax) as the stationary phase, provides efficient transmission and resolution of nanogram quantities of organic materials in the presence of millionfold excesses of water and carbon dioxide.

High throughput screening of active pharmaceutical ingredients by UPLC.

PubMed

Al-Sayah, Mohammad A; Rizos, Panagiota; Antonucci, Vincent; Wu, Naijun

2008-07-01

Ultra performance LC (UPLC) was evaluated as an efficient screening approach to facilitate method development for drug candidates. Three stationary phases were screened: C-18, phenyl, and Shield RP 18 with column dimensions of 150 mm x 2.1 mm, 1.7 microm, which should theoretically generate 35,000 plates or 175% of the typical column plate count of a conventional 250 mm x 4.6 mm, 5 microm particle column. Thirteen different active pharmaceutical ingredients (APIs) were screened using this column set with a standardized mobile-phase gradient. The UPLC method selectivity results were compared to those obtained for these compounds via methods developed through laborious trial and error screening experiments using numerous conventional HPLC mobile and stationary phases. Peak capacity was compared for columns packed with 5 microm particles and columns packed with 1.7 microm particles. The impurities screened by UPLC were confirmed by LC/MS. The results demonstrate that simple, high efficiency UPLC gradients are a feasible and productive alternative to more conventional multiparametric chromatographic screening approaches for many compounds in the early stages of drug development.

Approaches to characterise chromatographic column performance based on global parameters accounting for peak broadening and skewness.

PubMed

Baeza-Baeza, J J; Pous-Torres, S; Torres-Lapasió, J R; García-Alvarez-Coque, M C

2010-04-02

Peak broadening and skewness are fundamental parameters in chromatography, since they affect the resolution capability of a chromatographic column. A common practice to characterise chromatographic columns is to estimate the efficiency and asymmetry factor for the peaks of one or more solutes eluted at selected experimental conditions. This has the drawback that the extra-column contributions to the peak variance and skewness make the peak shape parameters depend on the retention time. We propose and discuss here the use of several approaches that allow the estimation of global parameters (non-dependent on the retention time) to describe the column performance. The global parameters arise from different linear relationships that can be established between the peak variance, standard deviation, or half-widths with the retention time. Some of them describe exclusively the column contribution to the peak broadening, whereas others consider the extra-column effects also. The estimation of peak skewness was also possible for the approaches based on the half-widths. The proposed approaches were applied to the characterisation of different columns (Spherisorb, Zorbax SB, Zorbax Eclipse, Kromasil, Chromolith, X-Terra and Inertsil), using the chromatographic data obtained for several diuretics and basic drugs (beta-blockers). Copyright (c) 2010 Elsevier B.V. All rights reserved.

Experimental Study on the Fire Performance of Tubular Steel Columns with Membrane Protections for Prefabricated and Modular Steel Construction

PubMed Central

Zhang, Xin; Peng, Lei; Ni, Zhao-peng; Ni, Tian-xiao; Huang, Yi-liang; Zhou, Yang

2018-01-01

Experimental research was conducted to study the fire resistance of steel tubular columns used in prefabricated and modular construction. In order to achieve high-efficient prefabrication and fast on-site installation, membrane protections using board products and thermal insulation blankets are adopted as the favorable protection method. Three protected tubular columns were tested in a full-scale column furnace with axial load applied. The study variables were different membranes, including fiber reinforced calcium silicate (FRCS) boards, rock wool and aluminum silica (Fiberfrax) insulations. The results suggest that one layer of 12 mm FRCS board with rock wool insulation has insufficient fire protection. However, steel columns protected with two layers of 12 mm FRCS boards with insulation appeared to have good fire resistances and could achieve a fire resistance rating as high as 2.5~3.0 h. PMID:29547574

Micro-fabricated packed gas chromatography column based on laser etching technology.

PubMed

Sun, J H; Guan, F Y; Zhu, X F; Ning, Z W; Ma, T J; Liu, J H; Deng, T

2016-01-15

In this work, a micro packed gas chromatograph column integrated with a micro heater was fabricated by using laser etching technology (LET) for analyzing environmental gases. LET is a powerful tool to etch deep well-shaped channels on the glass wafer, and it is the most effective way to increase depth of channels. The fabricated packed GC column with a length of over 1.6m, to our best knowledge, which is the longest so far. In addition, the fabricated column with a rectangular cross section of 1.2mm (depth) × 0.6mm (width) has a large aspect ratio of 2:1. The results show that the fabricated packed column had a large sample capacity, achieved a separation efficiency of about 5800 plates/m and eluted highly symmetrical Gaussian peaks. Copyright © 2015 Elsevier B.V. All rights reserved.

Aspartic acid incorporated monolithic columns for affinity glycoprotein purification.

PubMed

Armutcu, Canan; Bereli, Nilay; Bayram, Engin; Uzun, Lokman; Say, Rıdvan; Denizli, Adil

2014-02-01

Novel aspartic acid incorporated monolithic columns were prepared to efficiently affinity purify immunoglobulin G (IgG) from human plasma. The monolithic columns were synthesised in a stainless steel HPLC column (20 cm × 5 mm id) by in situ bulk polymerisation of N-methacryloyl-L-aspartic acid (MAAsp), a polymerisable derivative of L-aspartic acid, and 2-hydroxyethyl methacrylate (HEMA). Monolithic columns [poly(2-hydroxyethyl methacrylate-N-methacryloyl-L-aspartic acid) (PHEMAsp)] were characterised by swelling studies, Fourier transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM). The monolithic columns were used for IgG adsorption/desorption from aqueous solutions and human plasma. The IgG adsorption depended on the buffer type, and the maximum IgG adsorption from aqueous solution in phosphate buffer was 0.085 mg/g at pH 6.0. The monolithic columns allowed for one-step IgG purification with a negligible capacity decrease after ten adsorption-desorption cycles. Copyright © 2013 Elsevier B.V. All rights reserved.

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

PubMed

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

2015-08-07

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

Batch versus column modes for the adsorption of radioactive metal onto rice husk waste: conditions optimization through response surface methodology.

PubMed

Kausar, Abida; Bhatti, Haq Nawaz; Iqbal, Munawar; Ashraf, Aisha

2017-09-01

Batch and column adsorption modes were compared for the adsorption of U(VI) ions using rice husk waste biomass (RHWB). Response surface methodology was employed for the optimization of process variables, i.e., (pH (A), adsorbent dose (B), initial ion concentration (C)) in batch mode. The B, C and C 2 affected the U(VI) adsorption significantly in batch mode. The developed quadratic model was found to be validated on the basis of regression coefficient as well as analysis of variance. The predicted and actual values were found to be correlated well, with negligible residual value, and B, C and C 2 were significant terms. The column study was performed considering bed height, flow rate and initial metal ion concentration, and adsorption efficiency was evaluated through breakthrough curves and bed depth service time and Thomas models. Adsorption was found to be dependent on bed height and initial U(VI) ion concentration, and flow rate decreased the adsorption capacity. Thomas models fitted well to the U(VI) adsorption onto RHWB. Results revealed that RHWB has potential to remove U(VI) ions and batch adsorption was found to be efficient versus column mode.

Separation and purification of fructooligosaccharides on a zeolite fixed-bed column.

PubMed

Kuhn, Raquel Cristine; Mazutti, Marcio Antonio; Maugeri Filho, Francisco

2014-04-01

Fructooligosaccharides (FOS), a well-known prebiotic product, are obtained by enzymatic synthesis and consist of a mixture of mono- and disaccharides. In this work, a methodology for their separation and purification was developed using a zeolite fixed-bed column. The effects of column temperature (40-60°C), eluent flow rate (0.10-0.14 mL/min), injected to bed volume percent ratio (2.6-5.1%), and ethanol concentration in the eluent (40-60%, v/v) were investigated using a fractionary factorial design (2(4-1)), having the separation efficiency and purity as target responses. Additional experiments were performed as well, where the temperature and ethanol concentration were studied in a central composite design (2(2)). In this work, the zeolite fixed-bed column was shown to be a good alternative for FOS purification, allowing a FOS purity of 90% and separation efficiency of 6.86 between FOS and glucose, using an eluent at 45°C with 60% ethanol concentration. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Bacteriophage PRD1 batch experiments to study attachment, detachment and inactivation processes

NASA Astrophysics Data System (ADS)

Sadeghi, Gholamreza; Schijven, Jack F.; Behrends, Thilo; Hassanizadeh, S. Majid; van Genuchten, Martinus Th.

2013-09-01

Knowledge of virus removal in subsurface environments is pivotal for assessing the risk of viral contamination of water resources and developing appropriate protection measures. Columns packed with sand are frequently used to quantify attachment, detachment and inactivation rates of viruses. Since column transport experiments are very laborious, a common alternative is to perform batch experiments where usually one or two measurements are done assuming equilibrium is reached. It is also possible to perform kinetic batch experiments. In that case, however, it is necessary to monitor changes in the concentration with time. This means that kinetic batch experiments will be almost as laborious as column experiments. Moreover, attachment and detachment rate coefficients derived from batch experiments may differ from those determined using column experiments. The aim of this study was to determine the utility of kinetic batch experiments and investigate the effects of different designs of the batch experiments on estimated attachment, detachment and inactivation rate coefficients. The experiments involved various combinations of container size, sand-water ratio, and mixing method (i.e., rolling or tumbling by pivoting the tubes around their horizontal or vertical axes, respectively). Batch experiments were conducted with clean quartz sand, water at pH 7 and ionic strength of 20 mM, and using the bacteriophage PRD1 as a model virus. Values of attachment, detachment and inactivation rate coefficients were found by fitting an analytical solution of the kinetic model equations to the data. Attachment rate coefficients were found to be systematically higher under tumbling than under rolling conditions because of better mixing and more efficient contact of phages with the surfaces of the sand grains. In both mixing methods, more sand in the container yielded higher attachment rate coefficients. A linear increase in the detachment rate coefficient was observed with increased solid-water ratio using tumbling method. Given the differences in the attachment rate coefficients, and assuming the same sticking efficiencies since chemical conditions of the batch and column experiments were the same, our results show that collision efficiencies of batch experiments are not the same as those of column experiments. Upscaling of the attachment rate from batch to column experiments hence requires proper understanding of the mixing conditions. Because batch experiments, in which the kinetics are monitored, are as laborious as column experiments, there seems to be no major advantage in performing batch instead of column experiments.

Basic Oxygen Furnace steel slag aggregates for phosphorus treatment. Evaluation of its potential use as a substrate in constructed wetlands.

PubMed

Blanco, Ivan; Molle, Pascal; Sáenz de Miera, Luis E; Ansola, Gemma

2016-02-01

Basic Oxygen Furnace (BOF) steel slag aggregates from NW Spain were tested in batch and column experiments to evaluate its potential use as a substrate in constructed wetlands (CWs). The objectives of this study were to identify the main P removal mechanisms of BOF steel slag and determine its P removal capacity. Also, the results were used to discuss the suitability of this material as a substrate to be used in CWs. Batch experiments with BOF slag aggregates and increasing initial phosphate concentrations showed phosphate removal efficiencies between 84 and 99% and phosphate removal capacities from 0.12 to 8.78 mg P/g slag. A continuous flow column experiment filled with BOF slag aggregates receiving an influent synthetic solution of 15 mg P/L during 213 days showed a removal efficiency greater than 99% and a phosphate removal capacity of 3.1 mg P/g slag. In both experiments the main P removal mechanism was found to be calcium phosphate precipitation which depends on Ca(2+) and OH(-) release from the BOF steel slag after dissolution of Ca(OH)2 in water. P saturation of slag was reached within the upper sections of the column which showed phosphate removal capacities between 1.7 and 2.5 mg P/g slag. Once Ca(OH)2 was completely dissolved in these column sections, removal efficiencies declined gradually from 99% until reaching stable outlet concentrations with P removal efficiencies around 7% which depended on influent Ca(2+) for limited continuous calcium phosphate precipitation. Copyright © 2015 Elsevier Ltd. All rights reserved.

Removal of arsenic from drinking water using rice husk

NASA Astrophysics Data System (ADS)

Asif, Zunaira; Chen, Zhi

2017-06-01

Rice husk adsorption column method has proved to be a promising solution for arsenic (As) removal over the other conventional methods. The present work investigates the potential of raw rice husk as an adsorbent for the removal of arsenic [As(V)] from drinking water. Effects of various operating parameters such as diameter of column, bed height, flow rate, initial arsenic feed concentration and particle size were investigated using continuous fixed bed column to check the removal efficiency of arsenic. This method shows maximum removal of As, i.e., 90.7 % under the following conditions: rice husk amount 42.5 g; 7 mL/min flow rate in 5 cm diameter column at the bed height of 28 cm for 15 ppb inlet feed concentration. Removal efficiency was increased from 83.4 to 90.7 % by reducing the particle size from 1.18 mm to 710 µm for 15 ppb concentration. Langmuir and Freundlich isotherm models were employed to discuss the adsorption behavior. The effect of different operating parameters on the column adsorption was determined using breakthrough curves. In the present study, three kinetic models Adam-Bohart, Thomas and Yoon-Nelson were applied to find out the saturated concentration, fixed bed adsorption capacity and time required for 50 % adsorbate breakthrough, respectively. At the end, solidification was done for disposal of rice husk.

Influence of connection tubing in modern size exclusion chromatography and its impact on the characterization of mAbs.

PubMed

Fekete, Szabolcs; Guillarme, Davy

2018-02-05

The goal of the study was to evaluate the impact of connection tubing in modern size exclusion chromatography (SEC), since it may strongly impact the apparent column efficiency, as the compounds are not retained in SEC. For this purpose, a reference SEC column of 150×4.6mm, 1.8μm was considered, and various proteins were tested as model compounds. Different tube geometries (lengths and internal diameters) and materials (stainless steel and PEEK) were evaluated in a systematic way. Large proteins always showed larger tube dispersion vs. small molecules, especially when the residence time in the tube was long (at low flow rate). This confirms the need to drastically reduce the tube volume (using the shortest and narrowest connector tubing) to attain the full benefits of UHPSEC columns. In addition, PEEK tubing were found to be more appropriate than stainless steel tubing, since adsorption of proteins was less pronounced, and higher plate count can be obtained. Finally, after a careful system optimization, up to 40% increase of apparent column efficiency can be achieved compared to a regular UHPLC system, when using a 150×4.6mm UHPSEC columns packed with sub-3μm particles. Copyright © 2017 Elsevier B.V. All rights reserved.

[Isolation and purification of recombinant soluble and non-fusion angiogenesis inhibitor Kringle 5 using chromatography].

PubMed

Ma, Lina; Wu, Dan; Bian, Liujiao

2012-08-01

The Kringle 5 domain of plasminogen is one of the most potent angiogenesis inhibitors known to date, which can inhibit cell proliferation and migration efficiently. In the study, on the foundation of successful clone and expression of recombinant soluble and non-fusion angiogenesis inhibitor Kringle 5, a two-step chromatographic method, including the use of SP Sepharose Fast Flow cation exchanger and Sephacryl S-100 HR size exclusion chromatography in sequence, was established to separate and purify angiogenesis inhibitor Kringle 5. On the SP Sepharose Fast Flow column, the buffer A consisted of 50.0 mmol/L acetic acid-sodium acetate (pH 5.2), and the buffer B consisted of buffer A with the addition of 0.5 mol/L sodium chloride (pH 5.2); on Sephacryl S-100 HR column, the elution buffer was 5.0 mmol/L phosphate solution (pH 7.0). Through the two-step chromatographic purification process, the purity of the obtained Kringle 5 was more than 98%. In addition, it was found that the obtained Kringle 5 could inhibit the blood vessel growth of chick embryo chorioallantoic membrane effectively. Finally it is concluded that this method can effectively separate active recombinant soluble and non-fusion angiogenesis inhibitor Kringle 5.

Evaluation of alternative landfill cover soils for attenuating hydrogen sulfide from construction and demolition (C&D) debris landfills.

PubMed

Plaza, Cristine; Xu, Qiyong; Townsend, Timothy; Bitton, Gabriel; Booth, Matthew

2007-08-01

Hydrogen sulfide (H(2)S) generated from C&D debris landfills has emerged as a major environmental concern due to odor problems and possible health impacts to landfill employees and surrounding residents. Research was performed to evaluate the performance of various cover materials as control measures for H(2)S emissions from C&D debris landfills. Twelve laboratory-scale simulated landfill columns containing gypsum drywall were operated under anaerobic conditions to promote H(2)S production. Five different cover materials were placed on top of the waste inside duplicate columns: (1) sandy soil, (2) sandy soil amended with lime, (3) clayey soil, (4) fine concrete (particle size less than 2.5 cm), and (5) coarse concrete (particle size greater than 2.5 cm). No cover was placed on two of the columns, which were used as controls. H(2)S concentrations measured from the middle of the waste layer ranged from 50,000 to 150,000 ppm. The different cover materials demonstrated varying H(2)S removal efficiencies. The sandy soil amended with lime and the fine concrete were the most effective for the control of H(2)S emissions. Both materials exhibited reduction efficiencies greater than 99%. The clayey and sandy soils exhibited lower reduction efficiencies, with average removal efficiencies of 65% and 30%, respectively. The coarse concrete was found to be the least efficient material as a result of its large particle size.

Photo-Fenton Degradation of Organic Dyes Based on a Fe₃O₄ Nanospheres/Biomass Composite Loaded Column.

PubMed

Zheng, Kai; Zhang, Jubo; Wang, Yan; Gao, Longxue; Di, Mingyu; Yuan, Fang; Bao, Wenhui; Yang, Tao; Liang, Daxin

2018-06-01

In order to deal with pollution of organic dyes, magnetic Fe3O4 nanospheres (NPs) with an average diameter of 202 ± 0.5 nm were synthesized by a solvothermal method at 200 °C, and they can efficiently degrade organic dyes (methylene blue (MB), rhodamine B (RhB) and xylenol orange (XO)) aqueous solutions (20 mg/L) within 1 min. Based on this Fenton reagent, Fe3O4 NPs/biomass composite degradation column was made using sawdust as substrate, and it can efficiently degrade organic dyes continually. More importantly, the composite can be regenerated just by an ultrasonic treatment, and its degradation performance almost remains the same.

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

PubMed

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.

Development and application of a high-performance liquid chromatography method using monolithic columns for the analysis of ecstasy tablets.

PubMed

Mc Fadden, Kim; Gillespie, John; Carney, Brian; O'Driscoll, Daniel

2006-07-07

A rapid and selective HPLC method using monolithic columns was developed for the separation and quantification of the principal amphetamines in ecstasy tablets. Three monolithic (Chromolith RP18e) columns of different lengths (25, 50 and 100 mm) were assessed. Validation studies including linearity, selectivity, precision, accuracy and limit of detection and quantification were carried out using the Chromolith SpeedROD, RP-18e, 50 mm x 4.6 mm column. Column backpressure and van Deemter plots demonstrated that monolithic columns provide higher efficiency at higher flow rates when compared to particulate columns without the loss of peak resolution. Application of the monolithic column to a large number of ecstasy tablets seized in Ireland ensured its suitability for the routine analysis of ecstasy tablets.

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

PubMed Central

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

2009-01-01

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

Influence of phase type and solute structure on changes in retention with pressure in reversed-phase high performance liquid chromatography.

PubMed

Fallas, Morgane M; Tanaka, Nobuo; Buckenmaier, Stephan M C; McCalley, David V

2013-07-05

The influence of pressure on the retention of several types of solute, including acids, bases and neutrals, was studied by the use of restriction capillaries added to the end of various monomeric and polymeric octadecylsilyl-modified 5μm particle size columns. Although it appeared that certain polymeric columns could give somewhat greater increases in retention with pressure, differences in behaviour between these different C18 columns were rather small. Differences in solute molecular size were most important in determining increases in retention with pressure. However, solute structure such as polarity and planarity were also influential. A prototype C30 column gave interesting selectivity changes between planar and non-planar solutes as a function of pressure. Considerable selectivity differences with pressure were shown when diverse mixtures of solutes were analysed. For the solutes studied, only minor effects of increased pressure on column efficiency and peak shape were noted. Copyright © 2013 Elsevier B.V. All rights reserved.

Computing row and column counts for sparse QR and LU factorization

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

Gilbert, John R.; Li, Xiaoye S.; Ng, Esmond G.

2001-01-01

We present algorithms to determine the number of nonzeros in each row and column of the factors of a sparse matrix, for both the QR factorization and the LU factorization with partial pivoting. The algorithms use only the nonzero structure of the input matrix, and run in time nearly linear in the number of nonzeros in that matrix. They may be used to set up data structures or schedule parallel operations in advance of the numerical factorization. The row and column counts we compute are upper bounds on the actual counts. If the input matrix is strong Hall and theremore » is no coincidental numerical cancellation, the counts are exact for QR factorization and are the tightest bounds possible for LU factorization. These algorithms are based on our earlier work on computing row and column counts for sparse Cholesky factorization, plus an efficient method to compute the column elimination tree of a sparse matrix without explicitly forming the product of the matrix and its transpose.« less

Sonic hedgehog in the notochord is sufficient for patterning of the intervertebral discs

PubMed Central

Choi, Kyung-Suk; Lee, Chanmi; Harfe, Brian D.

2012-01-01

The intervertebral discs, located between adjacent vertebrae, are required for stability of the spine and distributing mechanical load throughout the vertebral column. All cell types located in thes middle regions of the discs, called nuclei pulposi, are derived from the embryonic notochord. Recently, it was shown that the hedgehog signaling pathway plays an essential role during formation of nuclei pulposi. However, during the time that nuclei pulposi are forming, Shh is expressed in both the notochord and the nearby floor plate. To determine the source of SHH protein sufficient for formation of nuclei pulposi we removed Shh from either the floor plate or the notochord using tamoxifen-inducible Cre alleles. Removal of Shh from the floor plate resulted in phenotypically normal intervertebral discs, indicating that Shh expression in this tissue is not required for disc patterning. In addition, embryos that lacked Shh in the floor plate had normal vertebral columns, demonstrating that Shh expression in the notochord is sufficient for pattering the entire vertebral column. Removal of Shh from the notochord resulted in the absence of Shh in the floor plate, loss of intervertebral discs and vertebral structures. These data indicate that Shh expression in the notochord is sufficient for patterning of the intervertebral discs and the vertebral column. PMID:22841806

Sonic hedgehog in the notochord is sufficient for patterning of the intervertebral discs.

PubMed

Choi, Kyung-Suk; Lee, Chanmi; Harfe, Brian D

2012-01-01

The intervertebral discs, located between adjacent vertebrae, are required for stability of the spine and distributing mechanical load throughout the vertebral column. All cell types located in the middle regions of the discs, called nuclei pulposi, are derived from the embryonic notochord. Recently, it was shown that the hedgehog signaling pathway plays an essential role during formation of nuclei pulposi. However, during the time that nuclei pulposi are forming, Shh is expressed in both the notochord and the nearby floor plate. To determine the source of SHH protein sufficient for formation of nuclei pulposi we removed Shh from either the floor plate or the notochord using tamoxifen-inducible Cre alleles. Removal of Shh from the floor plate resulted in phenotypically normal intervertebral discs, indicating that Shh expression in this tissue is not required for disc patterning. In addition, embryos that lacked Shh in the floor plate had normal vertebral columns, demonstrating that Shh expression in the notochord is sufficient for pattering the entire vertebral column. Removal of Shh from the notochord resulted in the absence of Shh in the floor plate, loss of intervertebral discs and vertebral structures. These data indicate that Shh expression in the notochord is sufficient for patterning of the intervertebral discs and the vertebral column. Copyright © 2012 Elsevier Ireland Ltd. All rights reserved.

Enantioselective ultra-high and high performance liquid chromatography: a comparative study of columns based on the Whelk-O1 selector.

PubMed

Kotoni, Dorina; Ciogli, Alessia; D'Acquarica, Ilaria; Kocergin, Jelena; Szczerba, Ted; Ritchie, Harald; Villani, Claudio; Gasparrini, Francesco

2012-12-21

This paper reports on the thermodynamic and kinetic evaluation of a new ultra-high performance liquid chromatography broad-spectrum Pirkle-type chiral stationary phase (CSP) for enantioselective applications (eUHPLC). The well-known Whelk-O1 selector was covalently immobilized onto 1.7-μm high-surface-area, porous spherical silica particles to produce a totally synthetic, covalently bonded CSP that was packed into 150 mm, 100mm, 75 mm and 50mm columns, either 4.6 or 3.0mm ID. A 100 mm × 4.6 mm ID column was fully characterized from a kinetic and thermodynamic point of view, using as reference a conventional HPLC Whelk-O1 column, 250 mm×4.6mm ID, based on 5-μm porous silica particles. On the eUHPLC column, van Deemter plots generated H(min) values of 3.53 μm for 1,3-dinitrobenzene, at an interstitial mobile phase linear velocity (μ(inter)) of 5.07 mm/s, and H(min) of 4.26 and 4.17 μm for the two enantiomers of acenaphthenol, at μ(inter) of 4.85 mm/s and 4.24 mm/s, respectively. Resolution of 21 enantiomeric pairs including alcohols, epoxides, sulfoxides, phosphine oxides, benzodiazepines and 2-aryloxyproprionic esters used as herbicides, were obtained with significant advantages in terms of efficiency and analysis time. Speed gain factors were calculated for the different column geometries (150 mm, 100mm, 75 mm and 50mm, either 4.6 or 3.0mm ID), with respect to the standard HPLC column (250 mm ×4.6 mm ID), and were as high as 13, in the case of the 50-mm-long column, affording sub-minute separations of enantiomers with excellent resolution factors. In particular, trans-stilbene oxide was resolved in only 10s, while a 50 mm×3.0 mm ID column was used as a compromise between reduced mobile phase consumption (less than 1 mL per analysis) and smaller extra-column band-broadening effect. Given the relatively low viscosity in NP mode, and the excellent permeability of these eUHPLC columns, with backpressure values under 600 bar for a wide range of flow rates, the use of standard HPLC hardware is possible. In this case, however, a significant loss in resolution is observed, compared to the UHPLC instrumentation, if no modifications are introduced in the HPLC apparatus to reduce extra-column variance. The excellent efficiency and selectivity, conjugated with the very high-throughput and the ultra-fast analysis time, prove the potentials of the eUHPLC Whelk-O1 columns in the development of enantioselective UHPLC methods. Copyright © 2012 Elsevier B.V. All rights reserved.

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

PubMed

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

2012-07-13

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

Cationized Magnetoferritin Enables Rapid Labeling and Concentration of Gram-Positive and Gram-Negative Bacteria in Magnetic Cell Separation Columns

PubMed Central

Spencer, J.; Schwarzacher, W.

2016-01-01

ABSTRACT In order to identify pathogens rapidly and reliably, bacterial capture and concentration from large sample volumes into smaller ones are often required. Magnetic labeling and capture of bacteria using a magnetic field hold great promise for achieving this goal, but the current protocols have poor capture efficiency. Here, we present a rapid and highly efficient approach to magnetic labeling and capture of both Gram-negative (Escherichia coli) and Gram-positive (Staphylococcus aureus) bacteria using cationized magnetoferritin (cat-MF). Magnetic labeling was achieved within a 1-min incubation period with cat-MF, and 99.97% of the labeled bacteria were immobilized in commercially available magnetic cell separation (MACS) columns. Longer incubation times led to more efficient capture, with S. aureus being immobilized to a greater extent than E. coli. Finally, low numbers of magnetically labeled E. coli bacteria (<100 CFU per ml) were immobilized with 100% efficiency and concentrated 7-fold within 15 min. Therefore, our study provides a novel protocol for rapid and highly efficient magnetic labeling, capture, and concentration of both Gram-positive and Gram-negative bacteria. IMPORTANCE Antimicrobial resistance (AMR) is a significant global challenge. Rapid identification of pathogens will retard the spread of AMR by enabling targeted treatment with suitable agents and by reducing inappropriate antimicrobial use. Rapid detection methods based on microfluidic devices require that bacteria are concentrated from large volumes into much smaller ones. Concentration of bacteria is also important to detect low numbers of pathogens with confidence. Here, we demonstrate that magnetic separation columns capture small amounts of bacteria with 100% efficiency. Rapid magnetization was achieved by exposing bacteria to cationic magnetic nanoparticles, and magnetized bacteria were concentrated 7-fold inside the column. Thus, bacterial capture and concentration were achieved within 15 min. This approach could be extended to encompass the capture and concentration of specific pathogens, for example, by functionalizing magnetic nanoparticles with antibodies or small molecule probes. PMID:27060124

Cationized Magnetoferritin Enables Rapid Labeling and Concentration of Gram-Positive and Gram-Negative Bacteria in Magnetic Cell Separation Columns.

PubMed

Correia Carreira, S; Spencer, J; Schwarzacher, W; Seddon, A M

2016-06-15

In order to identify pathogens rapidly and reliably, bacterial capture and concentration from large sample volumes into smaller ones are often required. Magnetic labeling and capture of bacteria using a magnetic field hold great promise for achieving this goal, but the current protocols have poor capture efficiency. Here, we present a rapid and highly efficient approach to magnetic labeling and capture of both Gram-negative (Escherichia coli) and Gram-positive (Staphylococcus aureus) bacteria using cationized magnetoferritin (cat-MF). Magnetic labeling was achieved within a 1-min incubation period with cat-MF, and 99.97% of the labeled bacteria were immobilized in commercially available magnetic cell separation (MACS) columns. Longer incubation times led to more efficient capture, with S. aureus being immobilized to a greater extent than E. coli Finally, low numbers of magnetically labeled E. coli bacteria (<100 CFU per ml) were immobilized with 100% efficiency and concentrated 7-fold within 15 min. Therefore, our study provides a novel protocol for rapid and highly efficient magnetic labeling, capture, and concentration of both Gram-positive and Gram-negative bacteria. Antimicrobial resistance (AMR) is a significant global challenge. Rapid identification of pathogens will retard the spread of AMR by enabling targeted treatment with suitable agents and by reducing inappropriate antimicrobial use. Rapid detection methods based on microfluidic devices require that bacteria are concentrated from large volumes into much smaller ones. Concentration of bacteria is also important to detect low numbers of pathogens with confidence. Here, we demonstrate that magnetic separation columns capture small amounts of bacteria with 100% efficiency. Rapid magnetization was achieved by exposing bacteria to cationic magnetic nanoparticles, and magnetized bacteria were concentrated 7-fold inside the column. Thus, bacterial capture and concentration were achieved within 15 min. This approach could be extended to encompass the capture and concentration of specific pathogens, for example, by functionalizing magnetic nanoparticles with antibodies or small molecule probes. Copyright © 2016 Correia Carreira et al.

Sugar microanalysis by HPLC with benzoylation: improvement via introduction of a C-8 cartridge and a high efficiency ODS column.

PubMed

Miyagi, Michiko; Yokoyama, Hirokazu; Hibi, Toshifumi

2007-07-01

An HPLC protocol for sugar microanalysis based on the formation of ultraviolet-absorbing benzoyl chloride derivatives was improved. Here, samples were prepared with a C-8 cartridge and analyzed with a high efficiency ODS column, in which porous spherical silica particles 3 microm in diameter were packed. These devices allowed us to simultaneously quantify multiple sugars and sugar alcohols up to 10 ng/ml and to provide satisfactory separations of some sugars, such as fructose and myo-inositol and sorbitol and mannitol. This protocol, which does not require special apparatuses, should become a powerful tool in sugar research.

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

PubMed

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

2013-11-08

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

Production of Truncated Candida antarctica Lipase B Gene Using Automated PCR Gene Assembly Protocol and Expression in Yeast for use in Ethanol and Biodiesel Production.

USDA-ARS?s Scientific Manuscript database

An improved column-based process for production of biodiesel was developed using a column containing a strongly basic anion-exchange resin in sequence with a column containing a resin to which a lipase biocatalyst is bound. Currently most biodiesel is produced by transesterification of triglyceride...

Supercritical fluid chromatography of metoprolol and analogues on aminopropyl and ethylpyridine silica without any additives.

PubMed

Lundgren, Johanna; Salomonsson, John; Gyllenhaal, Olle; Johansson, Erik

2007-06-22

Metoprolol and a number of related amino alcohols and similar analytes have been chromatographed on aminopropyl (APS) and ethylpyridine (EPS) silica columns. The mobile phase was carbon dioxide with methanol as modifier and no amine additive was present. Optimal isocratic conditions for the selectivity were evaluated based on experiments using design of experiments. A central composite circumscribed model for each column was used. Factors were column temperature, back-pressure and % (v/v) of modifier. The responses were retention and selectivity versus metoprolol. The % of modifier mainly controlled the retention on both columns but pressure and temperature could also be important for optimizing the selectivity between the amino alcohols. The compounds could be divided into four and five groups on both columns, with respect to the selectivity. Furthermore, on the aminopropyl silica the analytes were more spread out whereas on the ethylpyridine silica, due to its aromaticity, retention and selectivity were closer. For optimal conditions the column temperature and back-pressure should be high and the modifier concentration low. A comparison of the selectivity using optimized conditions show a few switches of retention order between the two columns. On aminopropyl silica an aldehyde failed to be eluted owing to Schiff-base formation. Peak symmetry and column efficiency were briefly studied for some structurally close analogues. This revealed some activity from the columns that affected analytes that had less protected amino groups, a methyl group instead of isopropyl. The tailing was more marked with the ethylpyridine column even with the more bulky alkyl substituents. Plate number N was a better measure than the asymmetry factor since some analyte peaks broadened without serious deterioration of symmetry compared to homologues.

Monolithic stationary phases with a longitudinal gradient of porosity.

PubMed

Urban, Jiří; Hájek, Tomáš; Svec, Frantisek

2017-04-01

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

Modelling by partial least squares the relationship between the HPLC mobile phases and analytes on phenyl column.

PubMed

Markopoulou, Catherine K; Kouskoura, Maria G; Koundourellis, John E

2011-06-01

Twenty-five descriptors and 61 structurally different analytes have been used on a partial least squares (PLS) to latent structure technique in order to study chromatographically their interaction mechanism on a phenyl column. According to the model, 240 different retention times of the analytes, expressed as Y variable (log k), at different % MeOH mobile-phase concentrations have been correlated with their theoretical most important structural or molecular descriptors. The goodness-of-fit was estimated by the coefficient of multiple determinations r(2) (0.919), and the root mean square error of estimation (RMSEE=0.1283) values with a predictive ability (Q(2)) of 0.901. The model was further validated using cross-validation (CV), validated by 20 response permutations r(2) (0.0, 0.0146), Q(2) (0.0, -0.136) and validated by external prediction. The contribution of certain mechanism interactions between the analytes, the mobile phase and the column, proportional or counterbalancing is also studied. Trying to evaluate the influence on Y of every variable in a PLS model, VIP (variables importance in the projection) plot provides evidence that lipophilicity (expressed as Log D, Log P), polarizability, refractivity and the eluting power of the mobile phase are dominant in the retention mechanism on a phenyl column. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A Versatile, Automatic Chromatographic Column Packing Device

ERIC Educational Resources Information Center

Barry, Eugene F.; And Others

1977-01-01

Describes an inexpensive apparatus for packing liquid and gas chromatographic columns of high efficiency. Consists of stainless steel support struts, an Automat Getriebmotor, and an associated three-pulley system capable of 10, 30, and 300 rpm. (MLH)

Silica particles encapsulated poly(styrene-divinylbenzene) monolithic stationary phases for micro-high performance liquid chromatography.

PubMed

Bakry, R; Stöggl, W M; Hochleitner, E O; Stecher, G; Huck, C W; Bonn, G K

2006-11-03

In the paper we demonstrate a new approach for the preparation and application of continuous silica bed columns that involve encapsulation (entrapment) of functionalized silica microparticles, which can be used as packing material in micro high performance liquid chromatography (micro-HPLC) and capillary electrochromatography (CEC). Like traditional packed columns, these capillaries possess characterized silica particles that offer high phase ratio and narrow pore size distribution leading to high retention and separation efficiency, respectively. More importantly, immobilization of the microparticles stabilizes the separation bed and eliminates the need for retaining frits. The developed capillary columns were fabricated in exactly the same way as a packed capillary column (slurry packing) but with an additional entrapment step. This immobilization of the packed bed was achieved by in situ polymerization of styrene and divinylbenzene in presence of decanol as a porogen and azobisisobutyronitrile as thermal initiator. Silica particles with different particle sizes and pore sizes ranging from 60 to 4000 A were studied. In addition different modified silica was used, including C-18 reversed phase, anion exchange and chiral stationary phases. Efficient separation of polyphenolic compounds, peptides, proteins and even DNA mutation were achieved using the developed technique depending on the properties of the silica particles used (particles pore size). For example, using 3 microm ProntoSIL C-18 particles with 300 A pore size, separation efficiencies in the range of 120,000-200,000 plates/m were obtained for protein separation, in a 6 cm x 200 microm i.d. capillary column. Using encapsulated silica C-18 with 1000 A pore size, separation of DNA homo and hetero duplexes were achieved under denaturing HPLC conditions for mutation detection. In addition, nucleotides were separated using anion exchange material encapsulated with poly(styrene-divinylbenzene) (PS/DVB), which indicated that the chromatographic properties of the silica packing material were still active after polymerization. The prepared capillary columns were found to be stable and could easily be operated continuously up to a pressure of 350 bar without column damage and capillary can be cut to any desired length.

Sol-gel technique for the preparation of beta-cyclodextrin derivative stationary phase in open-tubular capillary electrochromatography.

PubMed

Wang, Y; Zeng, Z; Guan, N; Cheng, J

2001-07-01

A novel open-tubular capillary electrochromatography (OT-CEC) column coated with 2,6-dibutyl-beta-cyclodextrin (DB-beta-CD) was prepared using sol-gel technique. In the sol-gel approach, owing to the three-dimensional network of sol-gel and the strong chemical bond between the stationary phase and the surface of capillary columns, good chromatographic characteristics and unique selectivity in separating isomers were shown. We achieved high efficiencies of 5-14 x 10(4) plates/m for the isomeric nitrophenols using the sol-gel-derived DB-beta-CD columns. The migration time reproducibility of the separation of the isomeric nitrophenols was better than 2.2% over five runs and 4.5% from column to column. These sol-gel-coated DB-beta-CD columns have shown improved separations of isomeric aminophenols, isomeric dihydroxybenzenes and isomeric nitrophenols, in comparison with the sol-gel matrix capillary column. The influences of buffer pH and methanol solvent on separation were investigated. The chiral resolution of enantiomers such as ibuprofen and binaphthol was explored primarily.

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

PubMed

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.

A narrow open tubular column for high efficiency liquid chromatographic separation.

PubMed

Chen, Huang; Yang, Yu; Qiao, Zhenzhen; Xiang, Piliang; Ren, Jiangtao; Meng, Yunzhu; Zhang, Kaiqi; Juan Lu, Joann; Liu, Shaorong

2018-04-30

We report a great feature of open tubular liquid chromatography when it is run using an extremely narrow (e.g., 2 μm inner diameter) open tubular column: more than 10 million plates per meter can be achieved in less than 10 min and under an elution pressure of ca. 20 bar. The column is coated with octadecylsilane and both isocratic and gradient separations are performed. We reveal a focusing effect that may be used to interpret the efficiency enhancement. We also demonstrate the feasibility of using this technique for separating complex peptide samples. This high-resolution and fast separation technique is promising and can lead to a powerful tool for trace sample analysis.

Development of pseudo-linear gradient elution for high-throughput resin selectivity screening in RoboColumn® Format.

PubMed

Kiesewetter, André; Menstell, Peter; Peeck, Lars H; Stein, Andreas

2016-11-01

Rapid development of chromatographic processes relies on effective high-throughput screening (HTS) methods. This article describes the development of pseudo-linear gradient elution for resin selectivity screening using RoboColumns ® . It gives guidelines for the implementation of this HTS method on a Tecan Freedom EVO ® robotic platform, addressing fundamental aspects of scale down and liquid handling. The creation of a flexible script for buffer preparation and column operation plus efficient data processing provided the basis for this work. Based on the concept of discretization, linear gradient elution was transformed into multistep gradients. The impact of column size, flow rate, multistep gradient design, and fractionation scheme on separation efficiency was systematically investigated, using a ternary model protein mixture. We identified key parameters and defined optimal settings for effective column performance. For proof of concept, we examined the selectivity of several cation exchange resins using various buffer conditions. The final protocol enabled a clear differentiation of resin selectivity on miniature chromatography column (MCC) scale. Distinct differences in separation behavior of individual resins and the influence of buffer conditions could be demonstrated. Results obtained with the robotic platform were representative and consistent with data generated on a conventional chromatography system. A study on antibody monomer/high molecular weight separation comparing MCC and lab scale under higher loading conditions provided evidence of the applicability of the miniaturized approach to practically relevant feedstocks with challenging separation tasks as well as of the predictive quality for larger scale. A comparison of varying degrees of robotic method complexity with corresponding effort (analysis time and labware consumption) and output quality highlights tradeoffs to select a method appropriate for a given separation challenge or analytical constraints. © 2016 American Institute of Chemical Engineers Biotechnol. Prog., 32:1503-1519, 2016. © 2016 American Institute of Chemical Engineers.

Revisiting resolution in hydrodynamic countercurrent chromatography: tubing bore effect.

PubMed

Berthod, A; Faure, K

2015-04-17

A major challenge in countercurrent chromatography (CCC), the technique that works with a support-free biphasic liquid system, is to retain the liquid stationary phase inside the CCC column (Sf parameter). Two solutions are commercially available: the hydrostatic CCC columns, also called centrifugal partition chromatographs (CPC), with disks of interconnected channels and rotary seals, and the hydrodynamic CCC columns with bobbins of coiled open tube and no rotary seals. It was demonstrated that the amount of liquid stationary phase retained by a coiled tube was higher with larger bore tubing than with small bore tubes. At constant column volume, small bore tubing will be longer producing more efficiency than larger bore tube that will better retain the liquid stationary phase. Since the resolution equation in CCC is depending on both column efficiency and stationary phase retention ratio, the influence of the tubing bore should be studied. This theoretical work showed that there is an optimum tubing bore size depending on solute partition coefficient and mobile phase flow rate. The interesting result of the theoretical study is that larger tubing bores allow for dramatically reduced experiment durations for all solutes: in reversed phase CCC (polar mobile phase), hydrophobic solutes are usually highly retained. These apolar solutes can be separated by the same coil at high flow rates and reduced Sf with similar retention times as polar solutes separated at smaller flow rates and much higher Sf. Copyright © 2015 Elsevier B.V. All rights reserved.

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

PubMed

Yuan, Ruijuan; Wang, Yan; Ding, Guosheng

2010-01-01

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

Are sub-2 μm particles best for separating small molecules? An alternative.

PubMed

DeStefano, Joseph J; Boyes, Barry E; Schuster, Stephanie A; Miles, William L; Kirkland, Joseph J

2014-11-14

Superficially porous particles (SPP) in the 2.5-2.7 μm range provide almost the same efficiency and resolution of sub-2 μm totally porous particles (TPP), but at one-half to one-third of the operating pressure. The advantage of SPP has led to the introduction of sub-2 μm SPP as a natural extension of this technology. While short columns of both SPP and TPP sub-2 μm particles allow very fast separations, the efficiency advantages of these very small particles often are not realized nor sufficient to overcome some of the practical limitations and disadvantages of such small particles. Advantages and disadvantages of columns packed with sub-2 μm particles are described for comparison with the characteristics of larger particles. The authors conclude that while sub-2 μm particles have utility in research studies, columns of larger particles are often better suited for most applications. A suggested 2.0 μm superficially porous particle diameter retains many of the advantages of sub-2 μm particles, but minimizes some of the disadvantages. The characteristics of these new 2.0 μm SPP are described in studies comparing some present sub-2 μm SPP commercial columns for efficiency, column bed homogeneity and stability. Copyright © 2014 Elsevier B.V. All rights reserved.

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

PubMed

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

2007-07-01

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

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

PubMed

Lin, Shu-Ling; Wang, Chih-Chieh; Fuh, Ming-Ren

2016-10-05

In this study, divinylbenzene (DVB) was used as the cross-linker to prepare alkyl methacrylate (AlMA) monoliths for incorporating π-π interactions between the aromatic analytes and AlMA-DVB monolithic stationary phases in capillary LC analysis. Various AlMA/DVB ratios were investigated to prepare a series of 30% AlMA-DVB monolithic stationary phases in fused-silica capillaries (250-μm i.d.). The physical properties (such as porosity, permeability, and column efficiency) of the synthesized AlMA-DVB monolithic columns were investigated for characterization. Isocratic elution of phenol derivatives was first employed to evaluate the suitability of the prepared AlMA-DVB columns for small molecule separation. The run-to-run (0.16-1.20%, RSD; n = 3) and column-to-column (0.26-2.95%, RSD; n = 3) repeatabilities on retention times were also examined using the selected AlMA-DVB monolithic columns. The π-π interactions between the aromatic ring and the DVB-based stationary phase offered better recognition on polar analytes with aromatic moieties, which resulted in better separation resolution of aromatic analytes on the AlMA-DVB monolithic columns. In order to demonstrate the capability of potential environmental and/or food safety applications, eight phenylurea herbicides with single benzene ring and seven sulfonamide antibiotics with polyaromatic moieties were analyzed using the selected AlMA-DVB monolithic columns. Copyright © 2016. Published by Elsevier B.V.

Maximizing performance in supercritical fluid chromatography using low-density mobile phases.

PubMed

Gritti, Fabrice; Fogwill, Michael; Gilar, Martin; Jarrell, Joseph A

2016-10-14

The performance of a 3.0mm×150mm column packed with 1.8μm fully porous HSS-SB-C 18 particles was investigated in supercritical fluid chromatography (SFC) with low-density, highly expansible carbon dioxide. These conditions are selected for the analysis of semi-volatile compounds. Elevated temperatures (>100°C) were then combined with low column back pressures (<100bar). In this work, the inlet temperature of pure carbon dioxide was set at 107°C, the active back pressure regulator (ABPR) pressure was fixed at 100bar, and the flow rate was set at 2.1mL/min at 12°C (liquefied carbon dioxide) and at an inlet column pressure close to 300bar. Nine n-alkylbenzenes (from benzene to octadecylbenzene) were injected under linear (no sample overload) conditions. The severe steepness of the temperature gradients across the column diameter were predicted from a simplified heat transfer model. Such conditions dramatically lower the column performance by affecting the symmetry of the peak shape. In order to cope with this problem, three different approaches were experimentally tested. They include (1) the decoupling and the proper selection of the inlet eluent temperature with respect to the oven temperature, (2) the partial thermal insulation of the column using polyethylene aerogel, and (3) the application of a high vacuum (10 -5 Torr provided by a turbo-molecular pump) in a housing chamber surrounding the whole column body. The results reveal that (1) the column efficiency can be maximized by properly selecting the difference between the eluent and the oven temperatures, (2) the mere wrapping of the column with an excellent insulating material is insufficient to fully eliminate heat exchanges by conduction and the undesirable radial density gradients across the column i.d., and (3) the complete thermal insulation of the SFC column under high vacuum allows to maximize the column efficiency by maintaining the integrity of the peak shape. Copyright © 2016 Elsevier B.V. All rights reserved.

Two-dimensional preparative liquid chromatography system for preparative separation of minor amount components from complicated natural products.

PubMed

Qiu, Ying-Kun; Chen, Fang-Fang; Zhang, Ling-Ling; Yan, Xia; Chen, Lin; Fang, Mei-Juan; Wu, Zhen

2014-04-11

An on-line comprehensive two-dimensional preparative liquid chromatography system was developed for preparative separation of minor amount components from complicated natural products. Medium-pressure liquid chromatograph (MPLC) was applied as the first dimension and preparative HPLC as the second one, in conjunction with trapping column and makeup pump. The performance of the trapping column was evaluated, in terms of column size, dilution ratio and diameter-height ratio, as well as system pressure from the view of medium pressure liquid chromatograph. Satisfactory trapping efficiency can be achieved using a commercially available 15 mm × 30 mm i.d. ODS pre-column. The instrument operation and the performance of this MPLC×preparative HPLC system were illustrated by gram-scale isolation of crude macro-porous resin enriched water extract of Rheum hotaoense. Automated multi-step preparative separation of 25 compounds, whose structures were identified by MS, (1)H NMR and even by less-sensitive (13)C NMR, could be achieved in a short period of time using this system, exhibiting great advantages in analytical efficiency and sample treatment capacity compared with conventional methods. Copyright © 2014 Elsevier B.V. All rights reserved.

Fabrication and characterization of superporous cellulose bead for high-speed protein chromatography.

PubMed

Wang, Dong-Mei; Hao, Gang; Shi, Qing-Hong; Sun, Yan

2007-03-30

Novel superporous cellulose (SC) matrix has been fabricated by water-in-oil emulsification-thermal regeneration using granules of calcium carbonate as porogenic agents. As a control, microporous cellulose (MC) bead was fabricated in the absence of calcium carbonate. Simultaneously, double cross-linking was applied to enhance the mechanical strength of the particles. The photographs by scanning electron microscopy of the SC bead illustrated that there were more "craters" of several microns scattering on the surface of the beads. It led to a higher water content and effective porosity of the SC medium. The two beads were then modified with diethylaminoethyl (DEAE) group to prepare anion exchangers. The dynamic uptake results of bovine serum albumin (BSA) exhibited that the pore diffusivity of BSA in the DEAE-SC bead was two to three times larger than that in the DEAE-MC bead. In addition, the column packed with the DEAE-SC showed lower backpressure, higher column efficiency and dynamic binding capacity than the column packed with the DEAE-MC at a flow rate range of 150-900cm/h. Moreover, the column efficiency of the DEAE-SC column was independent of flow velocity up to a flow rate of 1200cm/h. All the results exhibited the superior characteristics of the SC bead as a potential medium for high-speed protein chromatography.

Enhanced methodology for porting ion chromatography retention data.

PubMed

Park, Soo Hyun; Shellie, Robert A; Dicinoski, Greg W; Schuster, Georg; Talebi, Mohammad; Haddad, Paul R; Szucs, Roman; Dolan, John W; Pohl, Christopher A

2016-03-04

Porting is a powerful methodology to recalibrate an existing database of ion chromatography (IC) retention times by reflecting the changes of column behavior resulting from either batch-to-batch variability in the production of the column or the manufacture of new versions of a column. This approach has been employed to update extensive databases of retention data of inorganic and organic anions forming part of the "Virtual Column" software marketed by Thermo Fisher Scientific, which is the only available commercial optimization tool for IC separation. The current porting process is accomplished by performing three isocratic separations with two representative analyte ions in order to derive a porting equation which expresses the relationship between old and new data. Although the accuracy of retention prediction is generally enhanced on new columns, errors were observed on some columns. In this work, the porting methodology was modified in order to address this issue, where the porting equation is now derived by using six representative analyte ions (chloride, bromide, iodide, perchlorate, sulfate, and thiosulfate). Additionally, the updated porting methodology has been applied on three Thermo Fisher Scientific columns (AS20, AS19, and AS11HC). The proposed approach showed that the new porting methodology can provide more accurate and robust retention prediction on a wide range of columns, where average errors in retention times for ten test anions under three eluent conditions were less than 1.5%. Moreover, the retention prediction using this new approach provided an acceptable level of accuracy on a used column exhibiting changes in ion-exchange capacity. Crown Copyright © 2016. Published by Elsevier B.V. All rights reserved.

Removal of pharmaceuticals and personal care products during water recycling: microbial community structure and effects of substrate concentration.

PubMed

Onesios-Barry, Kathryn M; Berry, David; Proescher, Jody B; Sivakumar, I K Ashok; Bouwer, Edward J

2014-04-01

Many pharmaceuticals and personal care products (PPCPs) have been shown to be biotransformed in water treatment systems. However, little research exists on the effect of initial PPCP concentration on PPCP biotransformation or on the microbial communities treating impacted water. In this study, biological PPCP removal at various concentrations was assessed using laboratory columns inoculated with wastewater treatment plant effluent. Pyrosequencing was used to examine microbial communities in the columns and in soil from a soil aquifer treatment (SAT; a method of water treatment prior to reuse) site. Laboratory columns were supplied with different concentrations (0.25, 10, 100, or 1,000 μg liter(-1)) of each of 15 PPCPs. Five PPCPs (4-isopropyl-3-methylphenol [biosol], p-chloro-m-xylenol, gemfibrozil, ketoprofen, and phenytoin) were not removed at any tested concentrations. Two PPCPs (naproxen and triclosan) exhibited removals independent of PPCP concentration. PPCP removal efficiencies were dependent on initial concentrations for biphenylol, p-chloro-m-cresol, chlorophene, diclofenac, 5-fluorouracil, ibuprofen, and valproic acid, showing that PPCP concentration can affect biotransformation. Biofilms from sand samples collected from the 0.25- and 10-μg liter(-1) PPCP columns were pyrosequenced along with SAT soil samples collected on three consecutive days of a wetting and drying cycle to enable comparison of these two communities exposed to PPCPs. SAT communities were similar to column communities in taxonomy and phylotype composition, and both were found to contain close relatives of known PPCP degraders. The efficiency of biological removal of PPCPs was found to be dependent on the concentration at which the contamination occurs for some, but not all, PPCPs.

Removal of Pharmaceuticals and Personal Care Products during Water Recycling: Microbial Community Structure and Effects of Substrate Concentration

PubMed Central

Onesios-Barry, Kathryn M.; Berry, David; Proescher, Jody B.; Sivakumar, I. K. Ashok

2014-01-01

Many pharmaceuticals and personal care products (PPCPs) have been shown to be biotransformed in water treatment systems. However, little research exists on the effect of initial PPCP concentration on PPCP biotransformation or on the microbial communities treating impacted water. In this study, biological PPCP removal at various concentrations was assessed using laboratory columns inoculated with wastewater treatment plant effluent. Pyrosequencing was used to examine microbial communities in the columns and in soil from a soil aquifer treatment (SAT; a method of water treatment prior to reuse) site. Laboratory columns were supplied with different concentrations (0.25, 10, 100, or 1,000 μg liter−1) of each of 15 PPCPs. Five PPCPs (4-isopropyl-3-methylphenol [biosol], p-chloro-m-xylenol, gemfibrozil, ketoprofen, and phenytoin) were not removed at any tested concentrations. Two PPCPs (naproxen and triclosan) exhibited removals independent of PPCP concentration. PPCP removal efficiencies were dependent on initial concentrations for biphenylol, p-chloro-m-cresol, chlorophene, diclofenac, 5-fluorouracil, ibuprofen, and valproic acid, showing that PPCP concentration can affect biotransformation. Biofilms from sand samples collected from the 0.25- and 10-μg liter−1 PPCP columns were pyrosequenced along with SAT soil samples collected on three consecutive days of a wetting and drying cycle to enable comparison of these two communities exposed to PPCPs. SAT communities were similar to column communities in taxonomy and phylotype composition, and both were found to contain close relatives of known PPCP degraders. The efficiency of biological removal of PPCPs was found to be dependent on the concentration at which the contamination occurs for some, but not all, PPCPs. PMID:24509919

The Star Schema Benchmark and Augmented Fact Table Indexing

NASA Astrophysics Data System (ADS)

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

We provide a benchmark measuring star schema queries retrieving data from a fact table with Where clause column restrictions on dimension tables. Clustering is crucial to performance with modern disk technology, since retrievals with filter factors down to 0.0005 are now performed most efficiently by sequential table search rather than by indexed access. DB2’s Multi-Dimensional Clustering (MDC) provides methods to "dice" the fact table along a number of orthogonal "dimensions", but only when these dimensions are columns in the fact table. The diced cells cluster fact rows on several of these "dimensions" at once so queries restricting several such columns can access crucially localized data, with much faster query response. Unfortunately, columns of dimension tables of a star schema are not usually represented in the fact table. In this paper, we show a simple way to adjoin physical copies of dimension columns to the fact table, dicing data to effectively cluster query retrieval, and explain how such dicing can be achieved on database products other than DB2. We provide benchmark measurements to show successful use of this methodology on three commercial database products.

Achieving the full performance of highly efficient columns by optimizing conventional benchmark high-performance liquid chromatography instruments.

PubMed

Gritti, Fabrice; Sanchez, Carl A; Farkas, Tivadar; Guiochon, Georges

2010-04-30

A series of experiments and measurements demonstrate the importance of minimizing the extra-column band broadening contribution of the instrument used. The combination of several measures allowed the achievement of the full potential efficiency of three Kinetex-C(18) columns, using a conventional liquid chromatograph. The first measure consists in minimizing the extra-column volume of the instrument, without increasing much its back pressure contribution, by changing the needle seat volume, the inner diameter and length of the capillary connectors, and the volume of the detector cell of a standard instrument (Agilent 1100). The second measure consists in injecting a volume of weak eluent (less than half the elution strength of the mobile phase) right after the sample, before the sample had time to reach the column. Experimental results show that these changes could provide most of the resolution expected from the true column performance. After the changes were made, the resolutions of the 2.1 mm x 50 mm, 4.6 mm x 50 mm, and 4.6 mm x 100 mm Kinetex-C(18) columns for compounds having retention factors close to 1 were increased by about 180, 35, and 30%, respectively. The resolutions obtained are then similar to those measured with advanced instruments like the Agilent 1200, the Agilent 1290 Infinity HPLC, and the Acquity chromatographs. 2010 Elsevier B.V. All rights reserved.

Notochord-dependent expression of MFH1 and PAX1 cooperates to maintain the proliferation of sclerotome cells during the vertebral column development.

PubMed

Furumoto, T A; Miura, N; Akasaka, T; Mizutani-Koseki, Y; Sudo, H; Fukuda, K; Maekawa, M; Yuasa, S; Fu, Y; Moriya, H; Taniguchi, M; Imai, K; Dahl, E; Balling, R; Pavlova, M; Gossler, A; Koseki, H

1999-06-01

During axial skeleton development, the notochord is essential for the induction of the sclerotome and for the subsequent differentiation of cartilage forming the vertebral bodies and intervertebral discs. These functions are mainly mediated by the diffusible signaling molecule Sonic hedgehog. The products of the paired-box-containing Pax1 and the mesenchyme forkhead-1 (Mfh1) genes are expressed in the developing sclerotome and are essential for the normal development of the vertebral column. Here, we demonstrate that Mfh1 like Pax1 expression is dependent on Sonic hedgehog signals from the notochord, and Mfh1 and Pax1 act synergistically to generate the vertebral column. In Mfh1/Pax1 double mutants, dorsomedial structures of the vertebrae are missing, resulting in extreme spina bifida accompanied by subcutaneous myelomeningocoele, and the vertebral bodies and intervertebral discs are missing. The morphological defects in Mfh1/Pax1 double mutants strongly correlate with the reduction of the mitotic rate of sclerotome cells. Thus, both the Mfh1 and the Pax1 gene products cooperate to mediate Sonic hedgehog-dependent proliferation of sclerotome cells. Copyright 1999 Academic Press.

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

PubMed

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.

Bacteriophage PRD1 batch experiments to study attachment, detachment and inactivation processes.

PubMed

Sadeghi, Gholamreza; Schijven, Jack F; Behrends, Thilo; Hassanizadeh, S Majid; van Genuchten, Martinus Th

2013-09-01

Knowledge of virus removal in subsurface environments is pivotal for assessing the risk of viral contamination of water resources and developing appropriate protection measures. Columns packed with sand are frequently used to quantify attachment, detachment and inactivation rates of viruses. Since column transport experiments are very laborious, a common alternative is to perform batch experiments where usually one or two measurements are done assuming equilibrium is reached. It is also possible to perform kinetic batch experiments. In that case, however, it is necessary to monitor changes in the concentration with time. This means that kinetic batch experiments will be almost as laborious as column experiments. Moreover, attachment and detachment rate coefficients derived from batch experiments may differ from those determined using column experiments. The aim of this study was to determine the utility of kinetic batch experiments and investigate the effects of different designs of the batch experiments on estimated attachment, detachment and inactivation rate coefficients. The experiments involved various combinations of container size, sand-water ratio, and mixing method (i.e., rolling or tumbling by pivoting the tubes around their horizontal or vertical axes, respectively). Batch experiments were conducted with clean quartz sand, water at pH 7 and ionic strength of 20 mM, and using the bacteriophage PRD1 as a model virus. Values of attachment, detachment and inactivation rate coefficients were found by fitting an analytical solution of the kinetic model equations to the data. Attachment rate coefficients were found to be systematically higher under tumbling than under rolling conditions because of better mixing and more efficient contact of phages with the surfaces of the sand grains. In both mixing methods, more sand in the container yielded higher attachment rate coefficients. A linear increase in the detachment rate coefficient was observed with increased solid-water ratio using tumbling method. Given the differences in the attachment rate coefficients, and assuming the same sticking efficiencies since chemical conditions of the batch and column experiments were the same, our results show that collision efficiencies of batch experiments are not the same as those of column experiments. Upscaling of the attachment rate from batch to column experiments hence requires proper understanding of the mixing conditions. Because batch experiments, in which the kinetics are monitored, are as laborious as column experiments, there seems to be no major advantage in performing batch instead of column experiments. Copyright © 2013 Elsevier B.V. All rights reserved.

Efficient production of native lunasin with correct N-terminal processing by using the pH-induced self-cleavable Ssp DnaB mini-intein system in Escherichia coli.

PubMed

Setrerrahmane, Sarra; Zhang, Yi; Dai, Guangzhi; Lv, Jing; Tan, Shuhua

2014-09-01

To develop an efficient and cost-effective approach for the production of small preventive peptide lunasin with correct natural N terminus, a synthetic gene was designed by OPTIMIZER & Gene Designer and cloned into pTWIN1 vector at SapI and PstI sites. Thus, lunasin was N-terminally fused to the pH-induced self-cleavable Ssp DnaB mini-intein linked to a chitin binding domain (CBD) with no extra residues. The resultant fusion protein was highly expressed by lactose induction in Escherichia coli BL21 (DE3) in a 7-l bioreactor and bound to a chitin affinity column. After washing the impurities, the Ssp DnaB intein mediated on-column self-cleavage was easily triggered by shifting pH and temperature to allow the native lunasin released. The final purified lunasin yielded up to 75 mg/l medium. Tricine/SDS-PAGE and matrix-assisted laser desorption time-of-flight (MALDI-TOF)/mass spectrometry (MS) verified the structural authenticity of the product, implying the correct cleavage at the junction between Ssp DnaB intein and lunasin. MTT assay confirmed its potent proliferation inhibitory activity to human cancer cells HCT-116 and MDA-MB-231; however, no cytotoxicity to normal human lens epithelial cell SRA01/04 and hepatoma HepG2. Taken together, we provide a novel strategy to produce recombinant native lunasin with correct N-terminal processing by using the pH-induced self-cleavable Ssp DnaB mini-intein.

Analysis and simulation of industrial distillation processes using a graphical system design model

NASA Astrophysics Data System (ADS)

Boca, Maria Loredana; Dobra, Remus; Dragos, Pasculescu; Ahmad, Mohammad Ayaz

2016-12-01

The separation column used for experimentations one model can be configured in two ways: one - two columns of different diameters placed one within the other extension, and second way, one column with set diameter [1], [2]. The column separates the carbon isotopes based on the cryogenic distillation of pure carbon monoxide, which is fed at a constant flow rate as a gas through the feeding system [1],[2]. Based on numerical control systems used in virtual instrumentation was done some simulations of the distillation process in order to obtain of the isotope 13C at high concentrations. The experimental installation for cryogenic separation can be configured from the point of view of the separation column in two ways: Cascade - two columns of different diameters and placed one in the extension of the other column, and second one column with a set diameter. It is proposed that this installation is controlled to achieve data using a data acquisition tool and professional software that will process information from the isotopic column based on a logical dedicated algorithm. Classical isotopic column will be controlled automatically, and information about the main parameters will be monitored and properly display using one program. Take in consideration the very-low operating temperature, an efficient thermal isolation vacuum jacket is necessary. Since the "elementary separation ratio" [2] is very close to unity in order to raise the (13C) isotope concentration up to a desired level, a permanent counter current of the liquid-gaseous phases of the carbon monoxide is created by the main elements of the equipment: the boiler in the bottom-side of the column and the condenser in the top-side.

Fixed bed column study for Cu (II) removal from aqueous solution using water hyacinth (Eichornia crassipes) biomass.

PubMed

Gandhimathi, R; Ramesh, S T; Yadu, Anubhav; Bharathi, K S

2013-07-01

This paper reports the results of the study on the performance of low-cost biosorbent water hyacinth (WH) in removing Cu (II) from aqueous solution. The adsorbent material adopted was found to be an efficient media for the removal of Cu (II) in continuous mode using fixed bed column. The column studies were conducted with 10 mg/L metal solution with a flow rate of 10 mL/min with different bed depths such as 10, 20 and 30 cm. The column design parameters like adsorption rate constant, adsorption capacity and minimum bed depth were calculated. It was found that, the adsorption capacity of copper ions by water hyacinth increased by increasing the bed depth and the contact time.

First Commissioning of a Cryogenic Distillation Column for Low Radioactivity Underground Argon

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

Back, H. O.; Alexander, T.; Alton, A.

2012-04-01

We report on the performance and commissioning of a cryogenic distillation column for low radioactivity underground argon at Fermi National Accelerator Laboratory. The distillation column is designed to accept a mixture of argon, helium, and nitrogen and return pure argon with a nitrogen contamination less than 10 ppm. In the first commissioning, we were able to run the distillation column in a continuous mode and produce argon that is 99.9% pure. After running in a batch mode, the argon purity was increased to 99.95%, with 500 ppm of nitrogen remaining. The efficiency of collecting the argon from the gas mixturemore » was between 70% and 81%, at an argon production rate of 0.84-0.98 kg/day.« less

Core-Shell Columns in High-Performance Liquid Chromatography: Food Analysis Applications

PubMed Central

Preti, Raffaella

2016-01-01

The increased separation efficiency provided by the new technology of column packed with core-shell particles in high-performance liquid chromatography (HPLC) has resulted in their widespread diffusion in several analytical fields: from pharmaceutical, biological, environmental, and toxicological. The present paper presents their most recent applications in food analysis. Their use has proved to be particularly advantageous for the determination of compounds at trace levels or when a large amount of samples must be analyzed fast using reliable and solvent-saving apparatus. The literature hereby described shows how the outstanding performances provided by core-shell particles column on a traditional HPLC instruments are comparable to those obtained with a costly UHPLC instrumentation, making this novel column a promising key tool in food analysis. PMID:27143972

Catenin-dependent cadherin function drives divisional segregation of spinal motor neurons.

PubMed

Bello, Sanusi M; Millo, Hadas; Rajebhosale, Manisha; Price, Stephen R

2012-01-11

Motor neurons that control limb movements are organized as a neuronal nucleus in the developing ventral horn of the spinal cord called the lateral motor column. Neuronal migration segregates motor neurons into distinct lateral and medial divisions within the lateral motor column that project axons to dorsal or ventral limb targets, respectively. This migratory phase is followed by an aggregation phase whereby motor neurons within a division that project to the same muscle cluster together. These later phases of motor neuron organization depend on limb-regulated differential cadherin expression within motor neurons. Initially, all motor neurons display the same cadherin expression profile, which coincides with the migratory phase of motor neuron segregation. Here, we show that this early, pan-motor neuron cadherin function drives the divisional segregation of spinal motor neurons in the chicken embryo by controlling motor neuron migration. We manipulated pan-motor neuron cadherin function through dissociation of cadherin binding to their intracellular partners. We found that of the major intracellular transducers of cadherin signaling, γ-catenin and α-catenin predominate in the lateral motor column. In vivo manipulations that uncouple cadherin-catenin binding disrupt divisional segregation via deficits in motor neuron migration. Additionally, reduction of the expression of cadherin-7, a cadherin predominantly expressed in motor neurons only during their migration, also perturbs divisional segregation. Our results show that γ-catenin-dependent cadherin function is required for spinal motor neuron migration and divisional segregation and suggest a prolonged role for cadherin expression in all phases of motor neuron organization.

A spin column-free approach to sodium hydroxide-based glycan permethylation.

PubMed

Hu, Yueming; Borges, Chad R

2017-07-24

Glycan permethylation was introduced as a tool to facilitate the study of glycans in 1903. Since that time, permethylation procedures have been continually modified to improve permethylation efficiency and qualitative applicability. Typically, however, either laborious preparation steps or cumbersome and uneconomical spin columns have been needed to obtain decent permethylation yields on small glycan samples. Here we describe a spin column-free (SCF) glycan permethylation procedure that is applicable to both O- and N-linked glycans and can be employed upstream to intact glycan analysis by MALDI-MS, ESI-MS, or glycan linkage analysis by GC-MS. The SCF procedure involves neutralization of NaOH beads by acidified phosphate buffer, which eliminates the risk of glycan oxidative degradation and avoids the use of spin columns. Optimization of the new permethylation procedure provided high permethylation efficiency for both hexose (>98%) and HexNAc (>99%) residues-yields which were comparable to (or better than) those of some widely-used spin column-based procedures. A light vs. heavy labelling approach was employed to compare intact glycan yields from a popular spin-column based approach to the SCF approach. Recovery of intact N-glycans was significantly better with the SCF procedure (p < 0.05), but overall yield of O-glycans was similar or slightly diminished (p < 0.05 for tetrasaccharides or smaller). When the SCF procedure was employed upstream to hydrolysis, reduction and acetylation for glycan linkage analysis of pooled glycans from unfractionated blood plasma, analytical reproducibility was on par with that from previous spin column-based "glycan node" analysis results. When applied to blood plasma samples from stage III-IV breast cancer patients (n = 20) and age-matched controls (n = 20), the SCF procedure facilitated identification of three glycan nodes with significantly different distributions between the cases and controls (ROC c-statistics > 0.75; p < 0.01). In summary, the SCF permethylation procedure expedites and economizes both intact glycan analysis and linkage analysis of glycans from whole biospecimens.

A spin column-free approach to sodium hydroxide-based glycan permethylation†

PubMed Central

Hu, Yueming; Borges, Chad R.

2018-01-01

Glycan permethylation was introduced as a tool to facilitate the study of glycans in 1903. Since that time, permethylation procedures have been continually modified to improve permethylation efficiency and qualitative applicability. Typically, however, either laborious preparation steps or cumbersome and uneconomical spin columns have been needed to obtain decent permethylation yields on small glycan samples. Here we describe a spin column-free (SCF) glycan permethylation procedure that is applicable to both O- and N-linked glycans and can be employed upstream to intact glycan analysis by MALDI-MS, ESI-MS, or glycan linkage analysis by GC-MS. The SCF procedure involves neutralization of NaOH beads by acidified phosphate buffer, which eliminates the risk of glycan oxidative degradation and avoids the use of spin columns. Optimization of the new permethylation procedure provided high permethylation efficiency for both hexose (>98%) and HexNAc (>99%) residues—yields which were comparable to (or better than) those of some widely-used spin column-based procedures. A light vs. heavy labelling approach was employed to compare intact glycan yields from a popular spin-column based approach to the SCF approach. Recovery of intact N-glycans was significantly better with the SCF procedure (p < 0.05), but overall yield of O-glycans was similar or slightly diminished (p < 0.05 for tetrasaccharides or smaller). When the SCF procedure was employed upstream to hydrolysis, reduction and acetylation for glycan linkage analysis of pooled glycans from unfractionated blood plasma, analytical reproducibility was on par with that from previous spin column-based “glycan node” analysis results. When applied to blood plasma samples from stage III–IV breast cancer patients (n = 20) and age-matched controls (n = 20), the SCF procedure facilitated identification of three glycan nodes with significantly different distributions between the cases and controls (ROC c-statistics > 0.75; p < 0.01). In summary, the SCF permethylation procedure expedites and economizes both intact glycan analysis and linkage analysis of glycans from whole biospecimens. PMID:28635997

A fine coal circuitry study using column flotation and gravity separation. Quarterly report, 1 March 1995--31 May 1995

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

Honaker, R.Q.; Reed, S.

1995-12-31

Column flotation provides excellent recovery of ultrafine coal while producing low ash content concentrates. However, column flotation is not efficient for treating fine coal containing significant amounts of mixed-phase particles. Fortunately, enhanced gravity separation has proved to have the ability to treat the mixed-phased particles more effectively. A disadvantage of gravity separation is that ultrafine clay particles are not easily rejected. Thus, a combination of these two technologies may provide a circuit that maximizes both the ash and sulfur rejection that can be achieved by physical coal cleaning while maintaining a high energy recovery. This project is studying the potentialmore » of using different combinations of gravity separators, i.e., a Floatex hydrosizer and a Falcon Concentrator, and a proven flotation column, which will be selected based on previous studies by the principle investigator. During this reporting period, an extensive separation performance comparison between a pilot-scale Floatex Density Separator (18{times}18-inch) and an existing spiral circuit has been conducted at Kerf-McGee Coal Preparation plan for the treatment of nominally {minus}16 mesh coal. The results indicate that the Floatex is a more efficient separation device (E{sub p}=0.12) than a conventional coal spiral (E{sub p}=0.18) for Illinois seam coals. In addition, the treatment of {minus}100 mesh Illinois No. 5 fine coal from the same plant using Falcon concentrator, column flotation (Packed-Column) and their different combinations was also evaluated. For a single operation, both Falcon concentrator and column flotation can produce a clean coal product with 90% combustible recovery and 5% ash content. In the case of the combined circuit, column flotation followed by the Falcon achieved a higher combustible recovery value (about 75%) than that obtained by the individual units while maintaining an ash content less than 3%.« less

Preparation and evaluation of molecularly imprinted polymers based on 9-ethyladenine for the recognition of nucleotide bases in capillary electrochromatography.

PubMed

Huang, Yi-Chen; Lin, Chun-Chi; Liu, Chuen-Ying

2004-02-01

A molecularly imprinted polymer (MIP) comprising 9-ethyladenine was polymerized in situ inside the capillary for the electrochromatographic separation of nucleotide bases. The capillary wall was first functionalized with 3-trimethoxysilylpropyl methacrylate (10% v/v) and 1,1-diphenyl-2-picrylhydrazyl (0.01% w/v) in toluene. Following this treatment, the capillary was filled with acetonitrile containing 9-ethyladenine, methacrylic acid, ethylene glycol dimethacrylate, and initiator. After polymerization, the MIP was shrunk into a film against the inner wall of the capillary with the syringe pump. The template was then removed with methanol under nitrogen flow. For evaluation the feasibility of the MIP column for the separation of nucleotide bases, some parameters including the pH, concentration of the background electrolyte, the applied voltage as well as the effect of organic modifier were studied. The migration behavior of nucleotide bases on the MIP column was also compared with that on the bare fused-silica column. The results indicated that the MIP columns demonstrated better recognition properties at a pH range of 6-8. The efficiency (plates/m) at pH 8 for the nonimprinted analyte was 75,300 for cytosine, 50,200 for thymine, and 14,800 for guanine. However, the efficiency for the imprinted analyte, adenine, was quite low. This was evidenced by the broad peak, yielding only 2600 plates/m.

Experimental feasibility of the airborne measurement of absolute oil fluorescence spectral conversion efficiency

NASA Technical Reports Server (NTRS)

Hoge, F. E.; Swift, R. N.

1983-01-01

Airborne lidar oil spill experiments carried out to determine the practicability of the AOFSCE (absolute oil fluorescence spectral conversion efficiency) computational model are described. The results reveal that the model is suitable over a considerable range of oil film thicknesses provided the fluorescence efficiency of the oil does not approach the minimum detection sensitivity limitations of the lidar system. Separate airborne lidar experiments to demonstrate measurement of the water column Raman conversion efficiency are also conducted to ascertain the ultimate feasibility of converting such relative oil fluorescence to absolute values. Whereas the AOFSCE model is seen as highly promising, further airborne water column Raman conversion efficiency experiments with improved temporal or depth-resolved waveform calibration and software deconvolution techniques are thought necessary for a final determination of suitability.

Role of notochord cells and sclerotome-derived cells in vertebral column development in fugu, Takifugu rubripes: histological and gene expression analyses.

PubMed

Kaneko, Takamasa; Freeha, Khalid; Wu, Xiaoming; Mogi, Makoto; Uji, Susumu; Yokoi, Hayato; Suzuki, Tohru

2016-10-01

Despite the common structure of vertebrates, the development of the vertebral column differs widely between teleosts and tetrapods in several respects, including the ossification of the centrum and the function of the notochord. In contrast to tetrapods, vertebral development in teleosts is not fully understood, particularly for large fish with highly ossified bones. We therefore examined the histology and gene expression profile of vertebral development in fugu, Takifugu rubripes, a model organism for genomic research. Ossification of the fugu centrum is carried out by outer osteoblasts expressing col1a1, col2a1, and sparc, and the growing centra completely divide the notochord into double cone-shaped segments that function as intercentral joints. In this process, the notochord basal cells produce a thick notochord sheath exhibiting Alcian-blue-reactive cartilaginous properties and composing the intercentral ligament in cooperation with the external ligament connective tissue. Synthesis of the matrix by the basal cells was ascertained by an in vitro test. Expression of twist2 indicates that this connective tissue is descended from the embryonic sclerotome. Notochord basal cells express sox9, ihhb, shh, and col2a1a, suggesting that the signaling system involved in chondrocyte proliferation and matrix production also functions in notochord cells for notochord sheath formation. We further found that the notochord expression of both ntla and shh is maintained in the fugu vertebral column, whereas it is turned off after embryogenesis in zebrafish. Thus, our results demonstrate that, in contrast to zebrafish, a dynamic morphogenesis and molecular network continues to function in fugu until the establishment of the adult vertebral column.

Impact of substrates acclimation strategy on simultaneous biodegradation of hydrogen sulfide and ammonia.

PubMed

Jiang, Xia; Luo, Yiqun; Yan, Rong; Tay, Joo Hwa

2009-12-01

Three columns were differentiated with feeding mixture of H(2)S and NH(3) (MFC), feeding NH(3) followed by H(2)S (NFC), and feeding H(2)S followed by NH(3) (SFC). Removal performance, biodegradation capacity and microbial community structures in the three columns were compared. The results show that NFC has a shorter acclimation period for the removal of NH(3) gas and nitrification than MFC. Under the high loading of H(2)S and NH(3) at 164 and 82 gm(-3) h(-1), respectively, NFC exhibited high removal efficiency of NH(3) (>95%) while the removal efficiencies were obtained at 63 and 75% in MFC and SFC, respectively. The removal of NH(3) gas in NFC was significantly attributed to nitrification (over 50%), while adsorption and chemical reaction contributed to the removal of NH(3) in MFC and SFC. The different biodegradation capacities of NH(3) could be due to the dissimilarity in the microbial population presented in each column.

Production of Wnt4b by floor plate cells is essential for the segmental patterning of the vertebral column in medaka.

PubMed

Inohaya, Keiji; Takano, Yoshiro; Kudo, Akira

2010-06-01

The floor plate is a key organizer that controls the specification of neurons in the central nervous system. Here, we show a new role of the floor plate: segmental pattern formation of the vertebral column. Analysis of a spontaneous medaka mutant, fused centrum (fsc), which exhibits fused centra and the absence of the intervertebral ligaments, revealed that fsc encodes wnt4b, which was expressed exclusively in the floor plate. In fsc mutants, we found that wnt4b expression was completely lost in the floor plate and that abnormal conversion of the intervertebral ligament cells into osteoblasts appeared to cause a defect of the intervertebral ligaments. The establishment of the transgenic rescue lines and mosaic analyses allowed the conclusion to be drawn that production of wnt4b by floor plate cells is essential for the segmental patterning of the vertebral column. Our findings provide a novel perspective on the mechanism of vertebrate development.

On-line sample cleanup and enrichment chromatographic technique for the determination of ambroxol in human serum.

PubMed

Emara, Samy; Kamal, Maha; Abdel Kawi, Mohamed

2012-02-01

A sensitive and efficient on-line clean up and pre-concentration method has been developed using column-switching technique and protein-coated µ-Bondapak CN silica pre-column for quantification of ambroxol (AM) in human serum. The method is performed by direct injection of serum sample onto a protein-coated µ-Bondapak CN silica pre-column, where AM is pre-concentrated and retained, while proteins and very polar constituents are washed to waste using a phosphate buffer saline (pH 7.4). The retained analyte on the pre-column is directed onto a C(18) analytical column for separation, with a mobile phase consisting of a mixture of methanol and distilled deionized water (containing 1% triethylamine adjusted to pH 3.5 with ortho-phosphoric acid) in the ratio of 50:50 (v/v). Detection is performed at 254 nm. The calibration curve is linear over the concentration range of 12-120 ng/mL (r(2) = 0.9995). The recovery, selectivity, linearity, precision, and accuracy of the method are convenient for pharmacokinetic studies or routine assays.

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

PubMed

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

2015-01-02

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

Quantifying the condition of eruption column collapse during explosive volcanic eruptions

NASA Astrophysics Data System (ADS)

Koyaguchi, Takehiro; Suzuki, Yujiro

2016-04-01

During an explosive eruption, a mixture of pyroclasts and volcanic gas forms a buoyant eruption column or a pyroclastic flow. Generation of a pyroclastic flow caused by eruption column collapse is one of the most hazardous phenomena during explosive volcanic eruptions. The quantification of column collapse condition (CCC) is, therefore, highly desired for volcanic hazard assessment. Previously the CCC was roughly predicted by a simple relationship between magma discharge rate and water content (e.g., Carazzo et al., 2008). When a crater is present above the conduit, because of decompression/compression process inside/above the crater, the CCC based on this relationship can be strongly modified (Woods and Bower, 1995; Koyaguchi et al., 2010); however, the effects of the crater on CCC has not been fully understood in a quantitative fashion. Here, we have derived a semi-analytical expression of CCC, in which the effects of the crater is taken into account. The CCC depends on magma properties, crater shape (radius, depth and opening angle) as well as the flow rate at the base of crater. Our semi-analytical CCC expresses all these dependencies by a single surface in a parameter space of the dimensionless magma discharge rate, the dimensionless magma flow rate (per unit area) and the ratio of the cross-sectional areas at the top and the base of crater. We have performed a systematic parameter study of three-dimensional (3D) numerical simulations of eruption column dynamics to confirm the semi-analytical CCC. The results of the 3D simulations are consistent with the semi-analytical CCC, while they show some additional fluid dynamical features in the transitional state (e.g., partial column collapse). Because the CCC depends on such many parameters, the scenario towards the generation of pyroclastic flow during explosive eruptions is considered to be diverse. Nevertheless, our semi-analytical CCC together with the existing semi-analytical solution for the 1D conduit flow model (Koyaguchi, 2005) allows us to intuitively and quantitatively understand how the eruption column dynamics approaches to the CCC as the crater radius increases during the waxing stage of an eruption, or as the magma chamber pressure decreases during the waning stage.

Influence of cross-sectional ratio of down comer to riser on the efficiency of liquid circulation in loop air lift bubble column

NASA Astrophysics Data System (ADS)

Yamamoto, Tatsumi; Kawasaki, Hiroyuki; Mori, Hidetoshi

2017-11-01

Loop type bubble columns have good performance of liquid circulation and mass transfer by airlift effect, where the liquid circulation time is an important measurable characteristic parameter. This parameter is affected by the column construction, the aspect ratio of the column, the cross-sectional area ratio of down comer to riser (R), and the superficial gas velocity in the riser (UGR). In this work, the mean gas holdup and the liquid circulation time (TC) have been measured in four types of loop airlift type bubble column: concentric tube internal loop airlift type, rectangular internal loop airlift type, external loop airlift type, external loop airlift with separator. Air and tap water were used as gas and liquid phase, respectively. The results have demonstrated that the mean gas holdup in riser increases in proportion to UGR, and that it in downcomer changes according to the geometric parameters of each bubble column. TC has been found to conform to an empirical equation which depends on UGR and the length of draft tube or division plate in the region of 0.33 < R < 1.

Tlx-1 and Tlx-3 homeobox gene expression in cranial sensory ganglia and hindbrain of the chick embryo: markers of patterned connectivity.

PubMed

Logan, C; Wingate, R J; McKay, I J; Lumsden, A

1998-07-15

Recent evidence suggests that in vertebrates the formation of distinct neuronal cell types is controlled by specific families of homeodomain transcription factors. Furthermore, the expression domains of a number of these genes correlates with functionally integrated neuronal populations. We have isolated two members of the divergent T-cell leukemia translocation (HOX11/Tlx) homeobox gene family from chick, Tlx-1 and Tlx-3, and show that they are expressed in differentiating neurons of both the peripheral and central nervous systems. In the peripheral nervous system, Tlx-1 and Tlx-3 are expressed in overlapping domains within the placodally derived components of a number of cranial sensory ganglia. Tlx-3, unlike Tlx-1, is also expressed in neural crest-derived dorsal root and sympathetic ganglia. In the CNS, both genes are expressed in longitudinal columns of neurons at specific dorsoventral levels of the hindbrain. Each column has distinct anterior and/or posterior limits that respect inter-rhombomeric boundaries. Tlx-3 is also expressed in D2 and D3 neurons of the spinal cord. Tlx-1 and Tlx-3 expression patterns within the peripheral and central nervous systems suggest that Tlx proteins may be involved not only in the differentiation and/or survival of specific neuronal populations but also in the establishment of neuronal circuitry. Furthermore, by analogy with the LIM genes, Tlx family members potentially define sensory columns early within the developing hindbrain in a combinatorial manner.

Selectivity of hexaphenylbenzene-based hydrocarbon stationary phase with propeller-like conformation for aromatic and aliphatic isomers.

PubMed

Yang, Yinhui; Chang, Zhengfeng; Yang, Xiaohong; Qi, Meiling; Wang, Jinliang

2018-08-03

Herein we report a propeller-like hexaphenylbenzene-based hydrocarbon material (denoted as BT) as the stationary phase for capillary gas chromatography (GC). The statically-coated BT capillary column showed a high column efficiency of 4340 plates m -1 and weak polarity. Owing to its unique conformation, π-electron toroidal delocalization and intrinsic microporosity, the BT stationary phase exhibited interesting selectivity for aromatic compounds over alkanes. Compared with the graphene (G) column, the BT column showed much prolonged retention and high selectivity for aromatic isomers, especially methylnaphthalenes, dimethylnaphthalenes and phenanthrene/anthracene, mainly because of its propeller-like conformation with rich intercalation effects. Moreover, it exhibited good column repeatability (intra-day, inter-day) and reproducibility (between-column) with RSD values on the retention times less than 0.08% for intra-day, 0.32% for inter-day and 3.8% for between-column, respectively. Also, it showed good potential for determination of minor isomer impurities in real samples. To the best of our knowledge, this work presents the first example of employing an neat aromatic hydrocarbon material as the GC stationary phase with high selectivity for analytes of a wide ranging polarity. Copyright © 2018 Elsevier B.V. All rights reserved.

Separation analysis of macrolide antibiotics with good performance on a positively charged C18HCE column.

PubMed

Wei, Jie; Shen, Aijin; Yan, Jingyu; Jin, Gaowa; Yang, Bingcheng; Guo, Zhimou; Zhang, Feifang; Liang, Xinmiao

2016-03-01

The separation of basic macrolide antibiotics suffers from peak tailing and poor efficiency on traditional silica-based reversed-phase liquid chromatography columns. In this work, a C18HCE column with positively charged surface was applied to the separation of macrolides. Compared with an Acquity BEH C18 column, the C18HCE column exhibited superior performance in the aspect of peak shape and separation efficiency. The screening of mobile phase additives including formic acid, acetic acid and ammonium formate indicated that formic acid was preferable for providing symmetrical peak shapes. Moreover, the influence of formic acid content was investigated. Analysis speed and mass spectrometry compatibility were also taken into account when optimizing the separation conditions for liquid chromatography coupled with tandem mass spectrometry. The developed method was successfully utilized for the determination of macrolide residues in a honey sample. Azithromycin was chosen as the internal standard for the quantitation of spiramycin and tilmicosin, while roxithromycin was used for erythromycin, tylosin, clarithromycin, josamycin and acetylisovaleryltylosin. Good correlation coefficients (r(2) > 0.9938) for all macrolides were obtained. The intra-day and inter-day recoveries were 73.7-134.7% and 80.7-119.7% with relative standard deviations of 2.5-8.0% and 3.9-16.1%, respectively. Outstanding sensitivity with limits of quantitation (S/N ≥ 10) of 0.02-1 μg/kg and limits of detection (S/N ≥ 3) of 0.01-0.5 μg/kg were achieved. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Using Extreme Tropical Precipitation Statistics to Constrain Future Climate States

NASA Astrophysics Data System (ADS)

Igel, M.; Biello, J. A.

2017-12-01

Tropical precipitation is characterized by a rapid growth in mean intensity as the column humidity increases. This behavior is examined in both a cloud resolving model and with high-resolution observations of precipitation and column humidity from CloudSat and AIRS, respectively. The model and the observations exhibit remarkable consistency and suggest a new paradigm for extreme precipitation. We show that the total precipitation can be decomposed into a product of contributions from a mean intensity, a probability of precipitation, and a global PDF of column humidity values. We use the modeling and observational results to suggest simple, analytic forms for each of these functions. The analytic representations are then used to construct a simple expression for the global accumulated precipitation as a function of the parameters of each of the component functions. As the climate warms, extreme precipitation intensity and global precipitation are expected to increase, though at different rates. When these predictions are incorporated into the new analytic expression for total precipitation, predictions for changes due to global warming to the probability of precipitation and the PDF of column humidity can be made. We show that strong constraints can be imposed on the future shape of the PDF of column humidity but that only weak constraints can be set on the probability of precipitation. These are largely imposed by the intensification of extreme precipitation. This result suggests that understanding precisely how extreme precipitation responds to climate warming is critical to predicting other impactful properties of global hydrology. The new framework can also be used to confirm and discount existing theories for shifting precipitation.

Enhancing Bioremediation of Oil-contaminated Soils by Controlling Nutrient Transport using Dual Characteristics of Soil Pore Structure

NASA Astrophysics Data System (ADS)

Mori, Y.; Suetsugu, A.; Matsumoto, Y.; Fujihara, A.; Suyama, K.; Miyamoto, T.

2012-12-01

Soil structure is heterogeneous with cracks or macropores allowing bypass flow, which may lead to applied chemicals avoiding interaction with soil particles or the contaminated area. We investigated the bioremediation efficiency of oil-contaminated soils by applying suction at the bottom of soil columns during bioremediation. Unsaturated flow conditions were investigated so as to avoid bypass flow and achieve sufficient dispersion of chemicals in the soil column. The boundary conditions at the bottom of the soil columns were 0 kPa and -3 kPa, and were applied to a volcanic ash soil with and without macropores. Unsaturated flow was achieved with -3 kPa and an injection rate of 1/10 of the saturated hydraulic conductivity. The resultant biological activities of the effluent increased dramatically in the unsaturated flow with macropores condition. Unsaturated conditions prevented bypass flow and allowed dispersion of the injected nutrients. Unsaturated flow achieved 60-80% of saturation, which enhanced biological activity in the soil column. Remediation results were better for unsaturated conditions because of higher biological activity. Moreover, unsaturated flow with macropores achieved uniform remediation efficiency from upper through lower positions in the column. Finally, taking the applied solution volume into consideration, unsaturated flow with -3 kPa achieved 10 times higher efficiency when compared with conventional saturated flow application. These results suggest that effective use of nutrients or remediation chemicals is possible by avoiding bypass flow and enhancing biological activity using relatively simple and inexpensive techniques.

Analysis of essential oils and fragrances with a new generation of highly inert gas chromatographic columns coated with ionic liquids.

PubMed

Cagliero, Cecilia; Bicchi, Carlo; Cordero, Chiara; Liberto, Erica; Rubiolo, Patrizia; Sgorbini, Barbara

2017-04-28

In the fields of essential oils and fragrances, samples often consist of mixtures of compounds with similar structural and physical characteristics (e.g. mono- and sesquiterpenoids), whose correct identification closely depends on the synergic combination of chromatographic and mass spectral data. This sample complexity means that new GC stationary phases with different selectivities are continually being investigated. Ionic liquids (ILs) are of great interest as GC stationary phases in this field because of their selectivity (significantly different than that of currently phases) and their high temperature stability. A first generation of IL GC columns was found to be competitive when applied to these field, in terms of selectivity and efficiency, compared to conventional columns (polydimethylsiloxane, (e.g. OV-1), methyl-polysiloxane 5%-phenyl (e.g. SE-52), 7%-cyanopropyl, 7%-phenyl polysiloxane (e.g. OV-1701), and polyethylen glycol (e.g. PEG-20M). However, these columns showed significant activity towards polar or active analytes, which primarily affected their quantitative performance. A new generation of highly-inactive columns coated with three of the most widely-used ionic liquid GC stationary phases has recently been introduced; these phases are SLB-IL60i (1,12-di(tripropylphosphonium) dodecane bis(trifluoromethylsulfonyl) imide [NTf 2 ], SLB-IL76i (tri-(tripropylphosphonium-hexanamido)-triethylamine [NTf 2 ]), and SLB-IL111i (1,5-di (2,3-dimethyllimidazolium) pentane [NTf 2 ]). This study carefully tested the new inert IL columns, in view of their routine application in the fragrance and essential oil fields. They were found to have unusually high selectivity, comparable to that of first-generation IL columns, while their inertness and efficiency were competitive with those of currently-used conventional columns. The IL column performance of first and second generations was compared, through the quali-quantitative analysis of components in a group of different complexity samples; these included the Grob test, a standard mixture of "suspected" skin allergens, and the essential oils of chamomile and sandalwood. Copyright © 2017 Elsevier B.V. All rights reserved.

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

PubMed

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

2016-05-15

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

Vertically stabilized elongated cross-section tokamak

DOEpatents

Sheffield, George V.

1977-01-01

This invention provides a vertically stabilized, non-circular (minor) cross-section, toroidal plasma column characterized by an external separatrix. To this end, a specific poloidal coil means is added outside a toroidal plasma column containing an endless plasma current in a tokamak to produce a rectangular cross-section plasma column along the equilibrium axis of the plasma column. By elongating the spacing between the poloidal coil means the plasma cross-section is vertically elongated, while maintaining vertical stability, efficiently to increase the poloidal flux in linear proportion to the plasma cross-section height to achieve a much greater plasma volume than could be achieved with the heretofore known round cross-section plasma columns. Also, vertical stability is enhanced over an elliptical cross-section plasma column, and poloidal magnetic divertors are achieved.

Recent advances in capillary ultrahigh pressure liquid chromatography.

PubMed

Blue, Laura E; Franklin, Edward G; Godinho, Justin M; Grinias, James P; Grinias, Kaitlin M; Lunn, Daniel B; Moore, Stephanie M

2017-11-10

In the twenty years since its initial demonstration, capillary ultrahigh pressure liquid chromatography (UHPLC) has proven to be one of most powerful separation techniques for the analysis of complex mixtures. This review focuses on the most recent advances made since 2010 towards increasing the performance of such separations. Improvements in capillary column preparation techniques that have led to columns with unprecedented performance are described. New stationary phases and phase supports that have been reported over the past decade are detailed, with a focus on their use in capillary formats. A discussion on the instrument developments that have been required to ensure that extra-column effects do not diminish the intrinsic efficiency of these columns during analysis is also included. Finally, the impact of these capillary UHPLC topics on the field of proteomics and ways in which capillary UHPLC may continue to be applied to the separation of complex samples are addressed. Copyright © 2017 Elsevier B.V. All rights reserved.

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

PubMed

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.

Analysis of packing microstructure and wall effects in a narrow-bore ultrahigh pressure liquid chromatography column using focused ion-beam scanning electron microscopy.

PubMed

Reising, Arved E; Schlabach, Sabine; Baranau, Vasili; Stoeckel, Daniela; Tallarek, Ulrich

2017-09-01

Column wall effects are well recognized as major limiting factor in achieving high separation efficiency in HPLC. This is especially important for modern analytical columns packed with small particles, where wall effects dominate the band broadening. Detailed knowledge about the packing microstructure of packed analytical columns has so far not been acquired. Here, we present the first three-dimensional reconstruction protocol for these columns utilizing focused ion-beam scanning electron microscopy (FIB-SEM) on a commercial 2.1mm inner diameter×50mm length narrow-bore analytical column packed with 1.7μm bridged-ethyl hybrid silica particles. Two sections from the packed bed are chosen for reconstruction by FIB-SEM: one from the bulk packing region of the column and one from its critical wall region. This allows quantification of structural differences between the wall region and the center of the bed due to effects induced by the hard, confining column wall. Consequences of these effects on local flow velocity in the column are analyzed with flow simulations utilizing the lattice-Boltzmann method. The reconstructions of the bed structures reveal significant structural differences in the wall region (extending radially over approximately 62 particle diameters) compared to the center of the column. It includes the local reduction of the external porosity by up to 10% and an increase of the mean particle diameter by up to 3%, resulting in a decrease of the local flow velocity by up to 23%. In addition, four (more ordered) layers of particles in the direct vicinity of the column wall induce local velocity fluctuations by up to a factor of three regarding the involved velocity amplitudes. These observations highlight the impact of radial variations in packing microstructure on band migration and column performance. This knowledge on morphological peculiarities of column wall effects helps guiding us towards further optimization of the packing process for analytical HPLC columns. Copyright © 2017 Elsevier B.V. All rights reserved.

Separation of amino acids and antibiotics by narrow-bore and normal-bore high-performance liquid chromatography with pre-column derivatization.

PubMed

Fiedler, H P; Plaga, A

1987-01-16

The selectivity, efficiency and lifetime of normal- and narrow-bore columns for high-performance liquid chromatography were investigated for the separation and quantification of amino acids and the amino acid-like antibiotics phosphinothricin and phosphinothricylalanylalanine in biological samples. These compounds were determined by an automated pre-column derivatization with o-phthalaldehyde-2-mercaptoethanol reagent and UV detection at 338 nm.

An improved method for purification of recombinant truncated heme oxygenase-1 by expanded bed adsorption and gel filtration.

PubMed

Hu, Hong-Bo; Wang, Wei; Han, Ling; Zhou, Wen-Pu; Zhang, Xue-Hong

2007-03-01

Recombinant truncated human heme oxygenase-1 (hHO-1) expressed in Escherichia coli was efficiently separated and purified from feedstock by DEAE-ion exchange expanded bed adsorption. Protocol optimization of hHO-1 on DEAE adsorbent resulted in adsorption in 0 M NaCl and elution in 150 mM NaCl at a pH of 8.5. The active enzyme fractions separated from the expanded bed column were further purified by a Superdex 75 gel filtration step. The specific hHO-1 activity increased from 0.82 +/- 0.05 to 24.8 +/- 1.8 U/mg during the whole purification steps. The recovery and purification factor of truncated hHO-1 of the whole purification were 72.7 +/- 4.7 and 30.2 +/- 2.3%, respectively. This purification process can decrease the demand on the preparation of feedstock and simplify the purification process.

Superficially porous particles columns for super fast HPLC separations.

PubMed

Ali, Imran; Al-Othman, Zeid A; Al-Za'abi, Mohammed

2012-08-01

Superficially porous silica particles columns (SPSPCs) are manufactured by different companies. The most common have the brand names Halo, Ascentis Express and Kinetex. These columns provide super fast, sharp peaks and moderate sample loading and back pressure. These are available in different chemistries such as C₈, C₁₈, RP Amide and Hilic. Normally, the silica gel particles have 2.7 and 1.7 µm total and inner solid core diameters with 0.5 µm thick outer porous layer, 90 Å pore size and 150 m²/g surface area. They have been used for the separation and identification of low and high molecular weight compounds. The present article describes the state of the art of superficially porous silica particles based columns with special emphasis on their structures, mechanisms of separation, applications and comparison. Copyright © 2012 John Wiley & Sons, Ltd.

Removal efficiency of multiple poly- and perfluoroalkyl substances (PFASs) in drinking water using granular activated carbon (GAC) and anion exchange (AE) column tests.

PubMed

McCleaf, Philip; Englund, Sophie; Östlund, Anna; Lindegren, Klara; Wiberg, Karin; Ahrens, Lutz

2017-09-01

Poly- and perfluoroalkyl substances (PFASs) have been detected in drinking water at relatively high concentrations throughout the world which has led to implementation of regulatory guidelines for specific PFASs in drinking water in several European countries and in the U.S. The Swedish National Food Agency has determined that the drinking water of over one third of the country's municipal consumers is at risk or already affected by PFAS contamination. The present study investigated the effects of perfluorocarbon chain length, functional group and isomer structure (branched or linear) on removal of multiple PFASs using granular activated carbon (GAC, Filtrasorb ® 400) and anion exchange (AE, Purolite ® A600) column experiments. The removal of 14 different PFASs, i.e. the C 3 C 11 , C 14 perfluoroalkyl carboxylic acids (PFCAs) (PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUnDA, PFDoDA, PFTeDA), perfluorooctane sulfonamide (FOSA), and the C 4 , C 6 , C 8 perfluoroalkyl sulfonic acids (PFSAs) (PFBS, PFHxS, PFOS), was monitored for a 217 day period. The results indicate the selective nature of PFAS removal as the absorbents are loaded with PFASs and dissolved organic carbon (DOC). A clear relationship between perfluorocarbon chain length and removal efficiency of PFASs using GAC and AE was found while PFASs with sulfonate functional groups displayed greater removal efficiency than those with carboxylate groups. Similarly, time to column breakthrough increased with increasing perfluorocarbon chain length and was greater for the PFSAs than the PFCAs for both GAC and AE. Shorter carbon chained PFASs such as PFBA, PFPeA, PFHxA showed desorption behavior and long-chained PFASs showed increased removal towards the end of the experiment indicating agglomeration or micelle development. Linear isomers of PFOS, PFHxS, and perfluorooctane sulfonamide (FOSA) had greater column removal efficiencies using GAC (and also for AE at greater bed volume throughput) than the branched and this difference increased at greater bed volume throughputs. The GAC and AE columns showed a poor correlation between DOC and PFAS removal efficiency. The results indicate that designers and operators of AE and GAC treatment processes must take into consideration the selective nature of PFAS removal and associated desorption of short-chain PFCAs during co-removal of multiple PFASs. Copyright © 2017 Elsevier Ltd. All rights reserved.

Removal of dichloromethane from waste gas streams using a hybrid bubble column/biofilter bioreactor

PubMed Central

2014-01-01

The performance of a hybrid bubble column/biofilter (HBCB) bioreactor for the removal of dichloromethane (DCM) from waste gas streams was studied in continuous mode for several months. The HBCB bioreactor consisted of two compartments: bubble column bioreactor removing DCM from liquid phase and biofilter removing DCM from gas phase. Effect of inlet DCM concentration on the elimination capacity was examined in the DCM concentration range of 34–359 ppm with loading rates ranged from 2.2 to 22.8 g/m3.h and constant total empty bed retention time (EBRT) of 200 s. In the equal loading rates, the elimination capacity and removal efficiency of the biofilter were higher than the corresponding values of the bubble column bioreactor. The maximum elimination capacity of the HBCB bioreactor was determined to be 15.7 g/m3.h occurred in the highest loading rate of 22.8 g/m3.h with removal efficiency of 69%. The overall mineralization portion of the HBCB bioreactor was in the range of 72-79%. The mixed liquor acidic pH especially below 5.5 inhibited microbial activity and decreased the elimination capacity. Inhibitory effect of high ionic strength was initiated in the mixed liquor electrical conductivity of 12.2 mS/cm. This study indicated that the HBCB bioreactor could benefit from advantages of both bubble column and biofilter reactors and could remove DCM from waste gas streams in a better manner. PMID:24406056

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

PubMed

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

2018-06-06

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

[Determination of patulin in fruits and jam by solid phase extraction-ultra performance liquid chromatography].

PubMed

Lü, Weichao; Shen, Shuchang; Wang, Chao

2017-11-08

With magnesium silicate, silica gel, diatomite and calcium sulfate as raw materials, a new solid phase extraction column was prepared through a series of processes of grinding to ethanol homogenate, drying and packing into polypropylene tube. The sample was hydrolyzed by pectinase, extracted by acetonitrile and purified by solid phase extraction. The target compounds were separated on a C18 column (100 mm×2.1 mm, 1.8 μm), using 0.8% (v/v) tetrahydrofuran solution as mobile phase with a flow rate of 0.5 mL/min. The detection wavelength was 276 nm. The effect of pectinase on extraction yield and purification effect of solid-phase extraction column were investigated. The optimum chromatographic conditions were selected. There was a good linear relationship between the peak heights and the mass concentrations of patulin in the range of 0.1 to 10 mg/L with the correlation coefficient ( R 2 ) of 1. The limit of detection for this method was 10.22 μg/kg. The spiked recoveries of samples were 86.58%-94.84% with the relative standard deviations (RSDs) of 1.45%-2.28%. The results indicated that the self-made solid phase extraction column had a good purification efficiency, and the UPLC had a high separation efficiency. The method is simple, accurate and of great significance for the quality and safety control of fruit products.

Investigating Attachment Behaviors of Cryptosporidium Parvum Oocysts Using Collision Efficiency in Laboratory Column Experiments

NASA Astrophysics Data System (ADS)

Park, Y.; Hou, L.; Atwill, R.; Packman, A. I.; Harter, T.

2009-12-01

Cryptosporidium is one of the most common enteric parasites of humans and domestic animals, and a number of outbreaks of Cryprosporidiosis, a diarrheal disease caused by Cryptosporidium have been reported worldwide. Natural porous media has been demonstrated to be an effective filter for removing Cryptosporidium parvum from contaminated water and the amount of Cryptosporidium filtered is known to be highly dependent on physical and chemical conditions of the porous media and the water. Cryptosporidium deposition in saturated porous media involves two main steps: approach and attachment. In contrast to the approach mechanisms, attachment processes have not been systematically described to predict a priori because theories that represent attachment behavior (colloid stability) such as DLVO are insufficient to explain experimental data. For this reason, attachment efficiency is calculated based on empirical data, typically experimental breakthrough curves in laboratory columns or field experiments. In this study, collision (attachment) efficiencies (α) of C. parvum oocyst were calculated to test the effect of chemical property changes on the association of oocysts with sand grains. The breakthrough curve data obtained from twelve column experiments and three models were employed to calculate single collector efficiency (η) and α. The first ten experiments were conducted by changing ionic strength and pH, and mixing with natural sediments under the same physical properties (same η). Our experiment results show that iron coating or clay/suspended solids mixture drastically enhanced oocyst deposition. The experiments also showed that increase in ionic strength and decrease in pH enhanced the attachment efficiency. However, the experiment with 100mM NaCl resulted in low attachment efficiency and the experiment with pH 8.5 showed similar attachment efficiency to the one at pH 7. Based on the results from two additional experiments with different flow velocities, it appears that attachment efficiency changes when the flow velocity changes, which contradicts CFT. The results prove that predicting attachment efficiency of C. parvum oocyst using ionic strength or pH is inappropriate when non-DLVO interactions are involved. A review of our results and comparison to existing data shows that it is challenging to accurately predict the attachment efficiency using single peak value of breakthrough curve data from geochemical information of porous media.

Conventional-Flow Liquid Chromatography-Mass Spectrometry for Exploratory Bottom-Up Proteomic Analyses.

PubMed

Lenčo, Juraj; Vajrychová, Marie; Pimková, Kristýna; Prokšová, Magdaléna; Benková, Markéta; Klimentová, Jana; Tambor, Vojtěch; Soukup, Ondřej

2018-04-17

Due to its sensitivity and productivity, bottom-up proteomics based on liquid chromatography-mass spectrometry (LC-MS) has become the core approach in the field. The de facto standard LC-MS platform for proteomics operates at sub-μL/min flow rates, and nanospray is required for efficiently introducing peptides into a mass spectrometer. Although this is almost a "dogma", this view is being reconsidered in light of developments in highly efficient chromatographic columns, and especially with the introduction of exceptionally sensitive MS instruments. Although conventional-flow LC-MS platforms have recently penetrated targeted proteomics successfully, their possibilities in discovery-oriented proteomics have not yet been thoroughly explored. Our objective was to determine what are the extra costs and what optimization and adjustments to a conventional-flow LC-MS system must be undertaken to identify a comparable number of proteins as can be identified on a nanoLC-MS system. We demonstrate that the amount of a complex tryptic digest needed for comparable proteome coverage can be roughly 5-fold greater, providing the column dimensions are properly chosen, extra-column peak dispersion is minimized, column temperature and flow rate are set to levels appropriate for peptide separation, and the composition of mobile phases is fine-tuned. Indeed, we identified 2 835 proteins from 2 μg of HeLa cells tryptic digest separated during a 60 min gradient at 68 μL/min on a 1.0 mm × 250 mm column held at 55 °C and using an aqua-acetonitrile mobile phases containing 0.1% formic acid, 0.4% acetic acid, and 3% dimethyl sulfoxide. Our results document that conventional-flow LC-MS is an attractive alternative for bottom-up exploratory proteomics.

Site-directed immobilization of a genetically engineered anti-methotrexate antibody via an enzymatically introduced biotin label significantly increases the binding capacity of immunoaffinity columns.

PubMed

Davenport, Kaitlynn R; Smith, Christopher A; Hofstetter, Heike; Horn, James R; Hofstetter, Oliver

2016-05-15

In this study, the effect of random vs. site-directed immobilization techniques on the performance of antibody-based HPLC columns was investigated using a single-domain camelid antibody (VHH) directed against methotrexate (MTX) as a model system. First, the high flow-through support material POROS-OH was activated with disuccinimidyl carbonate (DSC), and the VHH was bound in a random manner via amines located on the protein's surface. The resulting column was characterized by Frontal Affinity Chromatography (FAC). Then, two site-directed techniques were explored to increase column efficiency by immobilizing the antibody via its C-terminus, i.e., away from the antigen-binding site. In one approach, a tetra-lysine tail was added, and the antibody was immobilized onto DSC-activated POROS. In the second site-directed approach, the VHH was modified with the AviTag peptide, and a biotin-residue was enzymatically incorporated at the C-terminus using the biotin ligase BirA. The biotinylated antibody was subsequently immobilized onto NeutrAvidin-derivatized POROS. A comparison of the FAC analyses, which for all three columns showed excellent linearity (R(2)>0.999), revealed that both site-directed approaches yield better results than the random immobilization; the by far highest efficiency, however, was determined for the immunoaffinity column based on AviTag-biotinylated antibody. As proof of concept, all three columns were evaluated for quantification of MTX dissolved in phosphate buffered saline (PBS). Validation using UV-detection showed excellent linearity in the range of 0.04-12μM (R(2)>0.993). The lower limit of detection (LOD) and lower limit of quantification (LLOQ) were found to be independent of the immobilization strategy and were 40nM and 132nM, respectively. The intra- and inter-day precision was below 11.6%, and accuracy was between 90.7% and 112%. To the best of our knowledge, this is the first report of the AviTag-system in chromatography, and the first application of immunoaffinity chromatography for the analysis of MTX. Copyright © 2016 Elsevier B.V. All rights reserved.

Comparative evaluation of seven commercial products for human serum enrichment/depletion by shotgun proteomics.

PubMed

Pisanu, Salvatore; Biosa, Grazia; Carcangiu, Laura; Uzzau, Sergio; Pagnozzi, Daniela

2018-08-01

Seven commercial products for human serum depletion/enrichment were tested and compared by shotgun proteomics. Methods were based on four different capturing agents: antibodies (Qproteome Albumin/IgG Depletion kit, ProteoPrep Immunoaffinity Albumin and IgG Depletion Kit, Top 2 Abundant Protein Depletion Spin Columns, and Top 12 Abundant Protein Depletion Spin Columns), specific ligands (Albumin/IgG Removal), mixture of antibodies and ligands (Albumin and IgG Depletion SpinTrap), and combinatorial peptide ligand libraries (ProteoMiner beads), respectively. All procedures, to a greater or lesser extent, allowed an increase of identified proteins. ProteoMiner beads provided the highest number of proteins; Albumin and IgG Depletion SpinTrap and ProteoPrep Immunoaffinity Albumin and IgG Depletion Kit resulted the most efficient in albumin removal; Top 2 and Top 12 Abundant Protein Depletion Spin Columns decreased the overall immunoglobulin levels more than other procedures, whereas specifically gamma immunoglobulins were mostly removed by Albumin and IgG Depletion SpinTrap, ProteoPrep Immunoaffinity Albumin and IgG Depletion Kit, and Top 2 Abundant Protein Depletion Spin Columns. Albumin/IgG Removal, a resin bound to a mixture of protein A and Cibacron Blue, behaved less efficiently than the other products. Copyright © 2018 Elsevier B.V. All rights reserved.

Enhanced biological nutrients removal using an integrated oxidation ditch with vertical circle from wastewater by adding an anaerobic column.

PubMed

Wang, Shu-mei; Liu, Jun-xin

2005-01-01

Compared to conventional oxidation ditches, an integrated oxidation ditch with vertical circle (IODVC) has the characters of concise configuration, simple operation and maintenance, land saving and automatical sludge returning. By the utilization of vertical circulation, an aerobic zone and an anoxic zone can be unaffectedly formed in the IODVC. Therefore, COD and nitrogen can be efficiently removed. However, the removal efficiency of phosphorus was low in the IODVC. In the experiment described, a laboratory scale system to add an anaerobic column to the IODVC has been tested to investigate the removal of phosphorus from wastewater. The experimental results showed that the removal efficiency of TP with the anaerobic column was increased to 54.0% from 22.3% without the anaerobic column. After the acetic sodium was added into the influent as carbon sources, the mean TP removal efficency of 77.5% was obtained. At the same time, the mean removal efficiencies of COD, TN and NH3-N were 92.2%, 81.6% and 98.1%, respectively, at 12 h of HRT and 21-25 d of SRT. The optimal operational conditions in this study were as follows: recycle rate = 1.5-2.0, COD/TN > 6, COD/TP > 40, COD loading rate = 0.26-0.32 kgCOD/(kgSS x d), TN loading rate = 0.028-0.034 kgTN/(kgSS x d) and TP loading rate = 0.003-0.005 kgTP/(kgSS x d), respectively.

An OAIS-Based Hospital Information System on the Cloud: Analysis of a NoSQL Column-Oriented Approach.

PubMed

Celesti, Antonio; Fazio, Maria; Romano, Agata; Bramanti, Alessia; Bramanti, Placido; Villari, Massimo

2018-05-01

The Open Archive Information System (OAIS) is a reference model for organizing people and resources in a system, and it is already adopted in care centers and medical systems to efficiently manage clinical data, medical personnel, and patients. Archival storage systems are typically implemented using traditional relational database systems, but the relation-oriented technology strongly limits the efficiency in the management of huge amount of patients' clinical data, especially in emerging cloud-based, that are distributed. In this paper, we present an OAIS healthcare architecture useful to manage a huge amount of HL7 clinical documents in a scalable way. Specifically, it is based on a NoSQL column-oriented Data Base Management System deployed in the cloud, thus to benefit from a big tables and wide rows available over a virtual distributed infrastructure. We developed a prototype of the proposed architecture at the IRCCS, and we evaluated its efficiency in a real case of study.

MBBR evaluation for oil refinery wastewater treatment, with post-ozonation and BAC, for wastewater reuse.

PubMed

Schneider, E E; Cerqueira, A C F P; Dezotti, M

2011-01-01

This work evaluated the performance of a Moving Bed Biofilm Reactor (MBBR) in the treatment of an oil refinery wastewater. Also, it investigated the possibility of reuse of the MBBR effluent, after ozonation in series with a biological activated carbon (BAC) column. The best performance of the MBBR was achieved with a hydraulic retention time (HRT) of 6 hours, employing a bed to bioreactor volume ratio (V(B)/V(R)) of 0.6. COD and N-NH₄(+) MBBR effluent concentrations ranged from 40 to 75 mg L⁻¹ (removal efficiency of 69-89%) and 2 to 6 mg L⁻¹ (removal efficiency of 45-86%), respectively. Ozonation carried out for 15 min with an ozone concentration of 5 mg L⁻¹ was able to improve the treated wastewater biodegradability. The treatment performance of the BAC columns was practically the same for ozonated and non ozonated MBBR effluents. The dissolved organic carbon (DOC) content of the columns of the activated carbon columns (CAG) was in the range of 2.1-3.8 mg L⁻¹, and the corresponding DOC removal efficiencies were comprised between 52 and 75%. The effluent obtained at the end of the proposed treatment presented a quality, which meet the requirements for water reuse in the oil refinery.

Preparation of chitosan-graft-(β-cyclodextrin) based sol-gel stationary phase for open-tubular capillary electrochromatography.

PubMed

Lü, Haixia; Li, Qingyin; Yu, Xiaowei; Yi, Jiaojiao; Xie, Zenghong

2013-07-01

A novel open-tubular CEC column coated with chitosan-graft-(β-CD) (CDCS) was prepared using sol-gel technique. In the sol-gel approach, owing to the 3D network of sol-gel and the strong chemical bond between the stationary phase and the surface of capillary columns, good chromatographic characteristics and unique selectivity in separating isomers were shown. The column efficiencies of 55,000∼163,000 plates/m for the isomeric xanthopterin and phenoxy acid herbicides using the sol-gel-derived CDCS columns were achieved. Good stabilities were demonstrated that the RSD values for the retention time of thiourea and isoxanthopterin were 1.3 and 1.4% (run to run, n = 5), 1.6 and 2.0% (day to day, n = 3), 2.9 and 3.1% (column to column, n = 3), respectively. The sol-gel-coated CDCS columns have shown improved separations of isomeric xanthopterin in comparison with CDCS-bonded capillary column. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Immobilization of uranium and arsenic by injectible iron and hydrogen stimulated autotrophic sulphate reduction

NASA Astrophysics Data System (ADS)

Burghardt, D.; Simon, E.; Knöller, K.; Kassahun, A.

2007-12-01

The main object of the study was the development of a long-term efficient and inexpensive in-situ immobilization technology for uranium (U) and arsenic (As) in smaller and decentralized groundwater discharges from abandoned mining processing sites. Therefore, corrosion of grey cast iron (gcFe) and nano-scale iron particles (naFe) as well as hydrogen stimulated autotrophic sulphate reduction (aSR) were investigated. Two column experiments with sulphate reducing bacterias (SRB) (biotic gcFe , biotic naFe) and one abiotic gcFe-column experiment were performed. In the biotic naFe column, no particle translocation was observed and a temporary but intensive naFe corrosion indicated by a decrease in Eh, a pH increase and H 2 evolution. Decreasing sulphate concentrations and 34S enrichment in the column effluent indicated aSR. Fe(II) retention could be explained by siderite and consequently FeS precipitation by geochemical modeling (PhreeqC). U and As were completely immobilised within the biotic naFe column. In the biotic gcFe column, particle entrapment in open pore spaces resulted in a heterogeneous distribution of Fe-enriched zones and an increase in permeability due to preferential flow. However, Fe(II) concentrations in the effluent indicated a constant and lasting gcFe corrosion. An efficient immobilization was found for As, but not for U.

On-line SPE-UHPLC method using fused core columns for extraction and separation of nine illegal dyes in chilli-containing spices.

PubMed

Khalikova, Maria A; Satínský, Dalibor; Smidrkalová, Tereza; Solich, Petr

2014-12-01

The presented work describes the development of a simple, fast and effective on-line SPE-UHPLC-UV/vis method using fused core particle columns for extraction, separation and quantitative analysis of the nine illegal dyes, most frequently found in chilli-containing spices. The red dyes Sudan I-IV, Sudan Red 7B, Sudan Red G, Sudan Orange G, Para Red, and Methyl Red were separated and analyzed in less than 9 min without labor-consuming pretreatment procedure. The chromatographic separation was performed on Ascentis Express RP-Amide column with gradient elution using mixture of acetonitrile and water, as a mobile phase at a flow rate of 1.0 mL min(-1) and 55°C of temperature. As SPE sorbent for cleanup and pre-concentration of illegal dyes short guard fused core column Ascentis Express F5 was used. The applicability of proposed method was proven for three different chilli-containing commercial samples. Recoveries for all compounds were between 90% and 108% and relative standard deviation ranged from 1% to 4% for within- and from 2% to 6% for between-day. Limits of detection showed lower values than required by European Union regulations and were in the range of 3.3-10.3 µg L(-1) for standard solutions, 5.6-235.6 µg kg(-1) for chilli-containing spices. Copyright © 2014 Elsevier B.V. All rights reserved.

Effect of bio-column composed of aged refuse on methane abatement--a novel configuration of biological oxidation in refuse landfill.

PubMed

Han, Dan; Zhao, Youcai; Xue, Binjie; Chai, Xiaoli

2010-01-01

An experimental bio-column composed of aged refuse was installed around the exhaust pipe as a new way to mitigate methane in refuse landfill. One of the objectives of this work was to assess the effect of aged refuse thickness in bio-column on reducing CH4 emissions. Over the study period, methane oxidation was observed at various thicknesses, 5 cm (small size), 10 cm (middle size) and 15 cm (large size), representing one to three times of pipeline diameters. The middle and large size both showed over 90% methane conversion, and the highest methane conversion rate of above 95% occurred in the middle-size column cell. Michaelis-Menten equation addressed the methanotrophs diffusion in different layers of the bio-columns. Maximum methanotrophic activity (Vmax) measured at the three thicknesses ranged from 6.4 x 10(-3) to 15.6 x 10(-3) units, and the half-saturation value (K(M)) ranged from 0.85% to 1.67%. Both the highest Vmax and K(M) were observed at the middle-size of the bio-column, as well as the largest methanotrophs population, suggesting a significant efficiency of methane mitigation happened in the optimum zone with greatest affinity and methanotrophic bacteria activities. Therefore, bio-column is a potential style for methane abatement in landfill, and the aged refuse both naturally formed and artificially placed in the column plays a critical role in CH4 emission.

Separation of cannabinoids on three different mixed-mode columns containing carbon/nanodiamond/amine-polymer superficially porous particles.

PubMed

Hung, Chuan-Hsi; Zukowski, Janusz; Jensen, David S; Miles, Andrew J; Sulak, Clayton; Dadson, Andrew E; Linford, Matthew R

2015-09-01

Three mixed-mode high-performance liquid chromatography columns packed with superficially porous carbon/nanodiamond/amine-polymer particles were used to separate mixtures of cannabinoids. Columns evaluated included: (i) reversed phase (C18 ), weak anion exchange, 4.6 × 33 mm, 3.6 μm, and 4.6 × 100 mm, 3.6 μm, (ii) reversed phase, strong anion exchange (quaternary amine), 4.6×33 mm, 3.6 μm, and (iii) hydrophilic interaction liquid chromatography, 4.6 × 150 mm, 3.6 μm. Different selectivities were achieved under various mobile phase and stationary phase conditions. Efficiencies and peak capacities were as high as 54 000 N/m and 56, respectively. The reversed phase mixed-mode column (C18 ) retained tetrahydrocannabinolic acid strongly under acidic conditions and weakly under basic conditions. Tetrahydrocannabinolic acid was retained strongly on the reversed phase, strong anion exchange mixed-mode column under basic polar organic mobile phase conditions. The hydrophilic interaction liquid chromatography column retained polar cannabinoids better than the (more) neutral ones under basic conditions. A longer reversed phase (C18 ) mixed-mode column (4.6 × 100 mm) showed better resolution for analytes (and a contaminant) than a shorter column. Fast separations were achieved in less than 5 min and sometimes 2 min. A real world sample (bubble hash extract) was also analyzed by gradient elution. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Topics in Chemical Instrumentation--An Introduction to Supercritical Fluid Chromatography: Part 1: Principles and Instrumentation.

ERIC Educational Resources Information Center

Palmieri, Margo D.

1988-01-01

Identifies the properties and characteristics of supercritical fluids. Discusses the methodology for supercritical fluid chromatography including flow rate, plate height, column efficiency, viscosity, and other factors. Reviews instruments, column types, and elution conditions. Lists supercritical fluid data for 22 compounds, mostly organic. (MVL)

Sol-gel open tubular ODS columns with reversed electroosmotic flow for capillary electrochromatography.

PubMed

Hayes, J D; Malik, A

2001-03-01

Sol-gel chemistry was successfully used for the fabrication of open tubular columns with surface-bonded octadecylsilane (ODS) stationary-phase coating for capillary electrochromatography (OT-CEC). Following column preparations, a series of experiments were performed to investigate the performance of the sol-gel coated ODS columns in OT-CEC. The incorporation of N-octadecyldimethyl[3-(trimethoxysilyl)propyl]ammonium chloride as one of the sol-gel precursors played an important role in the electrochromatographic performance of the prepared columns. This chemical reagent possesses a chromatographically favorable, bonded ODS moiety, in conjunction with three methoxy groups allowing for sol-gel reactivity. In addition, a positively charged nitrogen atom is present in the molecular structure of this reagent and provides a positively charged capillary surface responsible for the reversed electroosmotic flow (EOF) in the columns during CEC operation. Comparative studies involving the EOF within such sol-gel ODS coated and uncoated capillaries were performed using acetonitrile and methanol as the organic modifiers in the mobile phase. The use of a deactivating reagent, phenyldimethylsilane, in the sol-gel solution was evaluated. Efficiency values of over 400,000 theoretical plates per meter were achieved in CEC on a 64 cm x 25 microm i.d. sol-gel ODS open tubular column. Test mixtures of polycyclic aromatic hydrocarbons, benzene derivatives, and aromatic aldehydes and ketones were used to evaluate the CEC performances of both nondeactivated and deactivated open tubular sol-gel columns. The effects of mobile-phase organic modifier contents and pH on EOF in such columns were evaluated. The prepared sol-gel ODS columns are characterized by switchable electroosmotic flow. A pH value of approximately 8.5 was found correspond to the isoelectric point for the prepared sol-gel ODS coatings.

Growing Cobalt Silicide Columns In Silicon

NASA Technical Reports Server (NTRS)

Fathauer, Obert W.

1991-01-01

Codeposition by molecular-beam epitaxy yields variety of structures. Proposed fabrication process produces three-dimensional nanometer-sized structures on silicon wafers. Enables control of dimensions of metal and semiconductor epitaxial layers in three dimensions instead of usual single dimension (perpendicular to the plane of the substrate). Process used to make arrays of highly efficient infrared sensors, high-speed transistors, and quantum wires. For fabrication of electronic devices, both shapes and locations of columns controlled. One possible technique for doing this electron-beam lithography, see "Making Submicron CoSi2 Structures on Silicon Substrates" (NPO-17736).

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

PubMed

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

2007-09-14

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

Study on Gas-liquid Falling Film Flow in Internal Heat Integrated Distillation Column

NASA Astrophysics Data System (ADS)

Liu, Chong

2017-10-01

Gas-liquid internally heat integrated distillation column falling film flow with nonlinear characteristics, study on gas liquid falling film flow regulation control law, can reduce emissions of the distillation column, and it can improve the quality of products. According to the distribution of gas-liquid mass balance internally heat integrated distillation column independent region, distribution model of heat transfer coefficient of building internal heat integrated distillation tower is obtained liquid distillation falling film flow in the saturated vapour pressure of liquid water balance, using heat transfer equation and energy equation to balance the relationship between the circulating iterative gas-liquid falling film flow area, flow parameter information, at a given temperature, pressure conditions, gas-liquid flow falling film theory makes the optimal parameters to achieve the best fitting value with the measured values. The results show that the geometric gas-liquid internally heat integrated distillation column falling film flow heat exchange area and import column thermostat, the average temperature has significant. The positive correlation between the heat exchanger tube entrance due to temperature difference between inside and outside, the heat flux is larger, with the increase of internal heat integrated distillation column temperature, the slope decreases its temperature rise, which accurately describes the internal gas-liquid heat integrated distillation tower falling film flow regularity, take appropriate measures to promote the enhancement of heat transfer. It can enhance the overall efficiency of the heat exchanger.

Cell Therapy to Obtain Spinal Fusion

DTIC Science & Technology

2006-02-01

al, 2005). Since our previous studies (first progress report) demonstrated a significant reduction (≥50%) in the amount of BMP2 secreted from human...Ad5eGFP 2,500vp/cell, (3) Ad5eGFP 5,000vp/cell, or (4) Ad5eGFP 10,000vp/cell in the absence (solid columns) or presence ( open columns) of GeneJammer...20-fold reduction in BMP-2 protein compared with the controls (p < 0.001) and the expression was biphasic over the 15 d period with highest expression

Efficient secretory expression of the sweet-tasting protein brazzein in the yeast Kluyveromyces lactis.

PubMed

Jo, Hyun-Joo; Noh, Jin-Seok; Kong, Kwang-Hoon

2013-08-01

Brazzein is an intensely sweet-tasting protein with high water solubility, heat stability, and taste properties resembling those of carbohydrate sweeteners. In the present study, we describe the expression of the synthetic gene encoding brazzein, a sweet protein in the yeast Kluyveromyces lactis. The synthetic brazzein gene was designed based on the biased codons of the yeast, so as to optimize its expression, as well as on the extracellular secretion for expression in an active, soluble form. The synthesized brazzein gene was cloned into the secretion vector pKLAC2, which contains the yeast prepropeptide signal from the Saccharomycescerevisiae α-mating factor. The constructed plasmid pKLAC2-des-pE1M-brazzein was introduced into the yeast K. lactis GG799. The yeast transformants were cultured for high-yield secretion of the recombinant des-pE1M-brazzein in YPGal medium for 96 h at 30°C. The expressed recombinant des-pE1M-brazzein was purified by CM-Sepharose column chromatography and approximately 104 mg/L was obtained. The purity and conformational state of the recombinant des-pE1M-brazzein were confirmed using SDS-PAGE, HPLC, and circular dichroism. The identity of the recombinant protein was also confirmed by N-terminal amino acid analysis and taste testing. The purified recombinant des-pE1M-brazzein had an intrinsic sweetness in its minor form, approximately 2130 times sweeter than sucrose on a weight basis. These results demonstrate that the K. lactis expression system is useful for producing the recombinant brazzein in active form at a high yield with attributes useful in the food industry. Copyright © 2013 Elsevier Inc. All rights reserved.

Trypsin coatings on electrospun and alcohol-dispersed polymer nanofibers for trypsin digestion column

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

Jun, Seung-Hyun; Chang, Mun Seock; Kim, Byoung Chan

2010-09-15

The construction of a trypsin reactor in a chromatography column for rapid and efficient protein digestion in proteomics is described. Electrospun and alcohol-dispersed polymer nanofibers were used for the fabrication of highly stable trypsin coating, which was prepared by a two-step process of covalent attachment and enzyme crosslinking. In a comparative study with the trypsin coatings on asspun and non-dispersed nanofibers, it has been observed that a simple step of alcohol dispersion improved not only the enzyme loading but also the performance of protein digestion. In-column digestion of enolase was successfully performed in less than twenty minutes. By applying themore » alcohol dispersion of polymer nanofibers, the bypass of samples was reduced by filling up the column with well-dispersed nanofibers, and subsequently, interactions between the protein and the enzymes were improved yielding more complete and reproducible digestions. Regardless of alcohol-dispersion or not, trypsin coating showed better digestion performance and improved performance stability under recycled uses than covalently-attached trypsin. The combination of highly stable trypsin coating and alcoholdispersion of polymer nanofibers has opened up a new potential to develop a trypsin column for on-line and automated protein digestion.« less

Chocolate HILIC phases: development and characterization of novel saccharide-based stationary phases by applying non-enzymatic browning (Maillard reaction) on amino-modified silica surfaces.

PubMed

Schuster, Georg; Lindner, Wolfgang

2011-06-01

Novel saccharide-based stationary phases were developed by applying non-enzymatic browning (Maillard Reaction) on aminopropyl silica material. During this process, the reducing sugars glucose, lactose, maltose, and cellobiose served as "ligand primers". The reaction cascade using cellobiose resulted in an efficient chromatographic material which further served as our model Chocolate HILIC column. (Chocolate refers to the fact that these phases are brownish.) In this way, an amine backbone was introduced to facilitate convenient manipulation of selectivity by additional attractive or repulsive ionic solute-ligand interactions in addition to the typical HILIC retention mechanism. In total, six different test sets and five different mobile phase compositions were investigated, allowing a comprehensive evaluation of the new polar column. It became evident that, besides the so-called HILIC retention mechanism based on partition phenomena, additional adsorption mechanisms, including ionic interactions, take place. Thus, the new column is another example of a HILIC-type column characterized by mixed-modal retention increments. The glucose-modified materials exhibited the relative highest overall hydrophobicity of all grafted Chocolate HILIC columns which enabled retention of lipophilic analytes with high water content mobile phases.

A Rapid Spin Column-Based Method to Enrich Pathogen Transcripts from Eukaryotic Host Cells Prior to Sequencing

DOE PAGES

Bent, Zachary W.; Poorey, Kunal; LaBauve, Annette E.; ...

2016-12-21

When analyzing pathogen transcriptomes during the infection of host cells, the signal-to-background (pathogen-to-host) ratio of nucleic acids (NA) in infected samples is very small. Despite the advancements in next-generation sequencing, the minute amount of pathogen NA makes standard RNA-seq library preps inadequate for effective gene-level analysis of the pathogen in cases with low bacterial loads. In order to provide a more complete picture of the pathogen transcriptome during an infection, we developed a novel pathogen enrichment technique, which can enrich for transcripts from any cultivable bacteria or virus, using common, readily available laboratory equipment and reagents. To evenly enrich formore » pathogen transcripts, we generate biotinylated pathogen-targeted capture probes in an enzymatic process using the entire genome of the pathogen as a template. The capture probes are hybridized to a strand-specific cDNA library generated from an RNA sample. The biotinylated probes are captured on a monomeric avidin resin in a miniature spin column, and enriched pathogen-specific cDNA is eluted following a series of washes. To test this method, we performed an in vitro time-course infection using Klebsiella pneumoniae to infect murine macrophage cells. K. pneumoniae transcript enrichment efficiency was evaluated using RNA-seq. Bacterial transcripts were enriched up to ~400-fold, and allowed the recovery of transcripts from ~2000–3600 genes not observed in untreated control samples. These additional transcripts revealed interesting aspects of K. pneumoniae biology including the expression of putative virulence factors and the expression of several genes responsible for antibiotic resistance even in the absence of drugs.« less

A Rapid Spin Column-Based Method to Enrich Pathogen Transcripts from Eukaryotic Host Cells Prior to Sequencing

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

Bent, Zachary W.; Poorey, Kunal; LaBauve, Annette E.

When analyzing pathogen transcriptomes during the infection of host cells, the signal-to-background (pathogen-to-host) ratio of nucleic acids (NA) in infected samples is very small. Despite the advancements in next-generation sequencing, the minute amount of pathogen NA makes standard RNA-seq library preps inadequate for effective gene-level analysis of the pathogen in cases with low bacterial loads. In order to provide a more complete picture of the pathogen transcriptome during an infection, we developed a novel pathogen enrichment technique, which can enrich for transcripts from any cultivable bacteria or virus, using common, readily available laboratory equipment and reagents. To evenly enrich formore » pathogen transcripts, we generate biotinylated pathogen-targeted capture probes in an enzymatic process using the entire genome of the pathogen as a template. The capture probes are hybridized to a strand-specific cDNA library generated from an RNA sample. The biotinylated probes are captured on a monomeric avidin resin in a miniature spin column, and enriched pathogen-specific cDNA is eluted following a series of washes. To test this method, we performed an in vitro time-course infection using Klebsiella pneumoniae to infect murine macrophage cells. K. pneumoniae transcript enrichment efficiency was evaluated using RNA-seq. Bacterial transcripts were enriched up to ~400-fold, and allowed the recovery of transcripts from ~2000–3600 genes not observed in untreated control samples. These additional transcripts revealed interesting aspects of K. pneumoniae biology including the expression of putative virulence factors and the expression of several genes responsible for antibiotic resistance even in the absence of drugs.« less

Urban runoff treatment using nano-sized iron oxide coated sand with and without magnetic field applying

PubMed Central

2013-01-01

Increase of impervious surfaces in urban area followed with increases in runoff volume and peak flow, leads to increase in urban storm water pollution. The polluted runoff has many adverse impacts on human life and environment. For that reason, the aim of this study was to investigate the efficiency of nano iron oxide coated sand with and without magnetic field in treatment of urban runoff. In present work, synthetic urban runoff was treated in continuous separate columns system which was filled with nano iron oxide coated sand with and without magnetic field. Several experimental parameters such as heavy metals, turbidity, pH, nitrate and phosphate were controlled for investigate of system efficiency. The prepared column materials were characterized with Scanning Electron Microscopy (SEM) and Energy Dispersive X-ray analysis (EDXA) instruments. SEM and EDXA analyses proved that the sand has been coated with nano iron oxide (Fe3O4) successfully. The results of SEM and EDXA instruments well demonstrate the formation of nano iron oxide (Fe3O4) on sand particle. Removal efficiency without magnetic field for turbidity; Pb, Zn, Cd and PO4 were observed to be 90.8%, 73.3%, 75.8%, 85.6% and 67.5%, respectively. When magnetic field was applied, the removal efficiency for turbidity, Pb, Zn, Cd and PO4 was increased to 95.7%, 89.5%, 79.9%, 91.5% and 75.6% respectively. In addition, it was observed that coated sand and magnetic field was not able to remove NO3 ions. Statistical analyses of data indicated that there was a significant difference between removals of pollutants in two tested columns. Results of this study well demonstrate the efficiency of nanosized iron oxide-coated sand in treatment of urban runoff quality; upon 75% of pollutants could be removed. In addition, in the case of magnetic field system efficiency can be improved significantly. PMID:24360061

Global View of the Functional Molecular Organization of the Avian Cerebrum: Mirror Images and Functional Columns

PubMed Central

Jarvis, Erich D.; Yu, Jing; Rivas, Miriam V.; Horita, Haruhito; Feenders, Gesa; Whitney, Osceola; Jarvis, Syrus C.; Jarvis, Electra R.; Kubikova, Lubica; Puck, Ana E.P.; Siang-Bakshi, Connie; Martin, Suzanne; McElroy, Michael; Hara, Erina; Howard, Jason; Pfenning, Andreas; Mouritsen, Henrik; Chen, Chun-Chun; Wada, Kazuhiro

2014-01-01

Based on quantitative cluster analyses of 52 constitutively expressed or behaviorally regulated genes in 23 brain regions, we present a global view of telencephalic organization of birds. The patterns of constitutively expressed genes revealed a partial mirror image organization of three major cell populations that wrap above, around, and below the ventricle and adjacent lamina through the mesopallium. The patterns of behaviorally regulated genes revealed functional columns of activation across boundaries of these cell populations, reminiscent of columns through layers of the mammalian cortex. The avian functionally regulated columns were of two types: those above the ventricle and associated mesopallial lamina, formed by our revised dorsal mesopallium, hyperpallium, and intercalated hyperpallium; and those below the ventricle, formed by our revised ventral mesopallium, nidopallium, and intercalated nidopallium. Based on these findings and known connectivity, we propose that the avian pallium has four major cell populations similar to those in mammalian cortex and some parts of the amygdala: 1) a primary sensory input population (intercalated pallium); 2) a secondary intrapallial population (nidopallium/hyperpallium); 3) a tertiary intrapallial population (mesopallium); and 4) a quaternary output population (the arcopallium). Each population contributes portions to columns that control different sensory or motor systems. We suggest that this organization of cell groups forms by expansion of contiguous developmental cell domains that wrap around the lateral ventricle and its extension through the middle of the mesopallium. We believe that the position of the lateral ventricle and its associated mesopallium lamina has resulted in a conceptual barrier to recognizing related cell groups across its border, thereby confounding our understanding of homologies with mammals. PMID:23818122

Global view of the functional molecular organization of the avian cerebrum: mirror images and functional columns.

PubMed

Jarvis, Erich D; Yu, Jing; Rivas, Miriam V; Horita, Haruhito; Feenders, Gesa; Whitney, Osceola; Jarvis, Syrus C; Jarvis, Electra R; Kubikova, Lubica; Puck, Ana E P; Siang-Bakshi, Connie; Martin, Suzanne; McElroy, Michael; Hara, Erina; Howard, Jason; Pfenning, Andreas; Mouritsen, Henrik; Chen, Chun-Chun; Wada, Kazuhiro

2013-11-01

Based on quantitative cluster analyses of 52 constitutively expressed or behaviorally regulated genes in 23 brain regions, we present a global view of telencephalic organization of birds. The patterns of constitutively expressed genes revealed a partial mirror image organization of three major cell populations that wrap above, around, and below the ventricle and adjacent lamina through the mesopallium. The patterns of behaviorally regulated genes revealed functional columns of activation across boundaries of these cell populations, reminiscent of columns through layers of the mammalian cortex. The avian functionally regulated columns were of two types: those above the ventricle and associated mesopallial lamina, formed by our revised dorsal mesopallium, hyperpallium, and intercalated hyperpallium; and those below the ventricle, formed by our revised ventral mesopallium, nidopallium, and intercalated nidopallium. Based on these findings and known connectivity, we propose that the avian pallium has four major cell populations similar to those in mammalian cortex and some parts of the amygdala: 1) a primary sensory input population (intercalated pallium); 2) a secondary intrapallial population (nidopallium/hyperpallium); 3) a tertiary intrapallial population (mesopallium); and 4) a quaternary output population (the arcopallium). Each population contributes portions to columns that control different sensory or motor systems. We suggest that this organization of cell groups forms by expansion of contiguous developmental cell domains that wrap around the lateral ventricle and its extension through the middle of the mesopallium. We believe that the position of the lateral ventricle and its associated mesopallium lamina has resulted in a conceptual barrier to recognizing related cell groups across its border, thereby confounding our understanding of homologies with mammals. Copyright © 2013 Wiley Periodicals, Inc.

The Pythagorean table of opposites, symbolic classification, and Aristotle.

PubMed

Goldin, Owen

2015-06-01

At Metaphysics A 5 986a22-b2, Aristotle refers to a Pythagorean table, with two columns of paired opposites. I argue that 1) although Burkert and Zhmud have argued otherwise, there is sufficient textual evidence to indicate that the table, or one much like it, is indeed of Pythagorean origin; 2) research in structural anthropology indicates that the tables are a formalization of arrays of "symbolic classification" which express a pre-scientific world view with social and ethical implications, according to which the presence of a principle on one column of the table will carry with it another principle within the same column; 3) a close analysis of Aristotle's arguments shows that he thought that the table expresses real causal relationships; and 4) Aristotle faults the table of opposites with positing its principles as having universal application and with not distinguishing between those principles that are causally prior and those that are posterior. Aristotle's account of scientific explanation and his own explanations that he developed in accordance with this account are in part the result of his critical encounter with this prescientific Pythagorean table.

Enantioseparation of racemic aminoglutethimide using asynchronous simulated moving bed chromatography.

PubMed

Lin, Xiaojian; Gong, Rujin; Li, Jiaxu; Li, Ping; Yu, Jianguo; Rodrigues, Alirio E

2016-10-07

The separation of aminoglutethimide enantiomers by the continuous multicolumn chromatographic processes were investigated experimentally and theoretically, where the columns were packed with cellulose tris 3,5-dimethylphenyl-carbamate stationary phase (brand name Chiralcel OD) and mobile phase was a mixture of n-hexane and ethanol with monoethanolamine additive. The continuous enantioseparation processes included a synchronous shifting process (SMB) and an asynchronous shifting process (VARICOL), which allowed reducing the column number (here from six-column SMB to five-column VARICOL process). Transport-dispersive model with the consideration of both intraparticle mass transfer resistance and axial dispersion was adopted to design and optimize the operation conditions for the separation of aminoglutethimide enantiomers by SMB process and VARICOL process. According to the optimized operation conditions, experiments were carried out on VARICOL-Micro unit using five-column VARICOL process with 1/1.5/1.5/1 configuration and six-column SMB process with 1/2/2/1 configuration. Products of R-aminoglutethimide (R-AG) enantiomer and S-aminoglutethimide (S-AG) enantiomer with more than 99.0% purity were obtained continuously from extract stream and raffinate stream, respectively. Furthermore, the experiemntal data obtained from five-column VARICOL process were compared with that from six-column SMB process, the feasibility and efficiency for the separation of guaifenesin enantiomers by VARICOL processes were evaluated. Copyright © 2016 Elsevier B.V. All rights reserved.

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

PubMed

Kang, Jingwu; Wistuba, Dorothee; Schurig, Volker

2002-04-01

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

Refolding and simultaneous purification of recombinant human proinsulin from inclusion bodies on protein-folding liquid-chromatography columns.

PubMed

Yuan, Jie; Zhou, Huifang; Yang, Yicong; Li, Weimin; Wan, Yi; Wang, Lili

2015-05-01

Protein-folding liquid chromatography (PFLC) is an effective and scalable method for protein renaturation with simultaneous purification. However, it has been a challenge to fully refold inclusion bodies in a PFLC column. In this work, refolding with simultaneous purification of recombinant human proinsulin (rhPI) from inclusion bodies from Escherichia coli were investigated using the surface of stationary phases in immobilized metal ion affinity chromatography (IMAC) and high-performance size-exclusion chromatography (HPSEC). The results indicated that both the ligand structure on the surface of the stationary phase and the composition of the mobile phase (elution buffer) influenced refolding of rhPI. Under optimized chromatographic conditions, the mass recoveries of IMAC column and HPSEC column were 77.8 and 56.8% with purifies of 97.6 and 93.7%, respectively. These results also indicated that the IMAC column fails to refold rhPI, and the HPSEC column enables efficient refolding of rhPI with a low-urea gradient-elution method. The refolded rhPI was characterized by circular dichroism spectroscopy. The molecular weight of the converted human insulin was further confirmed with SDS-18% PAGE, Matrix-Assisted Laser Desorption/ Ionization Time of Flight Mass Spectrometry (MALDI-TOF-MS) and the biological activity assay by HP-RPLC. Copyright © 2014 John Wiley & Sons, Ltd.

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

PubMed

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

2017-05-19

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

The role of silica colloids on facilitated cesium transport through glass bead columns and modeling

NASA Astrophysics Data System (ADS)

Noell, Alan L.; Thompson, Joseph L.; Corapcioglu, M. Yavuz; Triay, Inés R.

1998-05-01

Groundwater colloids can act as a vector which enhances the migration of contaminants. While sorbed to mobile colloids, contaminants can be held in the aqueous phase which prevents them from interacting with immobile aquifer surfaces. In this study, an idealized laboratory set-up was used to examine the influence of amorphous silica colloids on the transport of cesium. Synthetic groundwater and saturated glass bead columns were used to minimize the presence of natural colloidal material. The columns were assembled in replicate, some packed with 150-210 μm glass bead and others packed with 355-420 μm glass beads. The colloids used in these experiments were 100 nm amorphous silica colloids from Nissan Chemical Company. In the absence of these colloids, the retardation factor for cesium was 8.0 in the 150-210 μm glass bead columns and 3.6 in the 355-420 μm glass bead columns. The influence of anthropogenic colloids was tested by injecting 0.09 pore volume slugs of an equilibrated suspension of cesium and colloids into the colloid-free columns. Although there was little noticeable facilitation in the smaller glass bead columns, there was a slight reduction in the retardation of cesium in the larger glass bead columns. This was attributed to cesium having less of a retention time in the larger glass bead columns. When cesium was injected into columns with a constant flux of colloids, the retardation of cesium was reduced by 14-32% in the 150-210 μm glass bead columns and by 38-51% in the 355-420 μm glass bead columns. A model based on Corapcioglu and Jiang (1993) [Corapcioglu, M.Y., Jiang, S., 1993. Colloid-facilitated groundwater contaminant transport, Water Resour. Res., 29 (7) 2215-2226] was compared with the experimental elution data. When equilibrium sorption expressions were used and the flux of colloids through the glass bead columns was constant, the colloid facilitated transport of cesium was able to be described using an effective retardation coefficient. Fully kinetic simulations, however, more accurately described the colloid facilitated transport of cesium.

Preparation of polyhedral oligomeric silsesquioxane based imprinted monolith.

PubMed

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

2015-12-18

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

A Fast Gradient Method for Nonnegative Sparse Regression With Self-Dictionary

NASA Astrophysics Data System (ADS)

Gillis, Nicolas; Luce, Robert

2018-01-01

A nonnegative matrix factorization (NMF) can be computed efficiently under the separability assumption, which asserts that all the columns of the given input data matrix belong to the cone generated by a (small) subset of them. The provably most robust methods to identify these conic basis columns are based on nonnegative sparse regression and self dictionaries, and require the solution of large-scale convex optimization problems. In this paper we study a particular nonnegative sparse regression model with self dictionary. As opposed to previously proposed models, this model yields a smooth optimization problem where the sparsity is enforced through linear constraints. We show that the Euclidean projection on the polyhedron defined by these constraints can be computed efficiently, and propose a fast gradient method to solve our model. We compare our algorithm with several state-of-the-art methods on synthetic data sets and real-world hyperspectral images.

An improved design of spiral tube assembly for separation of proteins by high-speed counter-current chromatography.

PubMed

Dasarathy, Dhweeja; Ito, Yoichiro

2015-10-30

A new spiral tube assembly was designed to improve the column capacity and partition efficiency for protein separation. This spiral tube assembly has greater column capacity than the original tubing because of an increase in radial grooves from 4 to 12 to accommodate more spiral layers and 12 narrow spots instead of 4 in each circular loop to interrupt the laminar flow that causes sample band broadening. Standard PTFE tubing (1.6mm ID) and the modified flat-twisted tubing were used as the separation column. The performances of both assemblies were compared for separating three stable test proteins including cytochrome c, myoglobin, and lysozyme using a two phase aqueous-aqueous solvent system composed of polyethylene glycol 1000 (12.5% w/w) and dibasic potassium phosphate (12.5% w/w). All samples were run at 1, 2, 3, and 5mL/min at both 800rpm and 1000rpm. The separation of these three protein samples produced high stationary phase retentions at 1, 2, and 3mL/min, yet separated efficiently at 5mL/min in 40min. After comparing the separation efficiency in terms of the peak resolutions, theoretical plate numbers, and separation times, it was determined that the flat-twisted tubing was more effective in separating these protein samples. In order to validate the efficacy of this novel assembly, a mixture of five protein samples (cytochrome c, myoglobin, ovalbumin, lysozyme, and hemoglobin) were separated, under the optimal conditions established with these three protein samples, at 1mL/min with a revolution speed of 1000rpm. There were high stationary phase retentions of around 60%, with effective separations, demonstrating the efficiency of the flat-twisted spiral tube assembly. The separation time of 6h was a limitation but can potentially be shortened by improving the strength of the column that will permit an increase in revolution speed and flow rate. This novel spiral separation column will allow rapid and efficient separation of mixtures with high yield of the constituent components. Published by Elsevier B.V.

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

PubMed

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

2011-08-05

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

Storage and computationally efficient permutations of factorized covariance and square-root information matrices

NASA Technical Reports Server (NTRS)

Muellerschoen, R. J.

1988-01-01

A unified method to permute vector-stored upper-triangular diagonal factorized covariance (UD) and vector stored upper-triangular square-root information filter (SRIF) arrays is presented. The method involves cyclical permutation of the rows and columns of the arrays and retriangularization with appropriate square-root-free fast Givens rotations or elementary slow Givens reflections. A minimal amount of computation is performed and only one scratch vector of size N is required, where N is the column dimension of the arrays. To make the method efficient for large SRIF arrays on a virtual memory machine, three additional scratch vectors each of size N are used to avoid expensive paging faults. The method discussed is compared with the methods and routines of Bierman's Estimation Subroutine Library (ESL).

Gas chromatographic column for the storage of sample profiles

NASA Technical Reports Server (NTRS)

Dimandja, J. M.; Valentin, J. R.; Phillips, J. B.

1994-01-01

The concept of a sample retention column that preserves the true time profile of an analyte of interest is studied. This storage system allows for the detection to be done at convenient times, as opposed to the nearly continuous monitoring that is required by other systems to preserve a sample time profile. The sample storage column is essentially a gas chromatography column, although its use is not the separation of sample components. The functions of the storage column are the selective isolation of the component of interest from the rest of the components present in the sample and the storage of this component as a function of time. Using octane as a test substance, the sample storage system was optimized with respect to such parameters as storage and readout temperature, flow rate through the storage column, column efficiency and storage time. A 3-h sample profile was collected and stored at 30 degrees C for 20 h. The profile was then retrieved, essentially intact, in 5 min at 130 degrees C.

A narrow open tubular column for high efficiency liquid chromatographic separation

DOE PAGES

Chen, Huang; Yang, Yu; Qiao, Zhenzhen; ...

2018-01-01

We report a great feature of open tubular liquid chromatography when it is run using an extremely narrow ( e.g. , 2 μm inner diameter) open tubular column: more than 10 million plates per meter can be achieved in less than 10 min and under an elution pressure of ca. 20 bar.

A narrow open tubular column for high efficiency liquid chromatographic separation

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

Chen, Huang; Yang, Yu; Qiao, Zhenzhen

We report a great feature of open tubular liquid chromatography when it is run using an extremely narrow ( e.g. , 2 μm inner diameter) open tubular column: more than 10 million plates per meter can be achieved in less than 10 min and under an elution pressure of ca. 20 bar.

Application of multiwalled carbon nanotubes and its magnetite derivative for emulsified oil removal from produced water.

PubMed

Ibrahim, Taleb H; Sabri, Muhammad A; Khamis, Mustafa I

2018-05-10

Multiwalled carbon nanotubes and their magnetite derivatives were employed as adsorbents for emulsified oil removal from produced water. The experimental parameters for maximum emulsified oil removal efficiency and effective regeneration of these adsorbents were determined. The optimum parameters in terms of adsorbent dosage, contact time, salinity, pH and temperature were 3.0 g/L, 20.0 min, 0 ppm, 7.0 and 25°C for both adsorbents. Due to their low density, multiwalledcarbon nanotubes could not be successfully employed in packed bed columns. The magnetite derivative has a larger density and hence, for the removal of emulsified oil from produced water packed bed column studies were performed utilizing multiwalled carbon magnetite nanotubes. The packed bed column efficiency and behaviour were evaluated using Thomas, Clark, Yan et al. and Bohart and Adams models. The Yan model was found to best describe the column experimental data. The adsorbents were regenerated using n-hexane and reused several times for oil removal from produced water without any significant decrease in their initial adsorption capacities.

Laboratory-scale column study for remediation of TCE-contaminated aquifers using three-section controlled-release potassium permanganate barriers.

PubMed

Yuan, Baoling; Li, Fei; Chen, Yanmei; Fu, Ming-Lai

2013-05-01

A laboratory-scale study with a sand column was designed to simulate trichloroethylene (TCE) pollution in the aquifer environment with three-section controlled-release potassium permanganate (CRP) barriers. The main objective of this study was to evaluate the feasibility of CRP barriers in remediation of TCE in aquifers in a long-term and controlled manner. CRP particles with a 1:3 molar ratio of KMnO4 to stearic acid showed the best controlled-release properties in pure water, and the theoretical release time was 138.5 days. The results of TCE removal in the test column indicated that complete removal efficiency of TCE in a sand column by three-section CRP barriers could be reached within 15 days. The molar ratio of KMnO4 to TCE in the three-section CRP barriers was 16:1, which was much lower than 82:1 as required when KMnO4 solution is used directly to achieve complete destruction of TCE. This result revealed that the efficiency of CRP for remediation of TCE was highly improved after encapsulation.

Design of Reforma 509 with High Strength Steel

NASA Astrophysics Data System (ADS)

Smith, Stuart; Whitby, William; Easton, Marc

Reforma 509 is a high-rise building located in the heart of the Central Business District of Mexico City. The building is comprised of office, hotel, residential and parking and forms part of a cluster of tall buildings in the area. If completed today, Reforma 509 would be the tallest building in Mexico, at 238m. All of the building's gravity and lateral (wind and seismic) loads are carried by an architecturally expressed perimeter frame that is formed from highly efficient Steel Reinforced Concrete (SRC) columns coupled together by steel tube perimeter bracing. This paper investigates the implications of substituting a grade 50 (fy=345 MPa) carbon steel with a higher strength micro-alloyed grade 70 (fy=480 MPa) steel in the design of Reforma 509.

Degradation of trichloroethylene by photocatalysis in an internally circulating slurry bubble column reactor.

PubMed

Jeon, Jin Hee; Kim, Sang Done; Lim, Tak Hyoung; Lee, Dong Hyun

2005-08-01

The effects of initial trichloroethylene (TCE) concentration, recirculating liquid flow rate and gas velocity on photodegradation of TCE have been determined in an internally circulating slurry bubble column reactor (0.15m-ID x 0.85 m-high). Titanium dioxide (TiO2) powder was employed as a photocatalyst and the optimum loading of TiO2 in the present system is found to be approximately 0.2 wt%. The stripping fraction of TCE by air flow increases but photodegradation fraction of TCE decreases with increasing the initial TCE concentration, recirculating liquid flow rate and gas velocity. The average removal efficiency of TCE is found to be approximately 97% in an internally circulating slurry bubble column reactor.

Optimization of SHINE Process: Design and Verification of Plant-Scale AG 1 Anion-Exchange Concentration Column and Titania Sorbent Pretreatment

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

Stepinski, Dominique C.; Abdul, Momen; Youker, Amanda J.

2016-06-01

Argonne National Laboratory has developed a Mo-recovery and -purification system for the SHINE medical technologies process, which uses a uranyl sulfate solution for the accelerator-driven production of Mo-99. The objective of this effort is to reduce the processing time for the acidification of the Mo-99 product prior to loading onto a concentration column and concentration of the Mo-99 product solution. Two methods were investigated: (1) the replacement of the titania concentration column by an anion-exchange column to decrease processing time and increase the radioiodine-decontamination efficiency and (2) pretreatment of the titania sorbent to improve its effectiveness for the Mo-recovery andmore » -concentration columns. Promising results are reported for both methods.« less

Efficient renaturation of inclusion body proteins denatured by SDS.

PubMed

He, Chuan; Ohnishi, Kouhei

2017-09-02

Inclusion bodies are often formed when the foreign protein is over expressed in Escherichia coli. Since proteins in inclusion bodies are inactive, denaturing and refolding of inclusion body proteins are necessary to obtain the active form. Instead of the conventional denaturants, urea and guanidine hydrochloride, a strong anionic detergent SDS was used to solubilize C-terminal His-tag form of ulvan lyase in the inclusion bodies. Solution containing SDS-solubilized enzyme were kept on ice to precipitate SDS, followed by SDS-KCl insoluble crystal formation to remove SDS completely. After removing the precipitate by centrifugation, the supernatant was applied to Ni-NTA column to purify His-tagged ulvan lyase. The purified protein showed a dimeric form and ulvan lyase activity, demonstrating that SDS-denatured protein was renatured and recovered enzyme activity. This simple method could be useful for refolding other inclusion body proteins. Copyright © 2017 Elsevier Inc. All rights reserved.

Removal of lead(II) by adsorption using treated granular activated carbon: batch and column studies.

PubMed

Goel, Jyotsna; Kadirvelu, Krishna; Rajagopal, Chitra; Kumar Garg, Vinod

2005-10-17

In the present study, a deeper understanding of adsorption behavior of Pb(II) from aqueous systems onto activated carbon and treated activated carbon has been attempted via static and column mode studies under various conditions. It probes mainly two adsorbents that is, activated carbon (AC) and modified activated carbon (AC-S). Characterization of both the adsorbents was one of the key focal areas of the present study. This has shown a clear change or demarcation in the various physical and chemical properties of the modified adsorbent from its precursor activated carbon. Both the adsorbents are subjected to static mode adsorption studies and then after a comparison based on isotherm analysis; more efficient adsorbent is screened for column mode adsorption studies. The lead removal increased for sample of treated carbon. The extent of Pb(II) removal was found to be higher in the treated activated carbon. The aim of carrying out the continuous-flow studies was to assess the effect of various process variables, viz., of bed height, hydraulic loading rate and initial feed concentration on breakthrough time and adsorption capacity. This has helped in ascertaining the practical applicability of the adsorbent. Breakthrough curves were plotted for the adsorption of lead on the adsorbent using continuous-flow column operation by varying different operating parameters like hydraulic loading rate (3.0-10.5 m3/(hm2)), bed height (0.3-0.5 m) and feed concentrations (2.0-6.0 mg/l). At the end, an attempt has also been made to model the data generated from column studies using the empirical relationship based on Bohart-Adams model. This model has provided an objective framework to the subjective interpretation of the adsorption system and the model constant obtained here can be used to achieve the ultimate objective of our study that is, up scaling and designing of adsorption process at the pilot plant scale level. AC-S column regeneration using 0.5 and 1.0M concentration of HNO3 has been investigated. It has shown a regeneration efficiency of 52.0% with 0.5 M HNO3.

Bacterial production in the water column of small streams highly depends on terrestrial dissolved organic carbon

NASA Astrophysics Data System (ADS)

Graeber, Daniel; Poulsen, Jane R.; Rasmussen, Jes J.; Kronvang, Brian; Zak, Dominik; Kamjunke, Norbert

2016-04-01

In the recent years it has become clear that the largest part of the terrestrial dissolved organic carbon (DOC) pool is removed on the way from the land to the ocean. Yet it is still unclear, where in the freshwater systems terrestrial DOC is actually taken up, and for streams DOC uptake was assumed to happen mostly at the stream bottom (benthic zone). However, a recent monitoring study implies that water column but not benthic bacteria are strongly affected by the amount and composition of DOM entering streams from the terrestrial zone. We conducted an experiment to compare the reaction of the bacterial production and heterotrophic uptake in the water column and the benthic zone to a standardized source of terrestrial DOC (leaf leachate from Beech litter). In detail, we sampled gravel and water from eight streams with a gradient in stream size and land use. For each stream four different treatments were incubated at 16°C for three days and each stream: filtered stream water with gravel stones (representing benthic zone bacteria) or unfiltered stream water (representing water column bacteria), both either with (n = 5) or, without (n = 3) leaf leachate. We found that the bacterial uptake of leaf litter DOC was higher for the benthic zone likely due to the higher bacterial production compared to the water column. In contrast, the bacterial production per amount of leaf leachate DOC taken up was significantly higher for the bacteria in the water column than for those in the benthic zone. This clearly indicates a higher growth efficiency with the leaf leachate DOC for the bacteria in the water column than in the benthic zone. We found a high variability for the growth efficiency in the water column, which was best explained by a negative correlation of the DOC demand with stream width (R² = 0.86, linear correlation of log-transformed data). This was not the case for the benthic zone bacteria (R² = 0.02). This implies that water column bacteria in very small streams are more dependent on terrestrial DOC sources for their growth than those in larger streams. Based on this experiment and literature data we hypothesize that: I) The response of the bacterial production to terrestrial DOC in the water column is stronger than for the benthic zone and is decreasing with increasing stream size, likely due to the increase of autochthonous DOC production within the stream. II) Independent of stream size there is only a small reaction to terrestrial DOC for the bacterial production in the benthic zone, either due to internal DOC production or a stronger dependency on particulate organic carbon. We propose that this terrestrial DOC dependency concept is generally applicable, however, its potential underlying mechanisms and concept predictions need to be tested further for other stream and river ecosystems.

In situ nitrogen removal from leachate by bioreactor landfill with limited aeration

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

Shao Liming; He Pinjing; Li Guojian

2008-07-01

The feasibility of simultaneous nitrification and denitrification in a bioreactor landfill with limited aeration was assessed. Three column reactors, simulating bioreactor landfill operations under anaerobic condition (as reference), intermittent forced aeration and enhanced natural aeration were hence established, where aerated columns passed through two phases, i.e., fresh landfill and well-decomposed landfill. The experimental results show that limited aeration decreased nitrogen loadings of leachate distinctly in the fresh landfill. In the well-decomposed landfill, the NH{sub 4}{sup +}-N of the input leachate could be nitrified completely in the aerated landfill columns. The nitrifying loadings of the column cross section reached 7.9 gmore » N/m{sup 2} d and 16.9 g N/m{sup 2} d in the simulated landfill columns of intermittent forced aeration and enhanced natural aeration, respectively. The denitrification was influenced by oxygen distribution in the landfill column. Intermittent existence of oxygen in the landfill with the intermittent forced aeration was favorable to denitrify the NO{sub 2}{sup -}-N and NO{sub 3}{sup -}-N, indicated by the high denitrification efficiency (>99%) under the condition of BOD{sub 5}/TN of more than 5.4 in leachate; locally persistent existence of oxygen in the landfill with enhanced natural aeration could limit the denitrification, indicated by relatively low denitrification efficiency of about 75% even when the BOD{sub 5}/TN in leachate had an average of 7.1.« less

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

PubMed

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

2015-07-07

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

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

PubMed

Gritti, Fabrice; Guiochon, Georges

2011-08-05

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

Long-term behavior of passively aerated compost methanotrophic biofilter columns.

PubMed

Wilshusen, J H; Hettiaratchi, J P A; Stein, V B

2004-01-01

The methane oxidation potential of several types of compost methanotrophic biofilter columns were compared in the laboratory over a period of 220 days. The results indicate an increase in methanotrophic activity over a period of about 100 days, up to a maximum of 400 g m(-2) day(-1), and a gradual decline to about 100 g m(-2) day(-1) within the next 120 days. High methane oxidation rates appear to be restricted to a small area of the column, 10-15 cm thick. Based on the laboratory investigations carried out to determine the cause for the decline in methane oxidation rate, it was concluded that the formation of exopolymeric substances (EPS), at the zones of maximum methane oxidation, was responsible for this decline. In monitoring methane oxidation in a column for up to 600 days, it was observed that mixing of the medium after formation of EPS enabled the column to temporarily recover high performance. The results suggest that stable, homogenous compost, with a low C/N and low ammonium content, mixed on a regular basis, could achieve and maintain high methane oxidation efficiencies. Copyright 2004 Elsevier Ltd.

Evaluation of a hydrophilic interaction liquid chromatography design space for sugars and sugar alcohols.

PubMed

Hetrick, Evan M; Kramer, Timothy T; Risley, Donald S

2017-03-17

Based on a column-screening exercise, a column ranking system was developed for sample mixtures containing any combination of 26 sugar and sugar alcohol analytes using 16 polar stationary phases in the HILIC mode with acetonitrile/water or acetone/water mobile phases. Each analyte was evaluated on the HILIC columns with gradient elution and the subsequent chromatography data was compiled into a statistical software package where any subset of the analytes can be selected and the columns are then ranked by the greatest separation. Since these analytes lack chromophores, aerosol-based detectors, including an evaporative light scattering detector (ELSD) and a charged aerosol detector (CAD) were employed for qualitative and quantitative detection. Example qualitative applications are provided to illustrate the practicality and efficiency of this HILIC column ranking. Furthermore, the design-space approach was used as a starting point for a quantitative method for the trace analysis of glucose in trehalose samples in a complex matrix. Knowledge gained from evaluating the design-space led to rapid development of a capable method as demonstrated through validation of the following parameters: specificity, accuracy, precision, linearity, limit of quantitation, limit of detection, and range. Copyright © 2017 Elsevier B.V. All rights reserved.

Separation of transition metals on a poly-iminodiacetic acid grafted polymeric resin column with post-column reaction detection utilising a paired emitter-detector diode system.

PubMed

Barron, Leon; O'Toole, Martina; Diamond, Dermot; Nesterenko, Pavel N; Paull, Brett

2008-12-05

The selectivity, retention and separation of transition metals on a short (2 mm x 50 mm) column packed with a poly-iminodiacetic acid functionalised polymer 10 microm resin (Dionex ProPac IMAC-10) are presented. This stationary phase, typically used for the separation of proteins, is composed of long chain poly-iminodiacetic acid groups grafted to a hydrophilic layer surrounding a 10 microm polymeric bead. Through the use of a combination of a multi-step pH and picolinic acid gradient, the separation of magnesium, iron, cobalt, cadmium, zinc, lead and copper was possible, followed by post-column reaction with 4-(2-pyridylazo) resorcinol (PAR) and absorbance detection at 510 nm using a novel and inexpensive optical detector, comprised of two light emitting diodes with one acting as a light source and the other as a detector. Column efficiency for selective transition metals was in excess of N=10,000, with the baseline separation of seven metal cations in <3 min possible under optimised conditions. Detection limits of between 5 and 81 microg/L were possible based upon a 50 microL injection volume.

Experimental studies on the physico-mechanical properties of jet-grout columns in sandy and silty soils

NASA Astrophysics Data System (ADS)

Akin, Muge K.

2016-04-01

The term of ground improvement states to the modification of the engineering properties of soils. Jet-grouting is one of the grouting methods among various ground improvement techniques. During jet-grouting, different textures of columns can be obtained depending on the characteristics of surrounding subsoil as well as the adopted jet-grouting system for each site is variable. In addition to textural properties, strength and index parameters of jet-grout columns are highly affected by the adjacent soil. In this study, the physical and mechanical properties of jet-grout columns constructed at two different sites in silty and sandy soil conditions were determined by laboratory tests. A number of statistical relationships between physical and mechanical properties of soilcrete were established in this study in order to investigate the dependency of numerous variables. The relationship between qu and γd is more reliable for sandy soilcrete than that of silty columns considering the determination coefficients. Positive linear relationships between Vp and γd with significantly high determination coefficients were obtained for the jet-grout columns in silt and sand. The regression analyses indicate that the P-wave velocity is a very dominant parameter for the estimation of physical and mechanical properties of jet-grout columns and should be involved during the quality control of soilcrete material despite the intensive use of uniaxial compressive strength test. Besides, it is concluded that the dry unit weight of jet-grout column is a good indicator of the efficiency of employed operational parameters during jet-grouting.

New Amphiphilic Composite for Preparing Efficient Coated Potassium-Fertilizers for Top-Dressing Fertilization of Annual Crops.

PubMed

Urrutia, Oscar; Erro, Javier; Zabini, Andre; Hoshiba, Kent; Blandin, Anne F; Baigorri, Roberto; Martín-Pastor, Manuel; Alis, Yves; Yvin, Jean C; García-Mina, José M

2018-05-16

This study describes the efficiency of a new coating material for preparing granulated potassium-fertilizers with a potassium release to the soil solution sensitive to rainfall intensity. The composite is prepared by reaction of an alkyd-resin with cement in the absence of water. The complementary use of diverse analytical techniques showed that the presence of the cement fraction induced alkyd resin reticulation and gradual cement-resin hardening. Scanning electron microscopy revealed the formation of micro and nanopores within cement-clusters, whose water permeability is affected by the resin reticulation and amphiphilic character. Potassium release was evaluated in water, soil-columns, and in soil-plant trials in pots and open-field. Agronomic results were consistent with potassium release rates obtained in water solution and soil columns. The composite-coated potassium fertilizer was more efficient than the noncoated one in providing plant available potassium, with this effect being dependent on water presence in soil.

A simple microfluidic platform for rapid and efficient production of the radiotracer [18F]fallypride.

PubMed

Zhang, Xin; Liu, Fei; Knapp, Karla-Anne; Nickels, Michael L; Manning, H Charles; Bellan, Leon M

2018-05-01

Herein, we report the development of a simple, high-throughput and efficient microfluidic system for synthesizing radioactive [18F]fallypride, a PET imaging radiotracer widely used in medical research. The microfluidic chip contains all essential modules required for the synthesis and purification of radioactive fallypride. The radiochemical yield of the tracer is sufficient for multiple animal injections for preclinical imaging studies. To produce the on-chip concentration and purification columns, we employ a simple "trapping" mechanism by inserting rows of square pillars with predefined gaps near the outlet of microchannel. Microspheres with appropriate functionality are suspended in solution and loaded into the microchannels to form columns for radioactivity concentration and product purification. Instead of relying on complicated flow control elements (e.g., micromechanical valves requiring complex external pneumatic actuation), external valves are utilized to control transfer of the reagents between different modules. The on-chip ion exchange column can efficiently capture [18F]fluoride with negligible loss (∼98% trapping efficiency), and subsequently release a burst of concentrated [18F]fluoride to the reaction cavity. A thin layer of PDMS with a small hole in the center facilitates rapid and reliable water evaporation (with the aid of azeotropic distillation and nitrogen flow) while reducing fluoride loss. During the solvent exchange and fluorination reaction, the entire chip is uniformly heated to the desired temperature using a hot plate. All aspects of the [18F]fallypride synthesis were monitored by high-performance liquid chromatography (HPLC) analysis, resulting in labelling efficiency in fluorination reaction ranging from 67-87% (n = 5). Moreover, after isolating unreacted [18F]fluoride, remaining fallypride precursor, and various by-products via an on-chip purification column, the eluted [18F]fallypride is radiochemically pure and of a sufficient quantity to allow for PET imaging (∼5 mCi). Finally, a positron emission tomography (PET) image of a rat brain injected with ∼300 μCi [18F]fallypride produced by our microfluidic chip is provided, demonstrating the utility of the product produced by the microfluidic reactor. With a short synthesis time (∼60 min) and a highly integrated on-chip modular configuration that allows for concentration, reaction, and product purification, our microfluidic chip offers numerous exciting advantages with the potential for applications in radiochemical research and clinical production. Moreover, due to its simplicity and potential for automation, we anticipate it may be easily integrated into a clinical environment.

Apparatus and process for the separation of hydrophobic and hydrophilic particles using microbubble column flotation together with a process and apparatus for generation of microbubbles

DOEpatents

Yoon, Roe-Hoan; Adel, Gregory T.; Luttrell, Gerald H.

1992-01-01

A method and apparatus are disclosed for the microbubble flotation separation of very fine and coarse particles, especially coal and minerals, so as to produce high purity and high recovery efficiency. This is accomplished through the use of a flotation column, microbubbles, recycling of the flotation pulp, and countercurrent wash water to gently wash the froth. Also disclosed are unique processes and apparatus for generating microbubbles for flotation in a highly efficient and inexpensive manner using either a porous tube or in-line static generators.

Apparatus for the separation of hydrophobic and hydrophilic particles using microbubble column flotation together with a process and apparatus for generation of microbubbles

DOEpatents

Yoon, Roe-Hoan; Adel, Gregory T.; Luttrell, Gerald H.

1995-01-01

An apparatus is disclosed for the microbubble flotation separation of very fine and coarse particles, especially coal, and minerals so as to produce high purity and high recovery efficiency. This is accomplished through the use of a flotation column, microbubbles, recycling of the flotation pulp, and countercurrent wash water to gently wash the froth. Also disclosed are unique processes and apparatus for generating microbubbles for flotation in a highly efficient and inexpensive manner using either a porous tube or in-line static generators.

Apparatus for the separation of hydrophobic and hydrophilic particles using microbubble column flotation together with a process and apparatus for generation of microbubbles

DOEpatents

Yoon, R.H.; Adel, G.T.; Luttrell, G.H.

1995-03-14

An apparatus is disclosed for the microbubble flotation separation of very fine and coarse particles, especially coal, and minerals so as to produce high purity and high recovery efficiency. This is accomplished through the use of a flotation column, microbubbles, recycling of the flotation pulp, and countercurrent wash water to gently wash the froth. Also disclosed are unique processes and apparatus for generating microbubbles for flotation in a highly efficient and inexpensive manner using either a porous tube or in-line static generators. 14 figs.

Apparatus and process for the separation of hydrophobic and hydrophilic particles using microbubble column flotation together with a process and apparatus for generation of microbubbles

DOEpatents

Yoon, Roe-Hoan; Adel, Gregory T.; Luttrell, Gerald H.

1998-01-01

A method and apparatus are disclosed for the microbubble flotation separation of very fine and coarse particles, especially coal and minerals, so as to produce high purity and high recovery efficiency. This is accomplished through the use of a flotation column, microbubbles, recycling of the flotation pulp, and countercurrent wash water to gently wash the froth. Also disclosed are unique processes and apparatus for generating microbubbles for flotation in a highly efficient and inexpensive manner using either a porous tube or in-line static generators.

On the Utility (or Futility) of Using Stable Water Isotopes to Constrain the Bulk Properties of Tropical Convection

NASA Astrophysics Data System (ADS)

Duan, Suqin Q.; Wright, Jonathon S.; Romps, David M.

2018-02-01

Atmospheric water-vapor isotopes have been proposed as a potentially powerful constraint on convection, which plays a critical role in Earth's present and future climate. It is shown here, however, that the mean tropical profile of HDO in the free troposphere does not usefully constrain the mean convective entrainment rate or precipitation efficiency. This is demonstrated using a single-column analytical model of atmospheric water isotopes. The model has three parameters: the entrainment rate, the precipitation efficiency, and the distance that evaporating condensates fall. At a given relative humidity, the possible range of HDO is small: its range is comparable to both the measurement uncertainty in the mean tropical profile and the structural uncertainty of a single-column model. Therefore, the mean tropical HDO profile is unlikely to add information about convective processes in a bulk-plume framework that cannot already be learned from relative humidity alone.

Simultaneous delivery time and aperture shape optimization for the volumetric-modulated arc therapy (VMAT) treatment planning problem

NASA Astrophysics Data System (ADS)

Mahnam, Mehdi; Gendreau, Michel; Lahrichi, Nadia; Rousseau, Louis-Martin

2017-07-01

In this paper, we propose a novel heuristic algorithm for the volumetric-modulated arc therapy treatment planning problem, optimizing the trade-off between delivery time and treatment quality. We present a new mixed integer programming model in which the multi-leaf collimator leaf positions, gantry speed, and dose rate are determined simultaneously. Our heuristic is based on column generation; the aperture configuration is modeled in the columns and the dose distribution and time restriction in the rows. To reduce the number of voxels and increase the efficiency of the master model, we aggregate similar voxels using a clustering technique. The efficiency of the algorithm and the treatment quality are evaluated on a benchmark clinical prostate cancer case. The computational results show that a high-quality treatment is achievable using a four-thread CPU. Finally, we analyze the effects of the various parameters and two leaf-motion strategies.

PNNL Report on the Development of Bench-scale CFD Simulations for Gas Absorption across a Wetted Wall Column

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

Wang, Chao; Xu, Zhijie; Lai, Canhai

This report is prepared for the demonstration of hierarchical prediction of carbon capture efficiency of a solvent-based absorption column. A computational fluid dynamics (CFD) model is first developed to simulate the core phenomena of solvent-based carbon capture, i.e., the CO2 physical absorption and chemical reaction, on a simplified geometry of wetted wall column (WWC) at bench scale. Aqueous solutions of ethanolamine (MEA) are commonly selected as a CO2 stream scrubbing liquid. CO2 is captured by both physical and chemical absorption using highly CO2 soluble and reactive solvent, MEA, during the scrubbing process. In order to provide confidence bound on themore » computational predictions of this complex engineering system, a hierarchical calibration and validation framework is proposed. The overall goal of this effort is to provide a mechanism-based predictive framework with confidence bound for overall mass transfer coefficient of the wetted wall column (WWC) with statistical analyses of the corresponding WWC experiments with increasing physical complexity.« less

Split Flow Online Solid-Phase Extraction Coupled with Inductively Coupled Plasma Mass Spectrometry System for One-Shot Data Acquisition of Quantification and Recovery Efficiency.

PubMed

Furukawa, Makoto; Takagai, Yoshitaka

2016-10-04

Online solid-phase extraction (SPE) coupled with inductively coupled plasma mass spectrometry (ICPMS) is a useful tool in automatic sequential analysis. However, it cannot simultaneously quantify the analytical targets and their recovery percentages (R%) in one-shot samples. We propose a system that simultaneously acquires both data in a single sample injection. The main flowline of the online solid-phase extraction is divided into main and split flows. The split flow line (i.e., bypass line), which circumvents the SPE column, was placed on the main flow line. Under program-controlled switching of the automatic valve, the ICPMS sequentially measures the targets in a sample before and after column preconcentration and determines the target concentrations and the R% on the SPE column. This paper describes the system development and two demonstrations to exhibit the analytical significance, i.e., the ultratrace amounts of radioactive strontium ( 90 Sr) using commercial Sr-trap resin and multielement adsorbability on the SPE column. This system is applicable to other flow analyses and detectors in online solid phase extraction.

Evaluation of the removal of Strontium-90 from groundwater using a zeolite rich-rock permeable treatment wall

NASA Astrophysics Data System (ADS)

Seneca, S. M.; Rabideau, A. J.; Bandilla, K.

2010-12-01

Experimental and modeling studies are in progress to evaluate the long-term performance of a permeable treatment wall comprised of zeolite-rich rock for the removal of strontium-90 from groundwater. Multiple column tests were performed at the University at Buffalo and on-site West Valley Environmental Services; columns were supplied with synthetic groundwater referenced to anticipate field conditions and radioactive groundwater on-site WVES. The primary focus in this work is on quantifying the competitive ion exchange among five cations (Na+, K+, Ca2+, Mg2+, and Sr2+); the data obtained from the column studies is used to support the robust estimation of zeolite cation exchange parameters. This research will produce a five-solute cation exchange model describing the removal efficiency of the zeolite, using the various column tests to calibrate and validate the geochemical transport model. The field-scale transport model provides flexibility to explore design parameters and potential variations in groundwater geochemistry to investigate the long-term performance of a full scale treatment wall at the Western New York nuclear facility.

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

PubMed

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

2015-10-16

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

Study of Pulsed Columns with the System. Uranyl Nitrate-Nitric Acid-Water- Tributylphosphate; ETUDE DES COLONNES A PULSATIONS A L'AIDE DU SYSTEME NITRATE D'URANYLE-ACIDE NITRIQUEEAU-TRIBUTYLPHOSPHATE

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

Durandet, J.; Defives, D.; Choffe, B.

1959-10-31

The performsnce of a pulsed column with perforated plates was studied with the aid of a uranyl nitrate-nitric acid --water --tributyl phosphate system. The extraction of uranium from an aqueous acidic solution by an organic solvent and the extraction of uranium from organic solutions by water were the two cases investigated. The variation of the efficiency and the capacity of the pulsed column was determined as a function of the pulse amplitude and frequency, of the total flow rate, of the diameter of the holes, and of the choice of dispersed phase. The results showed that for a given amplitudemore » and total flow rate the efficiency has a maximum with an increase in frequency. (J.S.R.)« less

Advantages of core-shell particle columns in Sequential Injection Chromatography for determination of phenolic acids.

PubMed

Chocholouš, Petr; Vacková, Jana; Srámková, Ivana; Satínský, Dalibor; Solich, Petr

2013-01-15

Currently, for Sequential Injection Chromatography (SIC), only reversed phase C18 columns have been used for chromatographic separations. This article presents the first use of three different stationary phases: three core-shell particle-packed reversed phase columns in flow systems. The aim of this work was to extend the chromatographic capabilities of the SIC system. Despite the particle-packed columns reaching system pressures of ≤ 610 PSI, their conditions matched those of a commercially produced and optimised SIC system (SIChrom™ (FIAlab(®), USA)) with a 8-port high-pressure selection valve and medium-pressure Sapphire™ syringe pump with a 4 mL reservoir and maximum system pressure of ≤ 1000 PSI. The selectivity of each of the tested columns, Ascentis(®) Express RP-Amide, Ascentis(®) Express Phenyl-Hexyl and Ascentis(®) Express C18 (30 mm × 4.6mm, core-shell particle size 2.7 μm), was compared by their ability to separate seven phenolic acids that are secondary metabolite substances widely distributed in plants. The separations of all of the components were performed by isocratic elution using binary mobile phases composed of acetonitrile and 0.065% phosphoric acid at pH 2.4 (a specific ratio was used for each column) at a flow-rate of 0.60 mL/min. The volume of the mobile phase was 3.8 mL for each separation. The injection volume of the sample was 10 μL for each separation. The UV detection wavelengths were set to 250, 280 and 325 nm. The RP-Amide column provided the highest chromatographic resolution and allowed for complete baseline separation of protocatechuic, syringic, vanillic, ferulic, sinapinic, p-coumaric and o-coumaric acids. The Phenyl-Hexyl and C18 columns were unable to completely separate the tested mixture, syringic and vanillic acid and ferulic and sinapinic acids could not be separated from one another. The analytical parameters were a LOD of 0.3 mg L(-1), a LOQ of 1.0 mg L(-1), a calibration range of 1.0-50.0 (100.0) mg L(-1) (r>0.997) and a system precision of 10 mg L(-1) with a RSD ≤ 1.65%. The high performance of the chromatography process with the RP-Amide column under optimised conditions was highlighted and well documented (HETP values ≤ 10 μm, peak symmetry ≤ 1.33, resolution ≥ 1.87 and time for one analysis <8.0 min). The results of these experiments confirmed the benefits of extending chromatographic selectivity using core-shell particle column technology in a SIC manifold. Copyright © 2012 Elsevier B.V. All rights reserved.

The Order-Restricted Association Model: Two Estimation Algorithms and Issues in Testing

ERIC Educational Resources Information Center

Galindo-Garre, Francisca; Vermunt, Jeroen K.

2004-01-01

This paper presents a row-column (RC) association model in which the estimated row and column scores are forced to be in agreement with a priori specified ordering. Two efficient algorithms for finding the order-restricted maximum likelihood (ML) estimates are proposed and their reliability under different degrees of association is investigated by…

Clean-up of a pesticide-lanolin mixture by gel permeation chromatography.

PubMed

López-Mesas, M; Crespi, M; Brach, J; Mullender, J P

2000-12-01

In this study, the efficiency of a clean-up method by gel permeation chromatography (GPC) for the separation of pesticides from lanolin is analyzed. The pesticides analyzed belong to two different families, organophosphorous and synthetic pyrethroids. Lanolin, a standard mixture of the pesticides, and a lanolin-pesticides mixture are injected in a GPC column. The recoveries and elution times from the GPC column of lanolin (by a gravimetric method) and pesticides (by gas chromatography-electron capture detector) are determined. From this column, a good separation of the lanolin-pesticides mixture is observed.

Low exchange element for nuclear reactor

DOEpatents

Brogli, Rudolf H.; Shamasunder, Bangalore I.; Seth, Shivaji S.

1985-01-01

A flow exchange element is presented which lowers temperature gradients in fuel elements and reduces maximum local temperature within high temperature gas-cooled reactors. The flow exchange element is inserted within a column of fuel elements where it serves to redirect coolant flow. Coolant which has been flowing in a hotter region of the column is redirected to a cooler region, and coolant which has been flowing in the cooler region of the column is redirected to the hotter region. The safety, efficiency, and longevity of the high temperature gas-cooled reactor is thereby enhanced.

ASTP Technical Air-To-Ground Voice Transcription

NASA Technical Reports Server (NTRS)

1975-01-01

The transcription of the technical air-to-ground voice communication of the Apollo-Soyuz Test Project mission was presented. The transcript was divided into three columns giving, respectively, the time, speaker, and text. All times are expressed in Greenwich mean time for the appropriate Julian dates. The speaker column indicates the source of transmission; the text column contains the verbatim transcript of the communications. Special symbols were used to report garbling, pauses or self-interruptions, interruptions by other speakers or abrupt terminations, emphasized words, obliterations, and material translated from Russian.

Preparation of catechin extracts and nanoemulsions from green tea leaf waste and their inhibition effect on prostate cancer cell PC-3

PubMed Central

Tsai, Yin-Jieh; Chen, Bing-Huei

2016-01-01

Green tea is one of the most commonly consumed natural health beverages in Taiwan’s market, with the major functional component catechin being shown to possess several biological activities such as antioxidation, anticancer, and prevention of cardiovascular disease. The objectives of this study were to develop a high-performance liquid chromatography–mass spectrometry method to determine the variety and content of catechins in green tea leaf waste, a by-product obtained during processing of tea beverage. In addition, catechin nanoemulsion was prepared to study its inhibition effect on prostate cancer cell PC-3. Results showed that a total of eight catechin standards were separated within 25 minutes by using a Gemini C18 column and a gradient mobile phase of 0.1% formic acid (A) and acetonitrile (B) with flow rate at 1 mL/min, column temperature at 30°C, and detection wavelength at 280 nm. Among various extraction solvents, 50% ethanol generated the highest yield of total catechins from tea leaf waste, of which five catechins were identified and quantified. The catechin nanoemulsion was composed of catechin extract, lecithin, Tween 80, and deionized water in an appropriate proportion, with the mean particle size being 11.45 nm, encapsulation efficiency 88.1%, and zeta potential −66.3 mV. A high stability of catechin nanoemulsion was shown over a storage period of 120 days at 4°C. Both catechin extract and nanoemulsion could inhibit growth of PC-3 tumor cells, with the half maximal inhibitory concentration being 15.4 μg/mL and 8.5 μg/mL, respectively. The PC-3 cell cycle was arrested at S phase through elevation of P27 expression and decline of cyclin A, cyclin B, cyclin-dependent kinase 2, and cyclin-dependent kinase 1 expression. In addition, both catechin extract and nanoemulsion could induce apoptosis of PC-3 cells through decrease in B-cell lymphoma 2 (bcl-2) expression and increase in cytochrome c expression for activation of caspase-3, caspase-8, and caspase-9. Taken together, both caspase-dependent and caspase-independent pathways may be involved in apoptosis of PC-3 cells. PMID:27226712

Organic matter processing by microbial communities throughout the Atlantic water column as revealed by metaproteomics.

PubMed

Bergauer, Kristin; Fernandez-Guerra, Antonio; Garcia, Juan A L; Sprenger, Richard R; Stepanauskas, Ramunas; Pachiadaki, Maria G; Jensen, Ole N; Herndl, Gerhard J

2018-01-16

The phylogenetic composition of the heterotrophic microbial community is depth stratified in the oceanic water column down to abyssopelagic layers. In the layers below the euphotic zone, it has been suggested that heterotrophic microbes rely largely on solubilized particulate organic matter as a carbon and energy source rather than on dissolved organic matter. To decipher whether changes in the phylogenetic composition with depth are reflected in changes in the bacterial and archaeal transporter proteins, we generated an extensive metaproteomic and metagenomic dataset of microbial communities collected from 100- to 5,000-m depth in the Atlantic Ocean. By identifying which compounds of the organic matter pool are absorbed, transported, and incorporated into microbial cells, intriguing insights into organic matter transformation in the deep ocean emerged. On average, solute transporters accounted for 23% of identified protein sequences in the lower euphotic and ∼39% in the bathypelagic layer, indicating the central role of heterotrophy in the dark ocean. In the bathypelagic layer, substrate affinities of expressed transporters suggest that, in addition to amino acids, peptides and carbohydrates, carboxylic acids and compatible solutes may be essential substrates for the microbial community. Key players with highest expression of solute transporters were Alphaproteobacteria, Gammaproteobacteria, and Deltaproteobacteria, accounting for 40%, 11%, and 10%, respectively, of relative protein abundances. The in situ expression of solute transporters indicates that the heterotrophic prokaryotic community is geared toward the utilization of similar organic compounds throughout the water column, with yet higher abundances of transporters targeting aromatic compounds in the bathypelagic realm. Copyright © 2018 the Author(s). Published by PNAS.

Organic matter processing by microbial communities throughout the Atlantic water column as revealed by metaproteomics

PubMed Central

Bergauer, Kristin; Fernandez-Guerra, Antonio; Garcia, Juan A. L.; Sprenger, Richard R.; Stepanauskas, Ramunas; Pachiadaki, Maria G.; Herndl, Gerhard J.

2018-01-01

The phylogenetic composition of the heterotrophic microbial community is depth stratified in the oceanic water column down to abyssopelagic layers. In the layers below the euphotic zone, it has been suggested that heterotrophic microbes rely largely on solubilized particulate organic matter as a carbon and energy source rather than on dissolved organic matter. To decipher whether changes in the phylogenetic composition with depth are reflected in changes in the bacterial and archaeal transporter proteins, we generated an extensive metaproteomic and metagenomic dataset of microbial communities collected from 100- to 5,000-m depth in the Atlantic Ocean. By identifying which compounds of the organic matter pool are absorbed, transported, and incorporated into microbial cells, intriguing insights into organic matter transformation in the deep ocean emerged. On average, solute transporters accounted for 23% of identified protein sequences in the lower euphotic and ∼39% in the bathypelagic layer, indicating the central role of heterotrophy in the dark ocean. In the bathypelagic layer, substrate affinities of expressed transporters suggest that, in addition to amino acids, peptides and carbohydrates, carboxylic acids and compatible solutes may be essential substrates for the microbial community. Key players with highest expression of solute transporters were Alphaproteobacteria, Gammaproteobacteria, and Deltaproteobacteria, accounting for 40%, 11%, and 10%, respectively, of relative protein abundances. The in situ expression of solute transporters indicates that the heterotrophic prokaryotic community is geared toward the utilization of similar organic compounds throughout the water column, with yet higher abundances of transporters targeting aromatic compounds in the bathypelagic realm. PMID:29255014

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

PubMed

Can, Nafiz O

2011-08-01

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

Nano-amylose-2,3-bis(3,5-dimethylphenylcarbamate)-silica hybrid sol immobilized on open tubular capillary column for capillary electrochromatography enantioseparation.

PubMed

Sun, Yaming; Wu, Qi; Shi, Xiaofeng; Gao, Jie; Dong, Shuqing; Zhao, Liang

2018-04-01

The chiral organic-inorganic hybrid materials can exhibit a high loading, and the chiral selector nanoparticles can create efficient stationary phases for open-tubular capillary electrochromatography (OT-CEC). Hence, a novel protocol for the preparation of an OT column coated with nano-amylose-2,3-bis(3,5-dimethylphenylcarbamate) (nano-ABDMPC)-silica hybrid sol through in situ layer-by-layer self-assembly method was developed for CEC enantioseparation. By controlling the assembly cycle number of nano-ABDMPC-silica hybrid sol, a homogeneous, dense and stable coating was successfully prepared, which was confirmed by SEM and elemental analysis. As the main parameter influencing the chiral separating effect, the nano-ABDMPC bearing 3-(triethoxysilyl)propyl residues concentration was investigated. The experimental results showed that 10.0 mg/mL nano-ABDMPC bearing 3-(triethoxysilyl)propyl residues coated OT capillary column possessed chiral recognition ability toward the six enantiomers (phenylalanine, tyrosine, tryptophan, phenethyl alcohol, 1-phenyl-2-propanol, and Tröger's base) at some of the different conditions tested. Additionally, the coated OT column revealed adequate repeatability concerning run-to-run, day-to-day and column-to-column. These results demonstrated the promising applicability of nano-ABDMPC-silica hybrid sol coated OT column in CEC enantioseparations. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Impact of the column hardware volume on resolution in very high pressure liquid chromatography non-invasive investigations.

PubMed

Gritti, Fabrice; McDonald, Thomas; Gilar, Martin

2015-11-13

The impact of the column hardware volume (≃ 1.7 μL) on the optimum reduced plate heights of a series of short 2.1 mm × 50 mm columns (hold-up volume ≃ 80-90 μL) packed with 1.8 μm HSS-T3, 1.7 μm BEH-C18, 1.7 μm CSH-C18, 1.6 μm CORTECS-C18+, and 1.7 μm BEH-C4 particles was investigated. A rapid and non-invasive method based on the reduction of the system dispersion (to only 0.15 μL(2)) of an I-class Acquity system and on the corrected plate heights (for system dispersion) of five weakly retained n-alkanophenones in RPLC was proposed. Evidence for sample dispersion through the column hardware volume was also revealed from the experimental plot of the peak capacities for smooth linear gradients versus the corrected efficiency of a weakly retained alkanophenone (isocratic runs). The plot is built for a constant gradient steepness irrespective of the applied flow rates (0.01-0.30 mL/min) and column lengths (2, 3, 5, and 10 cm). The volume variance caused by column endfittings and frits was estimated in between 0.1 and 0.7 μL(2) depending on the applied flow rate. After correction for system and hardware dispersion, the minimum reduced plate heights of short (5 cm) and narrow-bore (2.1mm i.d.) beds packed with sub-2 μm fully and superficially porous particles were found close to 1.5 and 0.7, respectively, instead of the classical h values of 2.0 and 1.4 for the whole column assembly. Copyright © 2015 Elsevier B.V. All rights reserved.

Expression and purification of lacticin Q by small ubiquitin-related modifier fusion in Escherichia coli.

PubMed

Ma, Qingshan; Yu, Zhanqiao; Han, Bing; Wang, Qing; Zhang, Rijun

2012-04-01

Lacticin Q is a broad-spectrum class II bacteriocin with potential as an alternative to conventional antibiotics. The objective of this study was to produce recombinant lacticin Q using a small ubiquitin-related modifier (SUMO) fusion protein expression system. The 168-bp lacticin Q gene was cloned into the expression vector pET SUMO and transformed into Escherichia coli BL21(DE3). The soluble fusion protein was recovered with a Ni-NTA Sepharose column (95% purity); 130 mg protein was obtained per liter of fermentation culture. The SUMO tag was then proteolytically cleaved from the protein, which was re-applied to the column. Finally, about 32 mg lacticin Q (≥96% purity) was obtained. The recombinant protein exhibited antimicrobial properties similar to that of the native protein, demonstrating that lacticin Q had been successfully expressed by the SUMO fusion system.

Optimal performance of single-column chromatography and simulated moving bed processes for the separation of optical isomers

NASA Astrophysics Data System (ADS)

Medi, Bijan; Kazi, Monzure-Khoda; Amanullah, Mohammad

2013-06-01

Chromatography has been established as the method of choice for the separation and purification of optically pure drugs which has a market size of about 250 billion USD. Single column chromatography (SCC) is commonly used in the development and testing phase of drug development while multi-column Simulated Moving Bed (SMB) chromatography is more suitable for large scale production due to its continuous nature. In this study, optimal performance of SCC and SMB processes for the separation of optical isomers under linear and overloaded separation conditions has been investigated. The performance indicators, namely productivity and desorbent requirement have been compared under geometric similarity for the separation of a mixture of guaifenesin, and Tröger's base enantiomers. SCC process has been analyzed under equilibrium assumption i.e., assuming infinite column efficiency, and zero dispersion, and its optimal performance parameters are compared with the optimal prediction of an SMB process by triangle theory. Simulation results obtained using actual experimental data indicate that SCC may compete with SMB in terms of productivity depending on the molecules to be separated. Besides, insights into the process performances in terms of degree of freedom and relationship between the optimal operating point and solubility limit of the optical isomers have been ascertained. This investigation enables appropriate selection of single or multi-column chromatographic processes based on column packing properties and isotherm parameters.

Repeatability of gradient ultrahigh pressure liquid chromatography-tandem mass spectrometry methods in instrument-controlled thermal environments.

PubMed

Grinias, James P; Wong, Jenny-Marie T; Kennedy, Robert T

2016-08-26

The impact of viscous friction on eluent temperature and column efficiency in liquid chromatography is of renewed interest as the need for pressures exceeding 1000bar to use with columns packed with sub-2μm particles has grown. One way the development of axial and radial temperature gradients that arise due to viscous friction can be affected is by the thermal environment the column is placed in. In this study, a new column oven integrated into an ultrahigh pressure liquid chromatograph that enables both still-air and forced-air operating modes is investigated to find the magnitude of the effect of the axial thermal gradient that forms in 2.1×100mm columns packed with sub-2μm particles in these modes. Temperature increases of nearly 30K were observed when the generated power of the column exceeded 25W/m. The impact of the heating due to viscous friction on the repeatability of peak capacity, elution time, and peak area ratio to an internal standard for a gradient UHPLC-MS/MS method to analyze neurotransmitters was found to be limited. This result indicates that high speed UHPLC-MS/MS gradient methods under conditions of high viscous friction may be possible without the negative effects typically observed with isocratic separations under similar conditions. Copyright © 2016 Elsevier B.V. All rights reserved.

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

PubMed

Ott, Sonja; Niessner, Reinhard; Seidel, Michael

2011-08-01

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

Calcium Isotope Analysis with "Peak Cut" Method on Column Chemistry

NASA Astrophysics Data System (ADS)

Zhu, H.; Zhang, Z.; Liu, F.; Li, X.

2017-12-01

To eliminate isobaric interferences from elemental and molecular isobars (e.g., 40K+, 48Ti+, 88Sr2+, 24Mg16O+, 27Al16O+) on Ca isotopes during mass determination, samples should be purified through ion-exchange column chemistry before analysis. However, large Ca isotopic fractionation has been observed during column chemistry (Russell and Papanastassiou, 1978; Zhu et al., 2016). Therefore, full recovery during column chemistry is greatly needed, otherwise uncertainties would be caused by poor recovery (Zhu et al., 2016). Generally, matrix effects could be enhanced by full recovery, as other elements might overlap with Ca cut during column chemistry. Matrix effects and full recovery are difficult to balance and both need to be considered for high-precision analysis of stable Ca isotopes. Here, we investigate the influence of poor recovery on δ44/40Ca using TIMS with the double spike technique. The δ44/40Ca values of IAPSO seawater, ML3B-G and BHVO-2 in different Ca subcats (e.g., 0-20, 20-40, 40-60, 60-80, 80-100%) with 20% Ca recovery on column chemistry display limited variation after correction by the 42Ca-43Ca double spike technique with the exponential law. Notably, δ44/40Ca of each Ca subcut is quite consistent with δ44/40Ca of Ca cut with full recovery within error. Our results indicate that the 42Ca-43Ca double spike technique can simultaneously correct both of the Ca isotopic fractionation that occurred during column chemistry and thermal ionization mass spectrometry (TIMS) determination properly, because both of the isotopic fractionation occurred during analysis follow the exponential law well. Therefore, we propose the "peak cut" method on Ca column chemistry for samples with complex matrix effects. Briefly, for samples with low Ca contents, we can add the double spike before column chemistry, and only collect the middle of the Ca eluate and abandon the both sides of Ca eluate that might overlap with other elements (e.g., K, Sr). This method would eliminate matrix effects and improve efficiency for the column chemistry.

High temperature normal phase liquid chromatography of aromatic hydrocarbons on bare zirconia.

PubMed

Paproski, Richard E; Liang, Chen; Lucy, Charles A

2011-11-04

The normal phase HPLC behavior of a bare zirconia column was studied at temperatures up to 200 °C using a hexane mobile phase. The use of elevated column temperatures significantly decreased the retention of twenty five aromatic model compounds according to the van't Hoff equation (>30-fold decrease for some compounds). Large improvements in peak shape, efficiency (>2.2-fold), aromatic group-type selectivity, and column re-equilibration times (>5-fold) were obtained at elevated temperatures. The thermal decomposition of two polar nitrogen compounds (indole and carbazole) was observed in a hexane/dichloromethane mobile phase at temperatures greater than 100 °C. The first order decomposition of carbazole was studied in further detail. Copyright © 2011 Elsevier B.V. All rights reserved.

Microchannel cross load array with dense parallel input

DOEpatents

Swierkowski, Stefan P.

2004-04-06

An architecture or layout for microchannel arrays using T or Cross (+) loading for electrophoresis or other injection and separation chemistry that are performed in microfluidic configurations. This architecture enables a very dense layout of arrays of functionally identical shaped channels and it also solves the problem of simultaneously enabling efficient parallel shapes and biasing of the input wells, waste wells, and bias wells at the input end of the separation columns. One T load architecture uses circular holes with common rows, but not columns, which allows the flow paths for each channel to be identical in shape, using multiple mirror image pieces. Another T load architecture enables the access hole array to be formed on a biaxial, collinear grid suitable for EDM micromachining (square holes), with common rows and columns.

Ammonium fluoride as a mobile phase additive in aqueous normal phase chromatography.

PubMed

Pesek, Joseph J; Matyska, Maria T

2015-07-03

The use of ammonium fluoride as a mobile phase additive in aqueous normal phase chromatography with silica hydride-based stationary phases and mass spectrometry detection is evaluated. Retention times, peak shape, efficiency and peak intensity are compared to the more standard additives formic acid and ammonium formate. The test solutes were NAD, 3-hydroxyglutaric acid, α-ketoglutaric acid, p-aminohippuric acid, AMP, ATP, aconitic acid, threonine, N-acetyl carnitine, and 3-methyladipic acid. The column parameters are assessed in both the positive and negative ion detection modes. Ammonium fluoride is potentially an aggressive mobile phase additive that could have detrimental effects on column lifetime. Column reproducibility is measured and the effects of switching between different additives are also tested. Copyright © 2015 Elsevier B.V. All rights reserved.

[Recent advances and applications of capillary electrochromatography and pressurized capillary electrochromatography].

PubMed

Wu, Yi; Zhang, Xiaohui; Wei, Juan; Xue, Yunyun; Bahatibieke, Marjan; Wang, Yan; Yan, Chao

2009-09-01

Capillary electrochromatography (CEC), in which electroosmotic flow (EOF) created from the electrical double layer is made to act as a pump to drive the mobile phase in a capillary column packed with micro-particulates or coated with stationary phase. Both neutral and charged species can be resolved by CEC. It has been demonstrated that the efficiency of a separation obtained by electroosmotic propulsion is superior to that obtained by pressure-driven flow (as is the case in HPLC). CEC combines the best features of CE and versatile selectivity and large sample capacity of HPLC, promising high efficiency, high resolution, high selectivity and high peak capacity. However, in practice, when CEC is used without pressure, often used on a commercial CE instrument, there are problems and difficulties associated with bubbles formation and column dry-out. These difficulties can be overcome by a pressurized CEC (pCEC) system, in which a supplementary pressure is applied to the column in addition to the EOF. In such a system, a pressure can be applied to the capillary column to suppress bubbles formation. Quantitative sample introduction in pCEC can be easily achieved through a rotary-type injector. Most importantly, it is amenable for a solvent gradient mode, similar to that in HPLC, by programming the composition of mobile phase. The article brings a comprehensive survey of recent development of CEC and pCEC, including the development of instrumentation, capillary columns and stationary phase as well as CEC and pCEC applications in life science, biotechnology, pharmaceutical analysis, food safety and environmental security. Prospects for CEC and pCEC development and application are also discussed.

Comparison of Total RNA Isolation Methods for Analysis of Immune-Related microRNAs in Market Milks

PubMed Central

2015-01-01

Bovine milk provides essential nutrients, including immunologically important molecules, as the primary source of nutrition to newborns. Recent studies showed that RNAs from bovine milk contain immune-related microRNAs (miRNA) that regulate various immune systems. To evaluate the biological and immunological activity of miRNAs from milk products, isolation methods need to be established. Six methods for extracting total RNAs from bovine colostrums were adopted to evaluate the isolating efficiency and expression of miRNAs. Total RNA from milk was presented in formulation of small RNAs, rather than ribosomal RNAs. Column-combined phenol isolating methods showed high recovery of total RNAs, especially the commercial columns for biofluid samples, which demonstrated outstanding efficiency for recovering miRNAs. We also evaluated the quantity of five immune-related miRNAs (miR-93, miR-106a, miR-155, miR-181a, miR-451) in milk processed by temperature treatments including low temperature for long time (LTLT, 63℃ for 30 min)-, high temperature for short time (HTST, 75℃ for 15 s)-, and ultra heat treatment (UHT, 120-130℃ for 0.5-4 s). All targeted miRNAs had significantly reduced levels in processed milks compared to colostrum and raw mature milk. Interestingly, the amount of immune-related miRNAs from HTST milk was more resistant than those of LTLT and UHT milks. Our present study examined defined methods of RNA isolation and quantification of immune-specific miRNAs from small volumes of milk for use in further analysis. PMID:26761866

Comparison of Total RNA Isolation Methods for Analysis of Immune-Related microRNAs in Market Milks.

PubMed

Oh, Sangnam; Park, Mi Ri; Son, Seok Jun; Kim, Younghoon

2015-01-01

Bovine milk provides essential nutrients, including immunologically important molecules, as the primary source of nutrition to newborns. Recent studies showed that RNAs from bovine milk contain immune-related microRNAs (miRNA) that regulate various immune systems. To evaluate the biological and immunological activity of miRNAs from milk products, isolation methods need to be established. Six methods for extracting total RNAs from bovine colostrums were adopted to evaluate the isolating efficiency and expression of miRNAs. Total RNA from milk was presented in formulation of small RNAs, rather than ribosomal RNAs. Column-combined phenol isolating methods showed high recovery of total RNAs, especially the commercial columns for biofluid samples, which demonstrated outstanding efficiency for recovering miRNAs. We also evaluated the quantity of five immune-related miRNAs (miR-93, miR-106a, miR-155, miR-181a, miR-451) in milk processed by temperature treatments including low temperature for long time (LTLT, 63℃ for 30 min)-, high temperature for short time (HTST, 75℃ for 15 s)-, and ultra heat treatment (UHT, 120-130℃ for 0.5-4 s). All targeted miRNAs had significantly reduced levels in processed milks compared to colostrum and raw mature milk. Interestingly, the amount of immune-related miRNAs from HTST milk was more resistant than those of LTLT and UHT milks. Our present study examined defined methods of RNA isolation and quantification of immune-specific miRNAs from small volumes of milk for use in further analysis.

The Neurological Compromised Spine Due to Ewing Sarcoma. What First: Surgery or Chemotherapy? Therapy, Survival, and Neurological Outcome of 15 Cases With Primary Ewing Sarcoma of the Vertebral Column.

PubMed

Mirzaei, Lida; Kaal, Suzanne E J; Schreuder, Hendrik W B; Bartels, Ronald H M A

2015-11-01

The vertebral column is an infrequent site of primary involvement in Ewing sarcoma. Yet when Ewing sarcoma is found in the spine, the urge for decompression is high because of the often symptomatic compression of neural structures. It is unclear in alleviating a neurological deficit whether chemotherapy is preferred over decompressive laminectomy. To underline, in this case series, the efficiency of initial chemotherapy before upfront surgery in the setting of high-grade spinal cord or cauda equina compression of primary Ewing sarcoma. Fifteen patients with Ewing sarcoma primarily located in the spine were treated at our institution between 1983 and 2015. Localization, neurological deficit expressed as Frankel grade, and outcome expressed as Rankin scale before and after initial chemotherapy, the recurrence rate, and overall survival were evaluated. The multidisciplinary approach of 1 case will be discussed in detail. Nine patients (60%) were female. The age at presentation was 15.0 ± 5.5 years (range: 0.9-22.8 years). Ten patients (67%) were initially treated with chemotherapy, and 1 patient (7%) was treated primarily with radiotherapy followed by chemotherapy. The remaining 4 patients (27%) were initially treated with decompressive surgery. All patients treated primarily nonsurgically improved neurologically at follow-up, showing the importance of chemotherapy as an effective initial treatment option. Adequate and quick decompression of neural structures with similar results can be achieved by chemotherapy and radiotherapy, avoiding the local spill of malignant cells.

Targeting Human Serum Fucome by an Integrated Liquid-phase Multi Column Platform Operating in “Cascade” to Facilitate Comparative Mass Spectrometric Analysis of Disease-Free and Breast Cancer Sera

PubMed Central

Selvaraju, Subhashini; Rassi, Ziad El

2013-01-01

A fully integrated platform was developed for capturing/fractionating human fucome from disease-free and breast cancer sera. It comprised multicolumn operated by HPLC pumps and switching valves for the simultaneous depletion of high abundance proteins via affinity-based subtraction and the capturing of fucosylated glycoproteins via lectin affinity chromatography followed by the fractionation of the captured glycoproteins by reversed phase chromatography (RPC). Two lectin columns specific to fucose, namely Aleuria aurantia lectin (AAL) and Lotus tetragonolobus agglutinin (LTA) were utilized. The platform allowed the “cascading” of the serum sample from column-to-column in the liquid phase with no sample manipulation between the various steps. This guaranteed no sample loss and no propagation of experimental biases between the various columns. Finally, the fucome was fractionated by RPC yielding desalted fractions in volatile acetonitrile-rich mobile phase, which after vacuum evaporation were subjected to trypsinolysis for LC-MS/MS analysis. This permitted the identification of the differentially expressed proteins (DEP) in breast cancer serum yielding a broad panel of 35 DEP from the combined LTA and AAL captured proteins and a narrower panel of 8 DEP that were commonly differentially expressed in both LTA and AAL fractions, which are considered as more representative of cancer altered fucome. PMID:23533108

Guar gum coupled microscale ZVI for in situ treatment of CAHs: continuous-flow column study.

PubMed

Velimirovic, Milica; Simons, Queenie; Bastiaens, Leen

2014-01-30

A column study was performed under in situ conditions to evaluate to which extend the inactivation of the microscale zerovalent iron (mZVI) by guar gum occurs under continuous flow conditions. Five aquifer containing columns were set up under different conditions. Efficient removal of trichloroethene was observed for the column amended by mZVI. Stabilization of the mZVI with guar gum led to slightly reduced activity. More reduced reactivity was observed in the poisoned column containing guar gum stabilized mZVI. This confirms that soil microorganisms can degrade guar gum and that subsequent removal of the oligosaccharides by the groundwater flow (flushing effect) can reactivate the mZVI. After more than six months of continuous operation the columns were dismantled. DNA-based qPCR analysis revealed that mZVI does not significantly affect the bacterial community, while guar gum stabilized mZVI particles can even induce bacterial growth. Overall, this study suggests that the temporarily decreased mZVI reactivity due to guar gum, has a rather limited impact on the performance of in situ reactive zones. The presence of guar gum slightly reduced the reactivity of iron, but also slowed down the iron corrosion rate which prolongs the life time of reactive zone. Copyright © 2013 Elsevier B.V. All rights reserved.

Tunnel frit: a nonmetallic in-capillary frit for nanoflow ultra high-performance liquid chromatography-mass spectrometryapplications.

PubMed

Chen, Chao-Jung; Chen, Wei-Yun; Tseng, Mei-Chun; Chen, Yet-Ran

2012-01-03

In this study, an easy method to fabricate a durable in-capillary frit was developed for use in nanoflow liquid chromatography (nanoLC). A small orifice was tunneled into the sol-gel frit during the polymerization process resulting in the simple fabrication of a tunnel frit. A short packing tunnel frit column (2 cm, C(18) particles) was able to sustain over 10,000 psi continuous liquid flow for 10 days without observation of particle loss, and back pressure variation was less than 5%. The tunnel frit was successfully applied to the fabrication of nanoflow ultra high-performance liquid chromatography (nano-UHPLC) trap and analytical columns. In the analysis of tryptic peptides, the tunnel frit trap and analytical columns were demonstrated to have high separation efficiency and sensitivity. In analysis of phosphopeptides, the use of the nonmetallic tunnel frit column showed better sensitivity than the metallic frit column. This design can facilitate the preparation of nano-HPLC and nano-UHPLC columns and the packing material can easily be refilled when the column is severely contaminated or clogged. © 2011 American Chemical Society

Tuning a Parallel Segmented Flow Column and Enabling Multiplexed Detection.

PubMed

Pravadali-Cekic, Sercan; Kocic, Danijela; Hua, Stanley; Jones, Andrew; Dennis, Gary R; Shalliker, R Andrew

2015-12-15

Active flow technology (AFT) is new form of column technology that was designed to overcome flow heterogeneity to increase separation performance in terms of efficiency and sensitivity and to enable multiplexed detection. This form of AFT uses a parallel segmented flow (PSF) column. A PSF column outlet end-fitting consists of 2 or 4 ports, which can be multiplexed to connect up to 4 detectors. The PSF column not only allows a platform for multiplexed detection but also the combination of both destructive and non-destructive detectors, without additional dead volume tubing, simultaneously. The amount of flow through each port can also be adjusted through pressure management to suit the requirements of a specific detector(s). To achieve multiplexed detection using a PSF column there are a number of parameters which can be controlled to ensure optimal separation performance and quality of results; that is tube dimensions for each port, choice of port for each type of detector and flow adjustment. This protocol is intended to show how to use and tune a PSF column functioning in a multiplexed mode of detection.

Low-density solvent based ultrasound-assisted emulsification microextraction and on-column derivatization combined with gas chromatography-mass spectrometry for the determination of carbamate pesticides in environmental water samples.

PubMed

Guo, Liang; Lee, Hian Kee

2012-04-27

A fast and efficient method for the determination of trace level of carbamate pesticides using a lower-density-than-water solvent for ultrasound-assisted emulsification microextraction coupled to on-column derivatization and analysis by GC-MS has been developed and studied. In this approach, a soft plastic Pasteur pipette was employed as a convenient extraction device. Fifty microliters of extraction solvent, of lower density than water, was injected into the sample solution held in the pipette. The latter was immediately immersed in an ultrasound water bath to form an emulsion. After 2 min extraction, the emulsion was fractionated into two layers by centrifugation. The upper layer (organic extract) could be collected conveniently by squeezing the bulb of the pipette, now held upside down, to move it into the narrow stem of the device, facilitating its retrieval for analysis. The extract was then combined with trimethylphenylammonium hydroxide and directly injected into a gas chromatography-mass spectrometry (GC-MS) system for on-column derivatization and analysis. The on-column derivatization provided an added convenience (since a separate step was not necessary). Parameters affecting the derivatization and extraction were investigated. Under the most favorable conditions, the method demonstrated high extraction efficiency with low limits of detection of between 0.01 and 0.1 μg/L, good linearity in the range of 0.05-50 μg/L, to 0.5-100 μg/L, and good repeatability (RSD below 9.2%, n=5). The proposed method was evaluated by determining carbamate pesticides in river water samples. Copyright © 2012 Elsevier B.V. All rights reserved.

Aerated biofilters with multiple-level air injection configurations to enhance biological treatment of methane emissions.

PubMed

Farrokhzadeh, Hasti; Hettiaratchi, J Patrick A; Jayasinghe, Poornima; Kumar, Sunil

2017-09-01

Aiming to improve conventional methane biofilter performance, a multiple-level aeration biofilter design is proposed. Laboratory flow-through column experiments were conducted to evaluate three actively-aerated methane biofilter configurations. Columns were aerated at one, two, and three levels of the bed depth, with air introduced at flow rates calculated from methane oxidation reaction stoichiometry. Inlet methane loading rates were increased in five stages between 6 and 18mL/min. The effects of methane feeding rate, levels of aeration, and residence time on methane oxidation rates were determined. Samples collected after completion of flow-through experiments were used to determine methane oxidation kinetic parameters, V max , K m , and methanotrophic community distribution across biofilter columns. Results obtained from mixed variances analysis and response surfaces, as well as methanotrophic activity data, suggested that, biofilter column with two aeration levels has the most even performance over time, maintaining 85.1% average oxidation efficiency over 95days of experiments. Copyright © 2017 Elsevier Ltd. All rights reserved.

Graphene oxide/chitin nanofibril composite foams as column adsorbents for aqueous pollutants.

PubMed

Ma, Zhongshi; Liu, Dagang; Zhu, Yi; Li, Zehui; Li, Zhenxuan; Tian, Huafeng; Liu, Haiqing

2016-06-25

A novel graphene oxide/chitin nanofibrils (GO-CNF) composite foam as a column adsorbent was prepared for aqueous contaminant disposal. The structures, morphologies and properties of composite foams supported by nanofibrils were characterized. As a special case, the adsorption of methylene blue (MB) on GO-CNF was investigated regarding the static adsorption and column adsorption-desorption tests. Results from equilibrium adsorption isotherms indicated that the adsorption behavior was well-fitted to Langmuir model. The composite foams reinforced by CNF were dimensionally stable during the column adsorption process and could be reused after elution. The removal efficiency of MB was still nearly 90% after 3 cycles. Furthermore, other inorganic or organic pollutants adsorbed by composite foams were also explored. Therefore, this novel composite foam with remarkable properties such as dimensional stability, universal adsorbent for cationic pollutants, high adsorption capacity, and ease of regeneration was a desirable adsorbent in the future practical application of water pollutant treatment. Copyright © 2016 Elsevier Ltd. All rights reserved.

Recent trends in ultra-fast HPLC: new generation superficially porous silica columns.

PubMed

Ali, Imran; Al-Othman, Zeid A; Nagae, Norikaju; Gaitonde, Vinay D; Dutta, Kamlesh K

2012-12-01

New generation columns, i.e. packed with superficially porous silica particles are available as trade names with following manufacturers: Halo, Ascentis Express, Proshell 120, Kinetex, Accucore, Sunshell, and Nucleoshell. These provide ultra-fast HPLC separations for a variety of compounds with moderate sample loading capacity and low back pressure. Chemistries of these columns are C(8), C(18), RP-Amide, hydrophilic interaction liquid chromatography, penta fluorophenyl (PFP), F5, and RP-aqua. Normally, the silica gel particles are of 2.7 and 1.7 μm as total and inner solid core diameters, respectively, with 0.5-μm-thick of outer porous layer having 90 Å pore sizes and 150 m(2)/g surface area. This article describes these new generation columns with special emphasis on their textures and chemistries, separations, optimization, and comparison (inter and intra stationary phases). Besides, future perspectives have also been discussed. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Effects of Cabin Upsets on Adsorption Columns for Air Revitalization

NASA Technical Reports Server (NTRS)

LeVan, Douglas

1999-01-01

The National Aeronautics and Space Administration (NASA) utilizes adsorption technology as part of contaminant removal systems designed for long term missions. A variety of trace contaminants can be effectively removed from gas streams by adsorption onto activated carbon. An activated carbon adsorption column meets NASA's requirements of a lightweight and efficient means of controlling trace contaminant levels aboard spacecraft and space stations. The activated carbon bed is part of the Trace Contaminant Control System (TCCS) which is utilized to purify the cabin atmosphere. TCCS designs oversize the adsorption columns to account for irregular fluctuations in cabin atmospheric conditions. Variations in the cabin atmosphere include changes in contaminant concentrations, temperature, and relative humidity. Excessively large deviations from typical conditions can result from unusual crew activity, equipment malfunctions, or even fires. The research carried out under this award focussed in detail on the effects of cabin upsets on the performance of activated carbon adsorption columns. Both experiments and modeling were performed with an emphasis on the roll of a change in relative humidity on adsorption of trace contaminants. A flow through fixed-bed apparatus was constructed at the NASA Ames Research Center, and experiments were performed there. Modeling work was performed at the University of Virginia.

Mobility of multiwalled carbon nanotubes in porous media.

PubMed

Liu, Xueying; O'Carroll, Denis M; Petersen, Elijah J; Huang, Qingguo; Anderson, C Lindsay

2009-11-01

Engineered multiwalled carbon nanotubes (MWCNTs) are the subject of intense research and are expected to gain widespread usage in a broad variety of commercial products. However, concerns have been raised regarding potential environmental and human health risks. The mobility of MWCNTs in porous media is examined in this study using one-dimensional flow-through column experiments under conditions representative of subsurface and drinking water treatment systems. Results demonstrate that pore water velocity strongly influenced MWCNT transport, with high MWCNT mobility at pore water velocities greater than 4.0 m/d. A numerical simulator, which incorporated a newly developed theoretical collector efficiency relationship for MWCNTs in spherical porous media, was developed to model observed column results. The model, which incorporated traditional colloid filtration theory in conjunction with a site-blocking term, yielded good agreement with observed results in quartz sand-packed column experiments. Experiments were also conducted in glass bead-packed columns with the same mean grain size as the quartz sand-packed columns. MWCNTs were more mobile in the glass bead-packed columns.

Methacrylate-bonded covalent-organic framework monolithic columns for high performance liquid chromatography.

PubMed

Liu, Li-Hua; Yang, Cheng-Xiong; Yan, Xiu-Ping

2017-01-06

Covalent-organic frameworks (COFs) are a newfangled class of intriguing microporous materials. Considering their unique properties, COFs should be promising as packing materials for high performance liquid chromatography (HPLC). However, the irregular shape and sub-micrometer size of COFs synthesized via the traditional methods render the main obstacles for the application of COFs in HPLC. Herein, we report the preparation of methacrylate-bonded COF monolithic columns for HPLC to overcome the above obstacles. The prepared COF bonded monolithic columns not only show good homogeneity and permeability, but also give high column efficiency, good resolution and precision for HPLC separation of small molecules including polycyclic aromatic hydrocarbons, phenols, anilines, nonsteroidal anti-inflammatory drugs and benzothiophenes. Compared with the bare polymer monolithic column, the COF bonded monolithic columns show enhanced hydrophobic, π-π and hydrogen bond interactions in reverse phase HPLC. The results reveal the great potential of COF bonded monoliths for HPLC and COFs in separation sciences. Copyright © 2016 Elsevier B.V. All rights reserved.

High-pressure liquid chromatography with direct injection of gas sample.

PubMed

Astanin, Anton I; Baram, Grigory I

2017-06-09

The conventional method of using liquid chromatography to determine the composition of a gaseous mixture entails dissolving vapors in a suitable solvent, then obtaining a chromatograph of the resulting solution. We studied the direct introduction of a gaseous sample into a C18 reversed-phase column, followed by separation of the components by HPLC with UV detection. Since the chromatography was performed at high pressure, vapors readily dissolved in the eluent and the substances separated in the column as effectively as in liquid samples. Samples were injected into the column in two ways: a) through the valve without a flow stop; b) after stopping the flow and relieving all pressure. We showed that an injectable gas volume could reach 70% of column dead volume. When an injected gaseous sample volume was less than 10% of the column dead volume, the resulting peaks were symmetrical and the column efficiency was high. Copyright © 2017 Elsevier B.V. All rights reserved.

Use of emulsified vegetable oil to support bioremediation of TCE DNAPL in soil columns.

PubMed

Harkness, Mark; Fisher, Angela

2013-08-01

The interaction between emulsified vegetable oil (EVO) and trichloroethylene (TCE) dense non-aqueous phase liquid (DNAPL) was observed using two soil columns and subsequent reductive dechlorination of TCE was monitored over a three year period. Dyed TCE DNAPL (~75 g) was emplaced in one column (DNAPL column), while the second was DNAPL-free (plume column). EVO was added to both columns and partitioning of the EVO into the TCE DNAPL was measured and quantified. TCE (1.9 mM) was added to the influent of the plume column to simulate conditions down gradient of a DNAPL source area and the columns were operated independently for more than one year, after which they were connected in series. Initially limited dechlorination of TCE to cDCE was observed in the DNAPL column, while the plume column supported complete reductive dechlorination of TCE to ethene. Upon connection and reamendment of the plume column with EVO, near saturation levels of TCE from the effluent of the DNAPL column were rapidly dechlorinated to c-DCE and VC in the plume column; however, this high rate dechlorination produced hydrochloric acid which overwhelmed the buffering capacity of the system and caused the pH to drop below 6.0. Dechlorination efficiency in the columns subsequently deteriorated, as measured by the chloride production and Dehalococcoides counts, but was restored by adding sodium bicarbonate buffer to the influent groundwater. Robust dechlorination was eventually observed in the DNAPL column, such that the TCE DNAPL was largely removed by the end of the study. Partitioning of the EVO into the DNAPL provided significant operational benefits to the remediation system both in terms of electron donor placement and longevity. Copyright © 2013 Elsevier B.V. All rights reserved.

Development of an achiral supercritical fluid chromatography method with ultraviolet absorbance and mass spectrometric detection for impurity profiling of drug candidates. Part II. Selection of an orthogonal set of stationary phases.

PubMed

Lemasson, Elise; Bertin, Sophie; Hennig, Philippe; Boiteux, Hélène; Lesellier, Eric; West, Caroline

2015-08-21

Impurity profiling of organic products that are synthesized as possible drug candidates requires complementary analytical methods to ensure that all impurities are identified. Supercritical fluid chromatography (SFC) is a very useful tool to achieve this objective, as an adequate selection of stationary phases can provide orthogonal separations so as to maximize the chances to see all impurities. In this series of papers, we have developed a method for achiral SFC-MS profiling of drug candidates, based on a selection of 160 analytes issued from Servier Research Laboratories. In the first part of this study, focusing on mobile phase selection, a gradient elution with carbon dioxide and methanol comprising 2% water and 20mM ammonium acetate proved to be the best in terms of chromatographic performance, while also providing good MS response [1]. The objective of this second part was the selection of an orthogonal set of ultra-high performance stationary phases, that was carried out in two steps. Firstly, a reduced set of analytes (20) was used to screen 23 columns. The columns selected were all 1.7-2.5μm fully porous or 2.6-2.7μm superficially porous particles, with a variety of stationary phase chemistries. Derringer desirability functions were used to rank the columns according to retention window, column efficiency evaluated with peak width of selected analytes, and the proportion of analytes successfully eluted with good peak shapes. The columns providing the worst performances were thus eliminated and a shorter selection of columns (11) was obtained. Secondly, based on 160 tested analytes, the 11 columns were ranked again. The retention data obtained on these columns were then compared to define a reduced set of the best columns providing the greatest orthogonality, to maximize the chances to see all impurities within a limited number of runs. Two high-performance columns were thus selected: ACQUITY UPC(2) HSS C18 SB and Nucleoshell HILIC. Copyright © 2015 Elsevier B.V. All rights reserved.

Industrial application of green chromatography--I. Separation and analysis of niacinamide in skincare creams using pure water as the mobile phase.

PubMed

Yang, Yu; Strickland, Zackary; Kapalavavi, Brahmam; Marple, Ronita; Gamsky, Chris

2011-03-15

In this work, chromatographic separation of niacin and niacinamide using pure water as the sole component in the mobile phase has been investigated. The separation and analysis of niacinamide have been optimized using three columns at different temperatures and various flow rates. Our results clearly demonstrate that separation and analysis of niacinamide from skincare products can be achieved using pure water as the eluent at 60°C on a Waters XTerra MS C18 column, a Waters XBridge C18 column, or at 80°C on a Hamilton PRP-1 column. The separation efficiency, quantification quality, and analysis time of this new method are at least comparable with those of the traditional HPLC methods. Compared with traditional HPLC, the major advantage of this newly developed green chromatography technique is the elimination of organic solvents required in the HPLC mobile phase. In addition, the pure water chromatography separations described in this work can be directly applied in industrial plant settings without further modification of the existing HPLC equipment. Copyright © 2011 Elsevier B.V. All rights reserved.

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

PubMed

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

2016-08-19

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

Axial thermal gradients in microchip gas chromatography.

PubMed

Wang, Anzi; Hynynen, Sampo; Hawkins, Aaron R; Tolley, Samuel E; Tolley, H Dennis; Lee, Milton L

2014-12-29

Fabrication technologies for microelectromechanical systems (MEMS) allow miniaturization of conventional benchtop gas chromatography (GC) to portable, palm-sized microfabricated GC (μGC) devices, which are suitable for on-site chemical analysis and remote sensing. The separation performance of μGC systems, however, has not been on par with conventional GC. Column efficiency, peak symmetry and resolution are often compromised by column defects and non-ideal injections. The relatively low performance of μGC devices has impeded their further commercialization and broader application. In this work, the separation performance of μGC columns was improved by incorporating thermal gradient gas chromatography (TGGC). The analysis time was ∼20% shorter for TGGC separations compared to conventional temperature-programmed GC (TPGC) when a wide sample band was introduced into the column. Up to 50% reduction in peak tailing was observed for polar analytes, which improved their resolution. The signal-to-noise ratios (S/N) of late-eluting peaks were increased by 3-4 fold. The unique focusing effect of TGGC overcomes many of the previous shortcomings inherent in μGC analyses. Copyright © 2014 Elsevier B.V. All rights reserved.

Cellular Targets of Dietary Polyphenol Resveratrol

DTIC Science & Technology

2005-03-01

attempts to generate affinity columns tagged with other polyphenols, e.g., epigallocatechin gallate ( EGCG ). Conceivably such columns, if generated, would...Similar affinity chromatography with the related polyphenol Epigallocatechin gallate does not produce similar results.” Answer: We did not make...addition, the PI does not provid expression. If there is “increased ex many bind the resveratrol affinity co related polyphenol Epigallocatechin Response

Magnetic nanoparticles enhance adenovirus transduction in vitro and in vivo.

PubMed

Sapet, Cédric; Pellegrino, Christophe; Laurent, Nicolas; Sicard, Flavie; Zelphati, Olivier

2012-05-01

Adenoviruses are among the most powerful gene delivery systems. Even if they present low potential for oncogenesis, there is still a need for minimizing widespread delivery to avoid deleterious reactions. In this study, we investigated Magnetofection efficiency to concentrate and guide vectors for an improved targeted delivery. Magnetic nanoparticles formulations were complexed to a replication defective Adenovirus and were used to transduce cells both in vitro and in vivo. A new integrated magnetic procedure for cell sorting and genetic modification (i-MICST) was also investigated. Magnetic nanoparticles enhanced viral transduction efficiency and protein expression in a dose-dependent manner. They accelerated the transduction kinetics and allowed non-permissive cells infection. Magnetofection greatly improved adenovirus-mediated DNA delivery in vivo and provided a magnetic targeting. The i-MICST results established the efficiency of magnetic nanoparticles assisted viral transduction within cell sorting columns. The results showed that the combination of Magnetofection and Adenoviruses represents a promising strategy for gene therapy. Recently, a new integrated method to combine clinically approved magnetic cell isolation devices and genetic modification was developed. In this study, we validated that magnetic cell separation and adenoviral transduction can be accomplished in one reliable integrated and safe system.

Characterisation of RPLC columns packed with porous sub-2 microm particles.

PubMed

Petersson, Patrik; Euerby, Melvin R

2007-08-01

Eight commercially available sub-2 microm octadecyl silane columns (C18 columns) have been characterised by the Tanaka protocol. The columns can be grouped into two groups that display large differences in selectivity and peak shape due to differences in hydrophobicity, degree of surface coverage and silanol activity. Measurements of particle size distributions were made using automated microscopy and electrical sensing zone measurements. Only a weak correlation could be found between efficiency and particle size. Large differences in column backpressure were observed. These differences are not related to particle size distribution. A more likely explanation is differences in packing density. In order to take full advantage of 100-150 mm columns packed with sub-2 microm particles, it is often necessary to employ not only an elevated pressure but also an elevated temperature. A comparison between columns packed with sub-2, 3 and 5 microm versions of the same packing indicates potential method transferability problems for several of the columns due to selectivity differences. Currently, the best alternative for fast high-resolution LC is the use of sub-2 microm particles in combination with elevated pressure and temperature. However, as shown in this study additional efforts are needed to improve transferability as well as column performance.

A fully automated and fast method using direct sample injection combined with fused-core column on-line SPE-HPLC for determination of ochratoxin A and citrinin in lager beers.

PubMed

Lhotská, Ivona; Šatínský, Dalibor; Havlíková, Lucie; Solich, Petr

2016-05-01

A new fast and sensitive method based on on-line solid-phase extraction on a fused-core precolumn coupled to liquid chromatography with fluorescence detection has been developed for ochratoxin A (OTA) and citrinin (CIT) determination in lager beer samples. Direct injection of 100 μL filtered beer samples into an on-line SPE-HPLC system enabled fast and effective sample extraction including separation in less than 6 min. Preconcentration of OTA and CIT from beer samples was performed on an Ascentis Express RP C18 guard column (5 × 4.6 mm), particle size 2.7 μm, with a mobile phase of methanol/0.5% aqueous acetic acid pH 2.8 (30:70, v/v) at a flow rate of 2.0 mL min(-1). The flow switch from extraction column to analytical column in back-flush mode was set at 2.0 min and the separation was performed on the fused-core column Ascentis Express Phenyl-Hexyl (100 × 4.6 mm), particle size 2.7 μm, with a mobile phase acetonitrile/0.5% aqueous acetic acid pH 2.8 in a gradient elution at a flow rate of 1.0 mL min(-1) and temperature of 50 °C. Fluorescence excitation/emission detection wavelengths were set at 335/497 nm. The accuracy of the method, defined as the mean recoveries of OTA and CIT from light and dark beer samples, was in the range 98.3-102.1%. The method showed high sensitivity owing to on-line preconcentration; LOQ values were found to be 10 and 20 ng L(-1) for OTA and CIT, respectively. The found values of OTA and CIT in all tested light, dark and wheat beer samples were significantly below the maximum tolerable limits (3.0 μg kg(-1) for OTA and 2000 μg kg(-1) for CIT) set by the European Union.

Prevention and suppression of metal packing fires.

PubMed

Roberts, Mark; Rogers, William J; Sam Mannan, M; Ostrowski, Scott W

2003-11-14

Structured packing has been widely used because of large surface area that makes possible columns with high capacity and efficiency. The large surface area also contributes to fire hazards because of hydrocarbon deposits that can easily combust and promote combustion of the thin metal packing materials. Materials of high surface area that can fuel fires include reactive metals, such as titanium, and materials that are not considered combustible, such as stainless steel. Column design and material selection for packing construction is discussed together with employee training and practices for safe column maintenance and operations. Presented also are methods and agents for suppression of metal fires. Guidance for prevention and suppression of metal fires is related to incidents involving packing fires in columns.

A practicable process for phenol removal with liquid surfactant membrane permeation column

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

Kataoka, Takeshi; Osaki, Katsuhiko; Nishiki, Tadaaki

1997-05-01

A practicable liquid surfactant membrane process for phenol removal is proposed with a stirred countercurrent column used as the liquid membrane contact equipment. The constituents of liquid membranes, such as internal aqueous phase and surfactant, the type of column, and the operating conditions for efficient and continuous performance of the liquid surfactant membrane process, have been examined. When NaOH solution was used as the internal aqueous phase and ECA4360J was used as the surfactant, the W/O emulsion was stable for the duration of column operation. More than 97% phenol could be removed from the feed solution. Nearly complete demulsification wasmore » also achieved by gentle agitation with an electrostatic demulsifier.« less

Apparatus and process for the separation of hydrophobic and hydrophilic particles using microbubble column flotation together with a process and apparatus for generation of microbubbles

DOEpatents

Yoon, R.H.; Adel, G.T.; Luttrell, G.H.

1992-12-01

A method and apparatus are disclosed for the microbubble flotation separation of very fine and coarse particles, especially coal and minerals, so as to produce high purity and high recovery efficiency. This is accomplished through the use of a flotation column, microbubbles, recycling of the flotation pulp, and countercurrent wash water to gently wash the froth. Also disclosed are unique processes and apparatus for generating microbubbles for flotation in a highly efficient and inexpensive manner using either a porous tube or in-line static generators. 14 figs.

Apparatus and process for the separation of hydrophobic and hydrophilic particles using microbubble column flotation together with a process and apparatus for generation of microbubbles

DOEpatents

Yoon, R.H.; Adel, G.T.; Luttrell, G.H.

1998-09-29

A method and apparatus are disclosed for the microbubble flotation separation of very fine and coarse particles, especially coal and minerals, so as to produce high purity and high recovery efficiency. This is accomplished through the use of a flotation column, microbubbles, recycling of the flotation pulp, and countercurrent wash water to gently wash the froth. Also disclosed are unique processes and apparatus for generating microbubbles for flotation in a highly efficient and inexpensive manner using either a porous tube or in-line static generators. 14 figs.

Column Number Density Expressions Through M = 0 and M = 1 Point Source Plumes Along Any Straight Path

NASA Technical Reports Server (NTRS)

Woronowicz, Michael

2016-01-01

Analytical expressions for column number density (CND) are developed for optical line of sight paths through a variety of steady free molecule point source models including directionally-constrained effusion (Mach number M = 0) and flow from a sonic orifice (M = 1). Sonic orifice solutions are approximate, developed using a fair simulacrum fitted to the free molecule solution. Expressions are also developed for a spherically-symmetric thermal expansion (M = 0). CND solutions are found for the most general paths relative to these sources and briefly explored. It is determined that the maximum CND from a distant location through directed effusion and sonic orifice cases occurs along the path parallel to the source plane that intersects the plume axis. For the effusive case this value is exactly twice the CND found along the ray originating from that point of intersection and extending to infinity along the plume's axis. For sonic plumes this ratio is reduced to about 4/3. For high Mach number cases the maximum CND will be found along the axial centerline path. Keywords: column number density, plume flows, outgassing, free molecule flow.

Hydrodynamic chromatography of polystyrene microparticles in micropillar array columns.

PubMed

Op de Beeck, Jeff; De Malsche, Wim; Vangelooven, Joris; Gardeniers, Han; Desmet, Gert

2010-09-24

We report on the possibility to perform HDC in micropillar array columns and the potential advantages of such a system. The HDC performance of a pillar array column with pillar diameter = 5 microm and an interpillar distance of 2.5 microm has been characterized using both a low MW tracer (FITC) and differently sized polystyrene bead samples (100, 200 and 500 nm). The reduced plate height curves that were obtained for the different investigated markers all overlapped very well, and attained a minimum value of about h(min)=0.3 (reduction based on the pillar diameter), corresponding to 1.6 microm in absolute value and giving good prospects for high efficiency separations. The obtained reduced retention time values were in fair agreement with that predicted by the Di Marzio and Guttman model for a flow between flat plates, using the minimal interpillar distance as characteristic interplate distance. Copyright 2010 Elsevier B.V. All rights reserved.

OTEC gas desorption studies

NASA Astrophysics Data System (ADS)

Chen, F. C.; Golshani, A.

1982-02-01

Experiments on deaeration in packed columns and barometric intake systems, and with hydraulic air compression for open-cycle OTEC systems are reported. A gas desorption test loop consisting of water storage tanks, a vacuum system, a liquid recirculating system, an air supply, a column test section, and two barometric leg test sections was used to perform the tests. The aerated water was directed through columns filled with either ceramic Raschig rings or plastic pall rings, and the system vacuum pressure, which drives the deaeration process, was found to be dependent on water velocity and intake pipe height. The addition of a barometric intake pipe increased the deaeration effect 10%, and further tests were run with lengths of PVC pipe as potential means for noncondensibles disposal through hydraulic air compression. Using the kinetic energy from the effluent flow to condense steam in the noncondensible stream improved the system efficiency.

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

PubMed

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

2014-11-07

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

Microwave assisted solvent extraction and coupled-column reversed-phase liquid chromatography with UV detection use of an analytical restricted-access-medium column for the efficient multi-residue analysis of acidic pesticides in soils.

PubMed

Hogendoom, E A; Huls, R; Dijkman, E; Hoogerbrugge, R

2001-12-14

A screening method has been developed for the determination of acidic pesticides in various types of soils. Methodology is based on the use of microwave assisted solvent extraction (MASE) for fast and efficient extraction of the analytes from the soils and coupled-column reversed-phase liquid chromatography (LC-LC) with UV detection at 228 nm for the instrumental analysis of uncleaned extracts. Four types of soils, including sand, clay and peat, with a range in organic matter content of 0.3-13% and ten acidic pesticides of different chemical families (bentazone, bromoxynil, metsulfuron-methyl, 2,4-D, MCPA, MCPP, 2,4-DP, 2,4,5-T, 2,4-DB and MCPB) were selected as matrices and analytes, respectively. The method developed included the selection of suitable MASE and LC-LC conditions. The latter consisted of the selection of a 5-microm GFF-II internal surface reversed-phase (ISRP, Pinkerton) analytical column (50 x 4.6 mm, I.D.) as the first column in the RAM-C18 configuration in combination with an optimised linear gradient elution including on-line cleanup of sample extracts and reconditioning of the columns. The method was validated with the analysis of freshly spiked samples and samples with aged residues (120 days). The four types of soils were spiked with the ten acidic pesticides at levels between 20 and 200 microg/kg. Weighted regression of the recovery data showed for most analyte-matrix combinations, including freshly spiked samples and aged residues, that the method provides overall recoveries between 60 and 90% with relative standard deviations of the intra-laboratory reproducibility's between 5 and 25%; LODs were obtained between 5 and 50 microg/kg. Evaluation of the data set with principal component analysis revealed that the parameters (i) increase of organic matter content of the soil samples and (ii) aged residues negatively effect the recovery of the analytes.

Effects of Low-Molecular-Weight Organic Acids on the Dissolution of Hydroxyapatite Nanoparticles in Batch and Column Experiments: A Perspective from Phosphate Oxygen Isotope Fractionation

NASA Astrophysics Data System (ADS)

Wang, D.; Jaisi, D. P.; Jin, Y.

2015-12-01

Hydroxyapatite nanoparticles (HANPs) are increasingly being advocated as an efficient and environment-friendly "green" phosphorus nanofertilizer attributed to their nanoscale dimension, large reactive surface area, and low leaching potential. However, knowledge of how naturally occurring low-molecular-weight organic acids (LMWOAs) that are secreted by plant roots mediate the dissolution of HANPs (releasing PO43- ion for plant growth) is nonexistent. Here three most commonly encountered LMWOAs (acetic acid, oxalic acid, and citric acid) at environmentally relevant concentration (1 mM) were evaluated for their effects on HANPs' dissolution in static batch and dynamic column systems. Particularly, phosphate oxygen isotope fractionation of HANPs during dissolution was examined to disentangle mechanisms controlling the evolution of O-isotopic composition of dissolved PO43- ion. Our results reveal that in batch experiments the dissolution of HANPs was fast but the overall dissolution efficiency of HANPs was limited (≤30%). In contrast, ~100% HANPs were dissolved in columns where LMWOAs were continuously injected. The limited dissolution of HANPs in static batch systems was due primarily to pH buffer effect (pH increased sharply when LMWOA was added in HANPs suspension), whereas in dynamic column systems the HANPs were continuously dissolved by low pH LMWOAs and leached away. Regardless of LMWOA type and experimental system, the isotopically light phosphate (P16O4) was preferentially released during dissolution and the O-isotopic composition of dissolved PO43- ion increased gradually with increasing dissolution due to equilibrium isotope effect between dissolved PO43- ion and HANPs. However, the overall magnitude of O-isotopic fractionation of dissolved PO43- ion was less in batch than in column systems, due to less mass transfer between dissolved PO43- ions and HANPs in batch relative to column experiments. Our findings provide new insights into bioavailability, transformation, and evolution of O-isotopic signatures of phosphate-based nanoparticles in agricultural soils particularly in the rhizosphere where such LMWOAs are ubiquitous.

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

PubMed

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

2016-06-01

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

At-line hyphenation of high-speed countercurrent chromatography with Sephadex LH-20 column chromatography for bioassay-guided separation of antioxidants from vine tea (Ampelopsis grossedentata).

PubMed

Ma, Ruyi; Zhou, Rongrong; Tong, Runna; Shi, Shuyun; Chen, Xiaoqing

2017-01-01

Vine tea (Ampelopsis grossedentata), a widely used healthy tea, beverage and herbal medicine, exhibited strong antioxidant activity. However, systematic purification of antioxidants, especially for those with similar structures or polarities, is a challenging work. Here, we present a novel at-line hyphenation of high-speed countercurrent chromatography with Sephadex LH-20 column chromatography (HSCCC-Sephadex LH-20 CC) for rapid and efficient separation of antioxidants from vine tea target-guided by 1,1-diphenyl-2-picryl-hydrazyl radical-high performance liquid chromatography (DPPH-HPLC) experiment. A makeup pump, a six-port switching valve and a trapping column were served as interface. The configuration had no operational time and mobile phase limitations between two dimensional chromatography and showed great flexibility without tedious sample-handling procedure. Seven targeted antioxidants were firstly separated by stepwise HSCCC using petroleum ether-ethyl acetate-methanol-water (4:9:4:9, v/v/v/v) and (4:9:5:8, v/v/v/v) as solvent systems, and then co-eluted antioxidants were on-line trapped, concentrated and desorbed to Sephadex LH-20 column for further off-line purification by methanol. It is noted that six elucidated antioxidants with purity over 95% exhibited stronger activity than ascorbic acid (VC). More importantly, this at-line hyphenated strategy could sever as a rapid and efficient pathway for systematic purification of bioactive components from complex matrix. Copyright © 2016 Elsevier B.V. All rights reserved.

Microbial biofilms for the removal of Cu²⁺ from CMP wastewater.

PubMed

Mosier, Aaron P; Behnke, Jason; Jin, Eileen T; Cady, Nathaniel C

2015-09-01

The modern semiconductor industry relies heavily on a process known as chemical mechanical planarization, which uses physical and chemical processes to remove excess material from the surface of silicon wafers during microchip fabrication. This process results in large volumes of wastewater containing dissolved metals including copper (Cu(2+)), which must then be filtered and treated before release into municipal waste systems. We have investigated the potential use of bacterial and fungal biomass as an alternative to the currently used ion-exchange resins for the adsorption of dissolved Cu(2+) from high-throughput industrial waste streams. A library of candidate microorganisms, including Lactobacillus casei and Pichia pastoris, was screened for ability to bind Cu(2+) from solution and to form static biofilm communities within packed-bed adsorption columns. The binding efficiency of these biomass-based adsorption columns was assessed under various flow conditions and compared to that of industrially used ion-exchange resins. We demonstrated the potential to regenerate the biomass within the adsorption columns through the use of a hydrochloric acid wash, and subsequently reuse the columns for additional copper binding. While the binding efficiency and capacity of the developed L. casei/P. pastoris biomass filters was inferior to ion-exchange resin, the potential for repeated reuse of these filters, coupled with the advantages of a more sustainable "green" adsorption process, make this technique an attractive candidate for use in industrial-scale CMP wastewater treatment. Copyright © 2015 Elsevier Ltd. All rights reserved.

Stochastic Accumulation by Cortical Columns May Explain the Scalar Property of Multistable Perception

NASA Astrophysics Data System (ADS)

Cao, Robin; Braun, Jochen; Mattia, Maurizio

2014-08-01

The timing of certain mental events is thought to reflect random walks performed by underlying neural dynamics. One class of such events—stochastic reversals of multistable perceptions—exhibits a unique scalar property: even though timing densities vary widely, higher moments stay in particular proportions to the mean. We show that stochastic accumulation of activity in a finite number of idealized cortical columns—realizing a generalized Ehrenfest urn model—may explain these observations. Modeling stochastic reversals as the first-passage time of a threshold number of active columns, we obtain higher moments of the first-passage time density. We derive analytical expressions for noninteracting columns and generalize the results to interacting columns in simulations. The scalar property of multistable perception is reproduced by a dynamic regime with a fixed, low threshold, in which the activation of a few additional columns suffices for a reversal.

Rapid determination of parabens in seafood sauces by high-performance liquid chromatography: A practical comparison of core-shell particles and sub-2 μm fully porous particles.

PubMed

Ye, Jing; Cao, Xiaoji; Cheng, Zhuo; Qin, Ye; Lu, Yanbin

2015-12-01

In this work, the chromatographic performance of superficially porous particles (Halo core-shell C18 column, 50 mm × 2.1 mm, 2.7 μm) was compared with that of sub-2 μm fully porous particles (Acquity BEH C18 , 50 mm × 2.1 mm, 1.7 μm). Four parabens, methylparaben, ethylparaben, propylparaben, and butylparaben, were used as representative compounds for calculating the plate heights in a wide flow rate range and analyzed on the basis of the Van Deemter and Knox equations. Theoretical Poppe plots were constructed for each column to compare their kinetic performance. Both phases gave similar minimum plate heights when using nonreduced coordinates. Meanwhile, the flat C-term of the core-shell column provided the possibilities for applying high flow rates without significant loss in efficiency. The low backpressure of core-shell particles allowed this kind of column, especially compatible with conventional high-performance liquid chromatography systems. Based on these factors, a simple high-performance liquid chromatography method was established and validated for the determination of parabens in various seafood sauces using the Halo core-shell C18 column for separation. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Further Examination of Biogeochemical Consequences of Mesoscale Eddies in the Sargasso Sea

NASA Astrophysics Data System (ADS)

Marquez, I. A., Jr.; Krause, J. W.; Lomas, M. W.

2016-02-01

The Bermuda Atlantic Time Series (BATS) is an ongoing 25-year biogeochemical record in the North Atlantic subtropical gyre. Contemporaneous data on the particulate phases of four major bioreactive elements, C, N, P, and Si only exist during two years and also for a companion project (Trophic BATS, i.e. TBATS). A combined dataset from BATS and TBATS was used to better understand the coupling of C, N, P, and Si in the Sargasso Sea by analyzing particulate phases of each element in the water column and exported material. Three conclusions are inferred: first, the effect of mesoscale eddies on standing stocks, export rates, and elemental coupling of C, N, P, and Si displays strong seasonality. Statistically significant differences between particulate water column and export ratios using internal and between site comparisons were robust in the summer only. Second, N, Si and particularly P were more efficiently recycled within the euphotic zones of eddies as elemental ratios in export material were greater than the corresponding ratios in the water column. This suggests that P may have a more critical biogeochemical role and its supply rate to the euphotic zone may control primary production in these closed systems. Third, the trends seen in these eddies do not support that export production was enhanced, instead these features had more efficient recycling of N, P, and Si relative to the BATS site. This decrease in export efficiency suggests a stimulation of export production above 'normal' BATS conditions within eddies would require significantly higher autotrophic standing stock and correspondingly high rates of organic matter production.

Impacts of Mass-dimension and Area-dimension relationships on retrieval ice particle effective radius from radar and lidar measurements

NASA Astrophysics Data System (ADS)

Ham, S. H.; Kato, S.; Rose, F. G.

2016-12-01

In the retrieval of ice clouds from Radar and Lidar Measurements, mass-Dimension (m-D) and Area-Dimension (A-D) relationships are often used to describe nonspherical ice particle shapes. This study analytically investigates how the assumption of m-D and A-D relationships affects retrieval of ice effective radius. We use gamma and lognormal particle distributions and integrate optical parameters over the size distribution. The effective radius is expressed as a function of radar reflectivity factor, visible extinction coefficient, and parameters describing m-D and A-D relationships. The analytic expressions are used for converting effective radius retrieved from one set of m-D and A-D relationships into that with another set of m-D and A-D, including plates, solid columns, bullets, and mixture of different habits. The conversion method can be used for consistent radiative transfer simulation with cloud retrieval algorithms. In addition, when we want to merge cloud effective radii retrieved from different m-D and A-D, the conversion method can be efficiently used to remove undesired biases caused by m-D and A-D assumptions. Furthermore, the sensitivity of the effective radius to m-D and A-D relationships can be quantified by taking the first derivative of the effective radius with respect to parameters expressing the m-D and A-D relationships.

Numerical modeling of the elution peak profiles of retained solutes in supercritical fluid chromatography

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

Kaczmarski, Krzysztof; Guiochon, Georges A

2011-01-01

In supercritical fluid chromatography (SFC), the significant expansion of the mobile phase along the column causes the formation of axial and radial gradients of temperature. Due to these gradients, the mobile phase density, its viscosity, its velocity, its diffusion coefficients, etc. are not constant throughout the column. This results in a nonuniform flow velocity distribution, itself causing a loss of column efficiency in certain cases, even at low flow rates, as they do in HPLC. At high flow rates, an important deformation of the elution profiles of the sample components may occur. The model previously used to account satisfactorily formore » the retention of an unsorbed solute in SFC is applied to the modeling of the elution peak profiles of retained compounds. The numerical solution of the combined heat and mass balance equations provides the temperature and the pressure profiles inside the column and values of the retention time and the band profiles of retained compounds that are in excellent agreement with independent experimental data for large value of mobile phase reduced density. At low reduced densities, the band profiles can strongly depend on the column axial distribution of porosity.« less

Electrophoretic Separation of Single Particles Using Nanoscale Thermoplastic Columns.

PubMed

Weerakoon-Ratnayake, Kumuditha M; Uba, Franklin I; Oliver-Calixte, Nyoté J; Soper, Steven A

2016-04-05

Phenomena associated with microscale electrophoresis separations cannot, in many cases, be applied to the nanoscale. Thus, understanding the electrophoretic characteristics associated with the nanoscale will help formulate relevant strategies that can optimize the performance of separations carried out on columns with at least one dimension below 150 nm. Electric double layer (EDL) overlap, diffusion, and adsorption/desorption properties and/or dielectrophoretic effects giving rise to stick/slip motion are some of the processes that can play a role in determining the efficiency of nanoscale electrophoretic separations. We investigated the performance characteristics of electrophoretic separations carried out in nanoslits fabricated in poly(methyl methacrylate), PMMA, devices. Silver nanoparticles (AgNPs) were used as the model system with tracking of their transport via dark field microscopy and localized surface plasmon resonance. AgNPs capped with citrate groups and the negatively charged PMMA walls (induced by O2 plasma modification of the nanoslit walls) enabled separations that were not apparent when these particles were electrophoresed in microscale columns. The separation of AgNPs based on their size without the need for buffer additives using PMMA nanoslit devices is demonstrated herein. Operational parameters such as the electric field strength, nanoslit dimensions, and buffer composition were evaluated as to their effects on the electrophoretic performance, both in terms of efficiency (plate numbers) and resolution. Electrophoretic separations performed at high electric field strengths (>200 V/cm) resulted in higher plate numbers compared to lower fields due to the absence of stick/slip motion at the higher electric field strengths. Indeed, 60 nm AgNPs could be separated from 100 nm particles in free solution using nanoscale electrophoresis with 100 μm long columns.

On-line Analysis of Catalytic Reaction Products Using a High-Pressure Tandem Micro-reactor GC/MS.

PubMed

Watanabe, Atsushi; Kim, Young-Min; Hosaka, Akihiko; Watanabe, Chuichi; Teramae, Norio; Ohtani, Hajime; Kim, Seungdo; Park, Young-Kwon; Wang, Kaige; Freeman, Robert R

2017-01-01

When a GC/MS system is coupled with a pressurized reactor, the separation efficiency and the retention time are directly affected by the reactor pressure. To keep the GC column flow rate constant irrespective of the reaction pressure, a restrictor capillary tube and an open split interface are attached between the GC injection port and the head of a GC separation column. The capability of the attached modules is demonstrated for the on-line GC/MS analysis of catalytic reaction products of a bio-oil model sample (guaiacol), produced under a pressure of 1 to 3 MPa.

Assessment of removal efficiency of perfluorocompounds (PFCs) in a semiconductor fabrication plant by gas chromatography.

PubMed

Ou Yang, Chang-Feng; Kam, Seak-Hong; Liu, Chia-Hung; Tzou, Jiren; Wang, Jia-Lin

2009-08-01

This study investigated a gas chromatographic (GC) method to assess the destruction or removal efficiency (DRE) of local scrubbers on five perfluorocompounds (PFCs), i.e., SF(6), NF(3), CF(4), C(2)F(6), and C(3)F(8), which are very potent greenhouse gases used in a semiconductor fabrication plant. Air samples taken at inlets and outlets of local scrubbers were analyzed by a self-constructed multi-column GC system equipped with thermal conductivity detection. Three packed columns were integrated into the heart-cut GC system to allow simultaneous analysis of the five target PFCs. The Porapak Q pre-column performs rough separation and cuts eluent groups to two analytical columns for optimal separation. The Molecular Sieve - 5A column separated NF(3), CF(4), and C(3)F(8) and the second Porapak Q separated SF(6) and C(2)F(6). Linearity was greater than 0.995 (R(2)) for the five PFCs, and the reproducibility was about 4% (relative standard deviation) for NF(3), and better than 0.5% for the other four PFCs. DRE for the combustion (CB) and electric-thermal types of local scrubbers was evaluated by taking into account the in-line dilution from air and fuel gases. Both flow and tracer methods were employed to deduce the dilution factors (DFs). For the tracer method, helium was employed as the tracer and injected upstream of the scrubbers and thus mixed with the exhaust gas. With this method, the DFs were determined to be in the range from 4.8 to 5.9 for the CB unit, significantly higher than the value of 3.3 based on the flow method. The DREs for the CB unit for C(3)F(8) were greater than 90% and between 40% and 50% for CF(4).

Effects of clay dispersion on aquifer storage and recovery in coastal aquifers

USGS Publications Warehouse

Konikow, Leonard F.; August, L.L.; Voss, C.I.

2001-01-01

Cyclic injection, storage, and withdrawal of freshwater in brackish aquifers is a form of aquifer storage and recovery (ASR) that can beneficially supplement water supplies in coastal areas. A 1970s field experiment in Norfolk, Virginia, showed that clay dispersion in the unconsolidated sedimentary aquifer occurred because of cation exchange on clay minerals as freshwater displaced brackish formation water. Migration of interstitial clay particles clogged pores, reduced permeability, and decreased recovery efficiency, but a calcium preflush was found to reduce clay dispersion and lead to a higher recovery efficiency. Column experiments were performed in this study to quantify the relations between permeability changes and clay mineralogy, clay content, and initial water salinity. The results of these experiments indicate that dispersion of montmorillonite clay is a primary contributor to formation damage. The reduction in permeability by clay dispersion may be expressed as a linear function of chloride content. Incorporating these simple functions into a radial, cross-sectional, variable-density, ground-water flow and transport model yielded a satisfactory simulation of the Norfolk field test - and represented an improvement over the model that ignored changes in permeability. This type of model offers a useful planning and design tool for ASR operations in coastal clastic aquifer systems.

Human recombinant soluble guanylyl cyclase: expression, purification, and regulation

NASA Technical Reports Server (NTRS)

Lee, Y. C.; Martin, E.; Murad, F.

2000-01-01

The alpha1- and beta1-subunits of human soluble guanylate cyclase (sGC) were coexpressed in the Sf9 cells/baculovirus system. In addition to the native enzyme, constructs with hexahistidine tag at the amino and carboxyl termini of each subunit were coexpressed. This permitted the rapid and efficient purification of active recombinant enzyme on a nickel-affinity column. The enzyme has one heme per heterodimer and was readily activated with the NO donor sodium nitroprusside or 3-(5'-hydroxymethyl-2'furyl)-1-benzyl-indazole (YC-1). Sodium nitroprusside and YC-1 treatment potentiated each other in combination and demonstrated a remarkable 2,200-fold stimulation of the human recombinant sGC. The effects were inhibited with 1H-(1,2, 4)oxadiazole(4,3-a)quinoxalin-1one (ODQ). The kinetics of the recombinant enzyme with respect to GTP was examined. The products of the reaction, cGMP and pyrophosphate, inhibited the enzyme. The extent of inhibition by cGMP depended on the activation state of the enzyme, whereas inhibition by pyrophosphate was not affected by the enzyme state. Both reaction products displayed independent binding and cooperativity with respect to enzyme inhibition. The expression of large quantities of active enzyme will facilitate structural characterization of the protein.

Nanocapillaries for Open Tubular Chromatographic Separations of Proteins in Femtoliter to Picoliter Samples

PubMed Central

Wang, Xiayan; Cheng, Chang; Wang, Shili; Zhao, Meiping; Dasgupta, Purnendu K.; Liu, Shaorong

2009-01-01

We have recently examined the potential of bare nanocapillaries for free solution DNA separations and demonstrated efficiencies exceeding 106 theoretical plates/m. In the present work, we demonstrate the use of bare and hydroxypropylcellulose (HPC) coated open tubular nanocapillaries for protein separations. Using 1.5 μm inner diameter (i.d.) capillary columns, hydrodynamically injecting femto to picoliter (fL-pL) volumes of fluorescent or fluorescent dye labeled protein samples, utilizing a pneumatically pressurized chamber containing 1.0 mM sodium tetraborate solution eluent (typ. 200 psi) as the pump and performing on-column detection using a simple laser-induced fluorescence detector, we demonstrate efficiencies of close to a million theoretical plates/m while generating single digit μL volumes of waste for a complete chromatographic run. We achieve baseline resolution for a protein mixture consisting of transferrin, α-lactalbumin, insulin, and α -2-macroglobulin. PMID:19663450

Countercurrent Chromatographic Separation of Proteins Using an Eccentric Coiled Column with Synchronous and Nonsynchronous Type-J Planetary Motions

PubMed Central

SHINOMIYA, Kazufusa; YOSHIDA, Kazunori; TOKURA, Koji; TSUKIDATE, Etsuhiro; YANAGIDAIRA, Kazuhiro; ITO, Yoichiro

2015-01-01

Protein separation was performed using the high-speed counter-current chromatograph (HSCCC) at both synchronous and nonsynchronous type-J planetary motions. The partition efficiency was evaluated with two different column configurations, eccentric coil and toroidal coil, on the separation of a set of stable protein samples including cytochrome C, myoglobin and lysozyme with a polymer phase system composed of 12.5% (w/w) polyethylene glycol 1000 and 12.5% (w/w) dibasic potassium phosphate. Better peak resolution was obtained by the eccentric coil than by the toroidal coil using either lower or upper phase as the mobile phase. The peak resolution was further improved using the eccentric coil by the nonsynchronous type-J planetary motion with the combination of 1066 rpm of column rotation and 1000 rpm of revolution. PMID:25765276

Countercurrent chromatographic separation of proteins using an eccentric coiled column with synchronous and nonsynchronous type-J planetary motions.

PubMed

Shinomiya, Kazufusa; Yoshida, Kazunori; Tokura, Koji; Tsukidate, Etsuhiro; Yanagidaira, Kazuhiro; Ito, Yoichiro

2015-01-01

Protein separation was performed using the high-speed countercurrent chromatograph (HSCCC) at both synchronous and nonsynchronous type-J planetary motions. The partition efficiency was evaluated with two different column configurations, eccentric coil and toroidal coil, on the separation of a set of stable protein samples including cytochrome C, myoglobin and lysozyme with a polymer phase system composed of 12.5% (w/w) polyethylene glycol 1000 and 12.5% (w/w) dibasic potassium phosphate. Better peak resolution was obtained by the eccentric coil than by the toroidal coil using either lower or upper phase as the mobile phase. The peak resolution was further improved using the eccentric coil by the nonsynchronous type-J planetary motion with the combination of 1066 rpm of column rotation and 1000 rpm of revolution.

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

PubMed

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

2005-02-01

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

Global Concerns and Local Realities: The "Making Education Inclusive" Conference in Johannesburg

ERIC Educational Resources Information Center

Walton, Elizabeth

2015-01-01

Inclusive education is a global phenomenon expressed differently in various countries, and different contextual realities support or constrain the process of making education more inclusive. This column reports on an international conference on inclusive education in Johannesburg, South Africa, which provided the opportunity for delegates to share…

Room temperature ionic liquids: new GC stationary phases with a novel selectivity for flavor and fragrance analyses.

PubMed

Cagliero, Cecilia; Bicchi, Carlo; Cordero, Chiara; Liberto, Erica; Sgorbini, Barbara; Rubiolo, Patrizia

2012-12-14

Ionic liquids (ILs) are of great interest as moderately polar to polar stationary phases for GC, because their selectivity differs markedly from that of conventionally used phases. In the flavor, fragrance and essential oil fields, analysts often deal with complex mixtures of compounds having similar structural and physical characteristics (e.g., mono- and sesquiterpenoids), therefore requiring an interactive combination between chromatographic and mass spectral data for correct identification. New GC stationary phases with different selectivity must therefore be continually tested. Performance and evolution over time of commercially available IL columns versus those commonly used in these fields are here evaluated, mainly in view of their routine use. Chromatographic and separative properties (efficiency, separation capability, inertness and/or activity) of commercially available IL columns were compared to those of columns coated with 5% phenyl-95% methylpolysiloxane, 14% cyanopropyl-86% polysiloxane, and polyethylene glycol, on different complexity samples, including standard mixtures of volatile suspected allergens and pesticides, and cornmint and vetiver essential oils. The results show that IL columns can successfully be used for a wide range of applications characteristic of these fields, mainly because of their unusual selectivity, in particular when separations based on functional groups are required. Moreover, the latest generation of IL columns (IL61 and IL60) presents chromatographic performance comparable to or only slightly lower than that of the conventional columns routinely used in these fields. Copyright © 2012 Elsevier B.V. All rights reserved.

Comparison of amphiphilic polyurethane nanoparticles to nonionic surfactants for flushing phenanthrene from soil.

PubMed

Kim, Ju-Young; Shim, Sun-Bo; Shim, Jin-Kie

2004-12-31

Amphiphilic polyurethane (APU) nanoparticles were synthesized through crosslinking polymerization of nano-aggregates of urethane acrylate nonionomer (UAN). The efficiency of in situ extraction of sorbed phenanthrene from aquifer material was tested using soil columns and compared with that of surfactants such as Triton X-100, Brij 30, and Tween 80. The extraction efficiency of those washing materials strongly depended on their concentration, flow rate, and the degree of sorption within soil column. That is, the extraction efficiency increased with the decrease of flow rate and the degree of sorption and the increase of the concentration. Even though the surfactants are superior to APU nanoparticles at solubilizing phenanthrene, at the same flow rate (0.02 mL/min) and concentration (4000 mg/L), the effectiveness of in situ soil washing of APU nanoparticles was about two times higher than those of surfactants. This is because, at the lower flow rates, the degree of sorption of APU nanoparticles was lower than that of surfactants, owing to the chemically crosslinked nature of APU nanoparticles.

Biclustering sparse binary genomic data.

PubMed

van Uitert, Miranda; Meuleman, Wouter; Wessels, Lodewyk

2008-12-01

Genomic datasets often consist of large, binary, sparse data matrices. In such a dataset, one is often interested in finding contiguous blocks that (mostly) contain ones. This is a biclustering problem, and while many algorithms have been proposed to deal with gene expression data, only two algorithms have been proposed that specifically deal with binary matrices. None of the gene expression biclustering algorithms can handle the large number of zeros in sparse binary matrices. The two proposed binary algorithms failed to produce meaningful results. In this article, we present a new algorithm that is able to extract biclusters from sparse, binary datasets. A powerful feature is that biclusters with different numbers of rows and columns can be detected, varying from many rows to few columns and few rows to many columns. It allows the user to guide the search towards biclusters of specific dimensions. When applying our algorithm to an input matrix derived from TRANSFAC, we find transcription factors with distinctly dissimilar binding motifs, but a clear set of common targets that are significantly enriched for GO categories.

Multi-wavelength campaign on NGC 7469. II. Column densities and variability in the X-ray spectrum

NASA Astrophysics Data System (ADS)

Peretz, U.; Behar, E.; Kriss, G. A.; Kaastra, J.; Arav, N.; Bianchi, S.; Branduardi-Raymont, G.; Cappi, M.; Costantini, E.; De Marco, B.; Di Gesu, L.; Ebrero, J.; Kaspi, S.; Mehdipour, M.; Middei, R.; Paltani, S.; Petrucci, P. O.; Ponti, G.; Ursini, F.

2018-01-01

We have investigated the ionic column density variability of the ionized outflows associated with NGC 7469, to estimate their location and power. This could allow a better understanding of galactic feedback of AGNs to their host galaxies. Analysis of seven XMM-Newton grating observations from 2015 is reported. We used an individual-ion spectral fitting approach, and compared different epochs to accurately determine variability on timescales of years, months, and days. We find no significant column density variability in a ten-year period implying that the outflow is far from the ionizing source. The implied lower bound on the ionization equilibrium time, ten years, constrains the lower limit on the distance to be at least 12 pc, and up to 31 pc, much less but consistent with the 1 kpc wide starburst ring. The ionization distribution of column density is reconstructed from measured column densities, nicely matching results of two 2004 observations, with one large high ionization parameter (ξ) component at 2 < log ξ< 3.5, and one at 0.5 < log ξ< 1 in cgs units. The strong dependence of the expression for kinetic power, ∝ 1 /ξ, hampers tight constraints on the feedback mechanism of outflows with a large range in ionization parameter, which is often observed and indicates a non-conical outflow. The kinetic power of the outflow is estimated here to be within 0.4 and 60% of the Eddington luminosity, depending on the ion used to estimate ξ.

Numerical modeling of elution peak profiles in supercritical fluid chromatography. Part I--elution of an unretained tracer.

PubMed

Kaczmarski, Krzysztof; Poe, Donald P; Guiochon, Georges

2010-10-15

When chromatography is carried out with high-density carbon dioxide as the main component of the mobile phase (a method generally known as "supercritical fluid chromatography" or SFC), the required pressure gradient along the column is moderate. However, this mobile phase is highly compressible and, under certain experimental conditions, its density may decrease significantly along the column. Such an expansion absorbs heat, cooling the column, which absorbs heat from the outside. The resulting heat transfer causes the formation of axial and radial gradients of temperature that may become large under certain conditions. Due to these gradients, the mobile phase velocity and most physico-chemical parameters of the system (viscosity, diffusion coefficients, etc.) are no longer constant throughout the column, resulting in a loss of column efficiency, even at low flow rates. At high flow rates and in serious cases, systematic variations of the retention factors and the separation factors with increasing flow rates and important deformations of the elution profiles of all sample components may occur. The model previously used to account satisfactorily for the effects of the viscous friction heating of the mobile phase in HPLC is adapted here to account for the expansion cooling of the mobile phase in SFC and is applied to the modeling of the elution peak profiles of an unretained compound in SFC. The numerical solution of the combined heat and mass balance equations provides temperature and pressure profiles inside the column, and values of the retention time and efficiency for elution of this unretained compound that are in excellent agreement with independent experimental data. Copyright © 2010 Elsevier B.V. All rights reserved.

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

PubMed

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

2007-09-01

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

Enantiomeric separation of triazole fungicides with 3-μm and 5-μml particle chiral columns by reverse-phase high-performance liquid chromatography.

PubMed

Qiu, Jing; Dai, Shouhui; Zheng, Chuangmu; Yang, Shuming; Chai, Tingting; Bie, Mei

2011-07-01

This study used chiral columns packed with 3-μm and 5-μm particles to comparatively separate enantiomers of 9 triazole fungicides, and Lux Cellulose-1 columns with chiral stationary phase of cellulose-tris-(3,5-dimethylphenylcarbamate) were used on reverse-phase high-performance liquid chromatography with flow rates of 0.3 and 1.0 mL min(-1) for 3-μm and 5-μm columns, respectively. The (+)-enantiomers of hexaconazole (1), tetraconazole (4), myclobutanil (7), fenbuconazole (8) and the (-)-enantiomers of flutriafol (2), diniconazole (3), epoxiconazole (5), penconazole (6), triadimefon (9) were firstly eluted from both columns, the elution orders identified with an optical rotation detector didn't change with variety of column particles and mobile phases (acetronitrile/water and methanol/water). The plots of natural logarithms of the selectivity factors (ln α) for all fungicides except penconazole (6) versus the inverse of temperature (1/T) were linear in range of 5-40°C. The thermodynamic parameters (ΔH°, ΔS°, ΔΔH° and ΔΔS°) were calculated using Van't Hoff equations to understand the thermosynamic driving forces for enantioseparation. This work will be very helpful to obtain good enantiomeric separation and establish more efficient analytical method for triazole fungicides. Chirality, 2011. © 2011 Wiley-Liss, Inc. Copyright © 2011 Wiley-Liss, Inc.

Determination of traces of 237Np in environmental samples by ICP-MS after separation using TOA extraction chromatography.

PubMed

Ji, Y Q; Li, J Y; Luo, S G; Wu, T; Liu, J L

2001-09-01

A simple, rapid, cost-efficient, and robust method for separation of 237Np with an extraction chromatographic column (TOA: tri-n-octylamine on Teflon powder) is outlined in detail and further improved for direct ICP-MS analysis. The column efficiently retained 237Np in 2 mol L(-1) HNO3 medium and all of the 237Np was easily eluted with 0.02 mol L(-1) oxalic acid in 0.16 mol L(-1) HNO3 at 95 degrees C. The separated solutions were free from most matrix elements and were aspirated into the ICP-MS directly. The decontamination factor for 238U is more than 10(4). The instrumental detection limit for 237Np was 0.46 pg mL(-1), which corresponds to 1.2 x 10(-5) Bq mL(-1). The method is more rapid than traditional radiometric techniques. It is also considered to be more suitable for environmental monitoring than existing methods based on TOA.

VizieR Online Data Catalog: Bessel (1825) calculation for geodesic measurements (Karney+, 2010)

NASA Astrophysics Data System (ADS)

Karney, C. F. F.; Deakin, R. E.

2010-06-01

The solution of the geodesic problem for an oblate ellipsoid is developed in terms of series. Tables are provided to simplify the computation. Included here are the tables that accompanied Bessel's paper (with corrections). The tables were crafted by Bessel to be minimize the labor of hand calculations. To this end, he adjusted the intervals in the tables, the number of terms included in the series, and the number of significant digits given so that the final results are accurate to about 8 places. For that reason, the most useful form of the tables is as the PDF file which provides the tables in a layout close to the original. Also provided is the LaTeX source file for the PDF file. Finally, the data has been put into a format so that it can be read easily by computer programs. All the logarithms are in base 10 (common logarithms). The characteristic and the mantissa should be read separately (indicated as x.c and x.m in the file description). Thus the first entry in the table, -4.4, should be parsed as "-4" (the characteristic) and ".4" (the mantissa); the anti-log for this entry is 10(-4+0.4)=2.5e-4. The "Delta" columns give the first difference of the preceding column, i.e., the difference of the preceding column in the next row and the preceding column in the current row. In the printed tables these are expressed as "units in the last place" and the differences are of the rounded representations in the preceding columns (to minimize interpolation errors). In table1.dat these are given scaled to a match the format used for the preceding column, as indicated by the units given for these columns. The unit log(") (in the description within square brackets [arcsec]) means the logarithm of a quantity expressed in arcseconds. (3 data files).

The quantitative impact of the mesopore size on the mass transfer mechanism of the new 1.9 μm fully porous Titan-C18 particles II--analysis of biomolecules.

PubMed

Gritti, Fabrice; Guiochon, Georges

2015-05-01

The kinetic performances of 3.0 × 100 mm columns packed with 1.9 μm Titan-C18 particles with average mesopore sizes of 80 Å and 120 Å were investigated quantitatively for the analysis of biomolecules. Large mesopores are expected to speed up the rate of diffusivity of high-molecular-weight compounds across the stationary phase and to generate higher plate counts at high velocities. The mass transfer mechanism of bradykinin acetate salt (1060 Da) and insulin (5733 Da) was determined over a range of flow rates from 0.025 to 1.0 mL/min. The pore diffusivities of these two biomolecules were accurately measured from the peak parking method. Even though the gain in column efficiency was not found significant for small molecules such as valerophenone (162 Da), enlarging the average pore size from 80 to 120 Å induces a measurable diminution of the reduced plate height, h, of bradykinin (from 17 to 11 or -35% at a reduced velocity of 50) and a significant reduction for insulin (from 43 to 12 or -72% at a reduced velocity of 90). Remarkably, while the increase of the column efficiency for bradykinin is consistent with a faster diffusivity of bradykinin across the 120 Å Titan-C18 particles, the higher column efficiencies measured for insulin are mostly due to a faster absorption kinetics into the 120 Å than that into the 80 Å Titan-C18 particles. This result is supported by the fact that the effective pore diffusivity of insulin is even slightly smaller across the 120 Å than that across the 80 Å 1.9μm Titan-C18 particles. Copyright © 2015 Elsevier B.V. All rights reserved.

One-Step Chromatographic Purification of Helicobacter pylori Neutrophil-Activating Protein Expressed in Bacillus subtilis

PubMed Central

Shih, Kuo-Shun; Lin, Chih-Chang; Hung, Hsiao-Fang; Yang, Yu-Chi; Wang, Chung-An; Jeng, Kee-Ching; Fu, Hua-Wen

2013-01-01

Helicobacter pylori neutrophil-activating protein (HP-NAP), a major virulence factor of Helicobacter pylori (H. pylori), is capable of activating human neutrophils to produce reactive oxygen species (ROS) and secrete inammatory mediators. HP-NAP is a vaccine candidate, a possible drug target, and a potential in vitro diagnostic marker for H. pylori infection. HP-NAP has also been shown to be a novel therapeutic agent for the treatment of allergic asthma and bladder cancer. Hence, an efficient way to obtain pure HP-NAP needs to be developed. In this study, one-step anion-exchange chromatography in negative mode was applied to purify the recombinant HP-NAP expressed in Bacillus subtilis (B. subtilis). This purification technique was based on the binding of host cell proteins and/or impurities other than HP-NAP to DEAE Sephadex resins. At pH 8.0, almost no other proteins except HP-NAP passed through the DEAE Sephadex column. More than 60% of the total HP-NAP with purity higher than 91% was recovered in the flow-through fraction from this single-step DEAE Sephadex chromatography. The purified recombinant HP-NAP was further demonstrated to be a multimeric protein with a secondary structure of α-helix and capable of activating human neutrophils to stimulate ROS production. Thus, this one-step negative chromatography using DEAE Sephadex resin can efficiently yield functional HP-NAP from B. subtilis in its native form with high purity. HP-NAP purified by this method could be further utilized for the development of new drugs, vaccines, and diagnostics for H. pylori infection. PMID:23577158

Grey water treatment in urban slums by a filtration system: optimisation of the filtration medium.

PubMed

Katukiza, A Y; Ronteltap, M; Niwagaba, C B; Kansiime, F; Lens, P N L

2014-12-15

Two uPVC columns (outer diameter 160 cm, internal diameter 14.6 cm and length 100 cm) were operated in parallel and in series to simulate grey water treatment by media based filtration at unsaturated conditions and constant hydraulic loading rates (HLR). Grey water from bathroom, laundry and kitchen activities was collected from 10 households in the Bwaise III slum in Kampala (Uganda) in separate containers, mixed in equal proportions followed by settling, prior to transferring the influent to the tanks. Column 1 was packed with lava rock to a depth of 60 cm, while column 2 was packed with lava rock (bottom 30 cm) and silica sand, which was later replaced by granular activated carbon (top 30 cm) to further investigate nutrient removal from grey water. Operating the two filter columns in series at a HLR of 20 cm/day resulted in a better effluent quality than at a higher (40 cm/day) HLR. The COD removal efficiencies by filter columns 1 and 2 in series amounted to 90% and 84% at HLR of 20 cm/day and 40 cm/day, respectively. TOC and DOC removal efficiency amounted to 77% and 71% at a HLR of 20 cm/day, but decreased to 72% and 67% at a HLR of 40 cm/day, respectively. The highest log removal of Escherichia coli, Salmonella sp. and total coliforms amounted to 3.68, 3.50 and 3.95 at a HLR of 20 cm/day respectively. The overall removal of pollutants increased with infiltration depth, with the highest pollutant removal efficiency occurring in the top 15 cm layer. Grey water pre-treatment followed by double filtration using coarse and fine media has the potential to reduce the grey water pollution load in slum areas by more than 60%. Copyright © 2014 Elsevier Ltd. All rights reserved.

Modeling of rotating disc contactor (RDC) column

NASA Astrophysics Data System (ADS)

Ismail, Wan Nurul Aiffah; Zakaria, Siti Aisyah; Noor, Nor Fashihah Mohd; Sulong, Ibrahim; Arshad, Khairil Anuar

2014-12-01

Liquid-liquid extraction is one of the most important separation processes. Different kinds of liquid-liquid extractor such as Rotating Disc Contactor (RDC) Column being used in industries. The study of liquid-liquid extraction in an RDC column has become a very important subject to be discussed not just among chemical engineers but mathematician as well. In this research, the modeling of small diameter RDC column using the chemical system involving cumene/isobutryric asid/water are analyzed by the method of Artificial Neural Network (ANN). In the previous research, we begin the process of analyzed the data using methods of design of the experiments (DOE) to identify which factor and their interaction factor are significant and to determine the percentage of contribution of the variance for each factor. From the result obtained, we continue the research by discussed the development and validation of an artificial neural network model in estimating the concentration of continuous and concentration of dispersed outlet for an RDC column. It is expected that an efficient and reliable model will be formed to predict RDC column performance as an alternative to speed up the simulation process.

Graphene-ZIF8 composite material as stationary phase for high-resolution gas chromatographic separations of aliphatic and aromatic isomers.

PubMed

Yang, Xiaohong; Li, Changxia; Qi, Meiling; Qu, Liangti

2016-08-19

This work presents the separation performance of graphene-ZIF8 (G-Z) composite material as stationary phase for capillary gas chromatography (GC). The G-Z stationary phase achieved high column efficiency of 5000 plates/m determined by n-dodecane (k=1.22) at 120°C and showed weakly polar nature. Importantly, it exhibited high selectivity and resolving capability for branched alkane isomers and aromatic positional isomers, showing clear advantages over the reported neat graphene and ZIF8. In addition, it attained high resolution for geometric cis-/trans-isomers. The G-Z column exhibited good column thermal stability up to 300°C and column repeatability with RSD values of retention times in the range of 0.01-0.19% for intra-day, 0.05-0.88% for inter-day and 0.66-5.6% for between-column, respectively, Moreover, the G-Z column was employed for the determination of minor impurity isomers in real reagent samples, which demonstrates its promising potential in GC applications. Copyright © 2016 Elsevier B.V. All rights reserved.

Determination of the boiling-point distribution by simulated distillation from n-pentane through n-tetratetracontane in 70 to 80 seconds.

PubMed

Lubkowitz, Joaquin A; Meneghini, Roberto I

2002-01-01

This work presents the carrying out of boiling-point distributions by simulated distillation with direct-column heating rather than oven-column heating. Column-heating rates of 300 degrees C/min are obtained yielding retention times of 73 s for n-tetratetracontane. The calibration curves of the retention time versus the boiling point, in the range of n-pentane to n-tetratetracontane, are identical to those obtained by slower oven-heating rates. The boiling-point distribution of the reference gas oil is compared with that obtained with column oven heating at rates of 15 to 40 degrees C/min. The results show boiling-point distribution values nearly the same (1-2 degrees F) as those obtained with oven column heating from the initial boiling point to 80% distilled off. Slightly higher differences are obtained (3-4 degrees F) for the 80% distillation to final boiling-point interval. Nonetheless, allowed consensus differences are never exceeded. Precision of the boiling-point distributions (expressed as standard deviations) are 0.1-0.3% for the data obtained in the direct column-heating mode.

In situ removal of arsenic from groundwater by using permeable reactive barriers of organic matter/limestone/zero-valent iron mixtures.

PubMed

Gibert, O; de Pablo, J; Cortina, J-L; Ayora, C

2010-08-01

In this study, two mixtures of municipal compost, limestone and, optionally, zero-valent iron were assessed in two column experiments on acid mine treatment. The effluent solution was systematically analysed throughout the experiment and precipitates from both columns were withdrawn for scanning electron microscopy, energy-dispersive X-ray spectroscopy, X-ray diffractometry analysis and, from the column containing zero-valent iron, solid digestion and sequential extraction analysis. The results showed that waters were cleaned of arsenic, metals and acidity, but chemical and morphological analysis suggested that metal removal was not due predominantly to biogenic sulphide generation but to pH increase, i.e. metal (oxy)hydroxide and carbonate precipitation. Retained arsenic and metal removal were clearly associated to co-precipitation with and/or sorption on iron and aluminum (oxy)hydroxides. An improvement on the arsenic removal efficiency was achieved when the filling mixture contained zero-valent iron. Values of arsenic concentrations were then always below 10 microg/L.

Purification method for recombinant proteins based on a fusion between the target protein and the C-terminus of calmodulin

NASA Technical Reports Server (NTRS)

Schauer-Vukasinovic, Vesna; Deo, Sapna K.; Daunert, Sylvia

2002-01-01

Calmodulin (CaM) was used as an affinity tail to facilitate the purification of the green fluorescent protein (GFP), which was used as a model target protein. The protein GFP was fused to the C-terminus of CaM, and a factor Xa cleavage site was introduced between the two proteins. A CaM-GFP fusion protein was expressed in E. coli and purified on a phenothiazine-derivatized silica column. CaM binds to the phenothiazine on the column in a Ca(2+)-dependent fashion and it was, therefore, used as an affinity tail for the purification of GFP. The fusion protein bound to the affinity column was then subjected to a proteolytic digestion with factor Xa. Pure GFP was eluted with a Ca(2+)-containing buffer, while CaM was eluted later with a buffer containing the Ca(2+)-chelating agent EGTA. The purity of the isolated GFP was verified by SDS-PAGE, and the fluorescence properties of the purified GFP were characterized.

Removing Chlorides From Metallurgical-Grade Silicon

NASA Technical Reports Server (NTRS)

Breneman, W. C.; Coleman, L. M.

1982-01-01

Process for making low-cost silicon for solar cells is further improved. Silane product recycled to feed stripper column converts some of heavy impurities to volatile ones that pass off at top of column with light wastes. Impurities--chlorides of arsenic, phosphorus, and boron-would otherwise be carried to subsequent distillations where they would be difficult to remove. Since only a small amount of silane is recycled, silicon production efficiency remains high.

A rapid silica spin column-based method of RNA extraction from fruit trees for RT-PCR detection of viruses.

PubMed

Yang, Fan; Wang, Guoping; Xu, Wenxing; Hong, Ni

2017-09-01

Efficient recovery of high quality RNA is very important for successful RT-PCR detection of plant RNA viruses. High levels of polyphenols and polysaccharides in plant tissues can irreversibly bind to and/or co-precipitate with RNA, which influences RNA isolation. In this study, a silica spin column-based RNA isolation method was developed by using commercially available silica columns combined with the application of a tissue lysis solution, and binding and washing buffers with high concentration guanidinium thiocyanate (GuSCN, 50% w/v), which helps remove plant proteins, polysaccharides and polyphenolic compounds. The method was successfully used to extract high quality RNA from citrus (Citrus aurantifolia), grapevine (Vitis vinifera), peach (Prunus persica), pear (Pyrus spp.), taro (Colocosia esculenta) and tobacco (Nicotiana benthamiana) samples. The method was comparable to conventional CTAB method in RNA isolation efficiency, but it was more sample-adaptable and cost-effective than commercial kits. High quality RNA isolated using silica spin column-based method was successfully used for the RT-PCR and/or multiplex RT-PCR amplification of woody fruit tree viruses and a viroid. The study provided a useful tool for the detection and characterization of plant viruses. Copyright © 2017 Elsevier B.V. All rights reserved.

Ultra high pressure liquid chromatography. Column permeability and changes of the eluent properties.

PubMed

Gritti, Fabrice; Guiochon, Georges

2008-04-11

The behavior of four similar liquid chromatography columns (2.1mm i.d. x 30, 50, 100, and 150 mm, all packed with fine particles, average d(p) approximately 1.7 microm, of bridged ethylsiloxane/silica hybrid-C(18), named BEH-C(18)) was studied in wide ranges of temperature and pressure. The pressure and the temperature dependencies of the viscosity and the density of the eluent (pure acetonitrile) along the columns were also derived, using the column permeabilities and applying the Kozeny-Carman and the heat balance equations. The heat lost through the external surface area of the chromatographic column was directly derived from the wall temperature of the stainless steel tube measured with a precision of +/-0.2 degrees C in still air and +/-0.1 degrees C in the oven compartment. The variations of the density and viscosity of pure acetonitrile as a function of the temperature and pressure was derived from empirical correlations based on precise experimental data acquired between 298 and 373 K and at pressures up to 1.5 kbar. The measurements were made with the Acquity UPLC chromatograph that can deliver a maximum flow rate of 2 mL/min and apply a maximum column inlet pressure of 1038 bar. The average Kozeny-Carman permeability constant of the columns was 144+/-3.5%. The temperature hence the viscosity and the density profiles of the eluent along the column deviate significantly from linear behavior under high-pressure gradients. For a 1000 bar pressure drop, we measured DeltaT=25-30 K, (Deltaeta/eta) approximately 100%, and (Deltarho/rho) approximately 10%. These results show that the radial temperature profiles are never fully developed within 1% for any of the columns, even under still-air conditions. This represents a practical advantage regarding the apparent column efficiency at high flow rates, since the impact of the differential analyte velocity between the column center and the column wall is not maximum. The interpretation of the peak profiles recorded in UPLC is discussed.

Integrated process of distillation with side reactors for synthesis of organic acid esters

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

Panchal, Chandrakant B; Prindle, John C; Kolah, Aspri

An integrated process and system for synthesis of organic-acid esters is provided. The method of synthesizing combines reaction and distillation where an organic acid and alcohol composition are passed through a distillation chamber having a plurality of zones. Side reactors are used for drawing off portions of the composition and then recycling them to the distillation column for further purification. Water is removed from a pre-reactor prior to insertion into the distillation column. An integrated heat integration system is contained within the distillation column for further purification and optimizing efficiency in the obtaining of the final product.

Cosmic distribution of highly ionized metals and their physical conditions in the EAGLE simulations

NASA Astrophysics Data System (ADS)

Rahmati, Alireza; Schaye, Joop; Crain, Robert A.; Oppenheimer, Benjamin D.; Schaller, Matthieu; Theuns, Tom

2016-06-01

We study the distribution and evolution of highly ionized intergalactic metals in the Evolution and Assembly of Galaxies and their Environment (EAGLE) cosmological, hydrodynamical simulations. EAGLE has been shown to reproduce a wide range of galaxy properties while its subgrid feedback was calibrated without considering gas properties. We compare the predictions for the column density distribution functions (CDDFs) and cosmic densities of Si IV, C IV, N V, O VI and Ne VIII absorbers with observations at redshift z = 0 to ˜6 and find reasonable agreement, although there are some differences. We show that the typical physical densities of the absorbing gas increase with column density and redshift, but decrease with the ionization energy of the absorbing ion. The typical metallicity increases with both column density and time. The fraction of collisionally ionized metal absorbers increases with time and ionization energy. While our results show little sensitivity to the presence or absence of AGN feedback, increasing/decreasing the efficiency of stellar feedback by a factor of 2 substantially decreases/increases the CDDFs and the cosmic densities of the metal ions. We show that the impact of the efficiency of stellar feedback on the CDDFs and cosmic densities is largely due to its effect on the metal production rate. However, the temperatures of the metal absorbers, particularly those of strong O VI, are directly sensitive to the strength of the feedback.

Immunochromatographic assay of cadmium levels in oysters.

PubMed

Nishi, Kosuke; Kim, In-Hae; Itai, Takaaki; Sugahara, Takuya; Takeyama, Haruko; Ohkawa, Hideo

2012-08-15

Oysters are one of foodstuffs containing a relatively high amount of cadmium. Here we report on establishment of an immunochromatographic assay (ICA) method of cadmium levels in oysters. Cadmium was extracted with 0.l mol L(-1) HCl from oysters and cleaned up from other metals by the use of an anion-exchange column. The behavior of five metals Mn, Fe, Cu, Zn, and Cd was monitored at each step of extraction and clean-up procedure for the ICA method in an inductively coupled plasma-mass spectrometry (ICP-MS) analysis. The results revealed that a simple extraction method with the HCl solution was efficient enough to extract almost all of cadmium from oysters. Clean-up with an anion-exchange column presented almost no loss of cadmium adsorbed on the column and an efficient removal of metals other than cadmium. When a spiked recovery test was performed in the ICA method, the recovery ranged from 98% to 112% with relative standard deviations between 5.9% and 9.2%. The measured values of cadmium in various oyster samples in the ICA method were favorably correlated with those in ICP-MS analysis (r(2)=0.97). Overall results indicate that the ICA method established in the present study is an adequate and reliable detection method for cadmium levels in oysters. Copyright © 2012 Elsevier B.V. All rights reserved.

Efficient Filtration of Effluent Organic Matter by Polycation-Clay Composite Sorbents: Effect of Polycation Configuration on Pharmaceutical Removal.

PubMed

Shabtai, Itamar A; Mishael, Yael G

2016-08-02

Hybrid polycation-clay composites, based on methylated poly vinylpyridinium, were optimized as sorbents for secondary effluent organic matter (EfOM) including emerging micropollutants. Composite structure was tuned by solution ionic strength and characterized by zeta potential, FTIR, X-ray diffraction, and thermal gravimetric analyses. An increase in ionic strength induced a transition from a train to a loops and tails configuration, accompanied by greater polycation adsorption. Composite charge reversal (zeta potential -18 to 45 mV) increased the adsorption of EfOM and humic acid (HA), moderately and sharply, respectively, suggesting electrostatic and also nonspecific interactions with EfOM. Filtration of EfOM by columns of positively charged composites was superior to that of granular activated carbon (GAC). The overall removal of EfOM was most efficient by the composite with a train configuration. Whereas a composite with a loops and tails configuration was beneficial for the removal of the anionic micropollutants diclofenac, gemfibrozil and ibuprofen from EfOM. These new findings suggest that the loops and tails may offer unique binding sites for small micropollutants which are overseen by the bulk EfOM. Furthermore, they may explain our previous observations that in the presence of dissolved organic matter, micropollutant filtration by GAC columns was reduced, while their filtration by composite columns remained high.

Olive mill wastewater treatment using a simple zeolite-based low-cost method.

PubMed

Aly, Anwar A; Hasan, Yousef N Y; Al-Farraj, Abdullah S

2014-12-01

Olive mill wastewater (OMW), a liquid by-product of the olive oil industry, represents a severe environmental problem owing to its high pollution load. In this study, successive columns containing different types of natural materials were investigated for their OMW treatment efficiency. Passing OMW through three columns of gravel, fine sand, and a mixture of acidified cotton and zeolite (weight:weight ratio of cotton:clinoptilolite of 2:1), followed by treatment with activated charcoal (AC) and lime, was the best treatment in terms of the quality of water obtained. This treatment decreased concentrations of [Formula: see text] , B, K, P, and total fat in OMW by mean percentages of 78.0, 92.4, 66.6, 48.3, and 93.3%, respectively. Furthermore, it decreased OMW turbidity and electric conductivity (EC) by 96.8 and 48.4%, respectively. Most contaminants were removed from the OMW in the cotton/clinoptilolite column owing to the high sorption affinity of clinoptilolite on its active sites. The AC was efficient for organic particle removal; meanwhile, lime was used to raise the pH of the treated OMW (TOMW) from 2.9 to 5.1. This simple method enables us to obtain environmentally friendly TOMW that can be safely used for irrigation. Copyright © 2014 Elsevier Ltd. All rights reserved.

Sol-gel chemistry-based Ucon-coated columns for capillary electrophoresis.

PubMed

Hayes, J D; Malik, A

1997-07-18

A sol-gel chemistry-based novel approach for the preparation of a Ucon-coated fused-silica capillary column in capillary electrophoresis is presented. In this approach the sol-gel process is carried out inside 25 microm I.D. fused-silica capillaries. The sol solution contained appropriate quantities of an alkoxide-based sol-gel precursor, a polymeric coating material (Ucon), a crosslinking reagent, a surface derivatizing reagent, controlled amounts of water and a catalyst dissolved in a suitable solvent system. The coating procedure involves filling a capillary with the sol solution and allowing the sol-gel process to proceed for an optimum period. Hydrolysis of the alkoxide precursor and polycondensation of the hydrolyzed products with the surface silanol groups and the hydroxy-terminated Ucon molecules lead to the formation of a surface-bonded sol-gel coating on the inner walls of the capillary. The thickness of the coated film can be controlled by varying the reaction time, coating solution composition and experimental conditions. Commercial availability of high purity sol-gel precursors (e.g., TEOS 99.999%), the ease of coating, run-to-run and column-to-column reproducibility, and long column lifetimes make sol-gel coating chemistry very much suitable for being applied in analytical microseparations column technology. Test samples of basic proteins and nucleotides were used to evaluate the column performance. These results show that the sol-gel coating scheme has allowed for the generation of bio-compatible surfaces characterized by high separation efficiencies in CE. For different types of solutes, the sol-gel coated Ucon column consistently provided migration time R.S.D. values of the order of 0.5%.

Experiment and modeling for the separation of guaifenesin enantiomers using simulated moving bed and Varicol units.

PubMed

Gong, Rujin; Lin, Xiaojian; Li, Ping; Yu, Jianguo; Rodrigues, Alirio E

2014-10-10

The separation of guaifenesin enantiomers by both simulated moving bed (SMB) process and Varicol process was investigated experimentally and theoretically, where the columns were packed with cellulose tris 3,5-dimethylphenylcarbamate (Chiralcel OD) stationary phase and a mixture of n-hexane and ethanol was used as mobile phase. The operation conditions were designed based on the separation region with the consideration of mass transfer resistance and axial dispersion, and the experiments to separate guaifenesin enantiomers were carried out on VARICOL-Micro unit using SMB process with the column configuration of 1/2/2/1 and Varicol process with the column configuration of 1/1.5/1.5/1, respectively. Single enantiomer with more than 99.0% purity was obtained in both processes with the productivity of 0.42 genantiomer/dcm(3) CSP for SMB process and 054 genantiomer/dcm(3) CSP for Varicol process. These experimental results obtained from SMB and Varicol processes were compared with those reported from literatures. In addition, according to the numerical simulation, the effects of solid-film mass transfer resistance and axial dispersion on the internal profiles were discussed, and the effect of column configuration on the separation performance of SMB and Varicol processes was analyzed for a few columns system. The feasibility and efficiency for the separation of guaifenesin enantiomers by SMB and Varicol processes were evaluated. Copyright © 2014 Elsevier B.V. All rights reserved.

Inhibitory effects of acidic pH and confounding effects of moisture content on methane biofiltration.

PubMed

Barzgar, Sonya; Hettiaratchi, Joseph Patrick; Pearse, Lauretta; Kumar, Sunil

2017-12-01

This study focussed on evaluating the effect of hydrogen sulfide (H 2 S) on biological oxidation of waste methane (CH 4 ) gas in compost biofilters, Batch experiments were conducted to determine the dependency of maximum methane oxidation rate (V max ) on two main factors; pH and moisture content, as well as their interaction effects. The maximum V max was observed at a pH of 7.2 with decreasing V max values observed with decreasing pH, irrespective of moisture content. Flow-through columns operated at a pH of 4.5 oxidized CH 4 at a flux rate of 53g/m 2 /d compared to 146g/m 2 /d in columns operated at neutral pH. No oxidation activity was observed for columns operated at pH 2.5, and DNA sequencing analysis of samples led to the conclusion that highly acidic conditions were responsible for inhibiting the ability of methanotrophs to oxidize CH 4 . Biofilter columns operated at pH 2.5 contained only 2% methanotrophs (type I) out of the total microbial population, compared to 55% in columns operated at pH 7.5. Overall, changes in the population of methanotrophs with acidification within the biofilters compromised its capacity to oxidize CH 4 which demonstrated that a compost biofilter could not operate efficiently in the presence of high levels of H 2 S. Copyright © 2017 Elsevier Ltd. All rights reserved.

Accuracy of three-dimensional seismic ground response analysis in time domain using nonlinear numerical simulations

NASA Astrophysics Data System (ADS)

Liang, Fayun; Chen, Haibing; Huang, Maosong

2017-07-01

To provide appropriate uses of nonlinear ground response analysis for engineering practice, a three-dimensional soil column with a distributed mass system and a time domain numerical analysis were implemented on the OpenSees simulation platform. The standard mesh of a three-dimensional soil column was suggested to be satisfied with the specified maximum frequency. The layered soil column was divided into multiple sub-soils with a different viscous damping matrix according to the shear velocities as the soil properties were significantly different. It was necessary to use a combination of other one-dimensional or three-dimensional nonlinear seismic ground analysis programs to confirm the applicability of nonlinear seismic ground motion response analysis procedures in soft soil or for strong earthquakes. The accuracy of the three-dimensional soil column finite element method was verified by dynamic centrifuge model testing under different peak accelerations of the earthquake. As a result, nonlinear seismic ground motion response analysis procedures were improved in this study. The accuracy and efficiency of the three-dimensional seismic ground response analysis can be adapted to the requirements of engineering practice.

Use of laterite for the removal of fluoride from contaminated drinking water.

PubMed

Sarkar, Mitali; Banerjee, Aparna; Pramanick, Partha Pratim; Sarkar, Asit R

2006-10-15

The effects of different operational variables on the mechanistic function of laterite in removal of fluoride have been investigated. Thermodynamic parameters such as free energy change, enthalpy, and entropy of the process, as well as the sorption isotherm, were evaluated. The extent of solute removal is determined by initial solute concentration, operational conditions, laterite dose, and solution pH. For a fixed set of experimental conditions, a model equation is developed from which the percent removal corresponding to each load of fluoride is determined. The mechanism of fluoride adsorption is governed by the zero point charge of laterite and follows a first-order rate equation. pH has a vital role influencing the surface characteristics of laterite. To simulate the flow dynamics, fluoride solution was run through a fixed bed column. The pattern of breakthrough curves for different influent fluoride concentration, pH, and column bed height was characterized. The column efficiency was tested from the bed depth-service time model. The elution of the retained fluoride was studied and the effectiveness of column operation was determined by the retention-elution cycles.

Computational analysis of vertical axis wind turbine arrays

NASA Astrophysics Data System (ADS)

Bremseth, J.; Duraisamy, K.

2016-10-01

Canonical problems involving single, pairs, and arrays of vertical axis wind turbines (VAWTs) are investigated numerically with the objective of understanding the underlying flow structures and their implications on energy production. Experimental studies by Dabiri (J Renew Sustain Energy 3, 2011) suggest that VAWTs demand less stringent spacing requirements than their horizontal axis counterparts and additional benefits may be obtained by optimizing the placement and rotational direction of VAWTs. The flowfield of pairs of co-/counter-rotating VAWTs shows some similarities with pairs of cylinders in terms of wake structure and vortex shedding. When multiple VAWTs are placed in a column, the extent of the wake is seen to spread further downstream, irrespective of the direction of rotation of individual turbines. However, the aerodynamic interference between turbines gives rise to regions of excess momentum between the turbines which lead to significant power augmentations. Studies of VAWTs arranged in multiple columns show that the downstream columns can actually be more efficient than the leading column, a proposition that could lead to radical improvements in wind farm productivity.

Heavy metal adsorption changes of EAF steel slag after phosphorus adsorption.

PubMed

Song, Guanling; Cao, Lijing; Chen, Xiao; Hou, Wenhua; Wang, Qunhui

2012-01-01

A kind of electric arc furnace (EAF) steel slag was phosphated, and its isothermal and dynamic adsorptions of copper, cadmium, and lead ions were measured to determine if heavy metal adsorption changes after phosphorus adsorption. The surface area increased greatly after the slag was phosphated. Isothermal adsorption experiments showed that the theoretical Q(max) of the EAF steel slag on Cu(2+), Cd(2+), and Pb(2+) improved 59, 50, and 89% respectively after it was phosphated. Dynamic adsorption results showed that the greatest adsorption capacities of unit volume of Cu(2+), Cd(2+), and Pb(2+) were 2.2, 1.8, and 1.8 times that of the column packed with original EAF steel slag when the column was packed with phosphate EAF steel slag at the same heavy metal ion concentration. The breakthrough time, the exhaustion time and elution efficiency of the column also increased when the column was packed with phosphated EAF steel slag compared with that packed with original EAF steel slag. Phosphorus adsorption could further improve the heavy metal ion adsorption of the EAF steel slag.

Analysis of programming properties and the row-column generation method for 1-norm support vector machines.

PubMed

Zhang, Li; Zhou, WeiDa

2013-12-01

This paper deals with fast methods for training a 1-norm support vector machine (SVM). First, we define a specific class of linear programming with many sparse constraints, i.e., row-column sparse constraint linear programming (RCSC-LP). In nature, the 1-norm SVM is a sort of RCSC-LP. In order to construct subproblems for RCSC-LP and solve them, a family of row-column generation (RCG) methods is introduced. RCG methods belong to a category of decomposition techniques, and perform row and column generations in a parallel fashion. Specially, for the 1-norm SVM, the maximum size of subproblems of RCG is identical with the number of Support Vectors (SVs). We also introduce a semi-deleting rule for RCG methods and prove the convergence of RCG methods when using the semi-deleting rule. Experimental results on toy data and real-world datasets illustrate that it is efficient to use RCG to train the 1-norm SVM, especially in the case of small SVs. Copyright © 2013 Elsevier Ltd. All rights reserved.

Pu Anion Exchange Process Intensification

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

Taylor-Pashow, Kathryn M. L.

This research is focused on improving the efficiency of the anion exchange process for purifying plutonium. While initially focused on plutonium, the technology could also be applied to other ion-exchange processes. Work in FY17 focused on the improvement and optimization of porous foam columns that were initially developed in FY16. These foam columns were surface functionalized with poly(4-vinylpyridine) (PVP) to provide the Pu specific anion-exchange sites. Two different polymerization methods were explored for maximizing the surface functionalization with the PVP. The open-celled polymeric foams have large open pores and large surface areas available for sorption. The fluid passes through themore » large open pores of this material, allowing convection to be the dominant mechanism by which mass transport takes place. These materials generally have very low densities, open-celled structures with high cell interconnectivity, small cell sizes, uniform cell size distributions, and high structural integrity. These porous foam columns provide advantages over the typical porous resin beads by eliminating the slow diffusion through resin beads, making the anion-exchange sites easily accessible on the foam surfaces. The best performing samples exceeded the Pu capacity of the commercially available resin, and also offered the advantage of sharper elution profiles, resulting in a more concentrated product, with less loss of material to the dilute heads and tails cuts. An alternate approach to improving the efficiency of this process was also explored through the development of a microchannel array system for performing the anion exchange.« less

Investigation related to hydrogen isotopes separation by cryogenic distillation

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

Bornea, A.; Zamfirache, M.; Stefanescu, I.

2008-07-15

Research conducted in the last fifty years has shown that one of the most efficient techniques of removing tritium from the heavy water used as moderator and coolant in CANDU reactors (as that operated at Cernavoda (Romania)) is hydrogen cryogenic distillation. Designing and implementing the concept of cryogenic distillation columns require experiments to be conducted as well as computer simulations. Particularly, computer simulations are of great importance when designing and evaluating the performances of a column or a series of columns. Experimental data collected from laboratory work will be used as input for computer simulations run at larger scale (formore » The Pilot Plant for Tritium and Deuterium Separation) in order to increase the confidence in the simulated results. Studies carried out were focused on the following: - Quantitative analyses of important parameters such as the number of theoretical plates, inlet area, reflux flow, flow-rates extraction, working pressure, etc. - Columns connected in series in such a way to fulfil the separation requirements. Experiments were carried out on a laboratory-scale installation to investigate the performance of contact elements with continuous packing. The packing was manufactured in our institute. (authors)« less

Study on bubble column humidification and dehumidification system for coal mine wastewater treatment.

PubMed

Gao, Penghui; Zhang, Meng; Du, Yuji; Cheng, Bo; Zhang, Donghai

2018-04-01

Water is important resource for human survival and development. Coal mine wastewater (CMW) is a byproduct of the process of coal mining, which is about 7.0 × 10 10 m 3 in China in 2016. Considering coal mine wastewater includes different ingredients, a new bubble column humidification and dehumidification system is proposed for CMW treatment. The system is mainly composed of a bubble column humidification and dehumidification unit, solar collector, fan and water tank, in which air is used as a circulating medium. The system can avoid water treatment component blocking for reverse osmosis (RO) and multi effect distillation (MED) dealing with CMW, and produce water greenly. By analysis of heat and mass transfer, the effects of solar radiation, air bubble velocity and mine water temperature on water treatment production characteristics are studied. Compared with other methods, thermal energy consumption (TEC) of bubble column humidification and dehumidification (BCHD) is moderate, which is about 700 kJ/kg (powered by solar energy). The results would provide a new method for CMW treatment and insights into the efficient coal wastewater treatment, besides, it helps to identify the parameters for the technology development in mine water treatment.

Removal of arsenic from aqueous solutions using waste iron columns inoculated with iron bacteria.

PubMed

Azhdarpoor, Abooalfazl; Nikmanesh, Roya; Samaei, Mohammad Reza

2015-01-01

Arsenic contamination of water resources is one of the serious risks threatening natural ecosystems and human health. This study investigates arsenic removal using a waste iron column with and without iron bacteria in continuous and batch phases. In batch experiments, the effects of pH, contact time, initial concentration of arsenic and adsorbent dose were investigated. Results indicated that the highest arsenate removal efficiency occurred at pH 7 (96.76%). On increasing the amount of waste iron from 0.25 to 1 g, the removal rate changed from about 42.37%-96.70%. The results of continuous experiments on the column containing waste iron showed that as the empty bed contact time increased from 5 to 60 min, the secondary arsenate concentration changed from 23 to 6 µg/l. In experiments involving a waste iron column with iron bacteria, an increase in residence time from 5 to 60 min decreased the secondary arsenate concentration from 14.97 to 4.86 µg/l. The results of this study showed that waste iron containing iron bacteria is a good adsorbent for removal of arsenic from contaminated water.

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

PubMed

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

2016-07-13

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

The Design of Airplane-engine Superchargers

NASA Technical Reports Server (NTRS)

Von Der Null, Werner

1937-01-01

With the forms of superchargers and underlying principles of computation, delivery heads per stage of 7,000 to 8,500 meters (air column) at an effective efficiency, based on the adiabatic process, of 0.7 may be attained, the space and weight requirements being kept within reasonable limits.

Integrated continuous processing of proteins expressed as inclusion bodies: GCSF as a case study.

PubMed

Kateja, Nikhil; Agarwal, Harshit; Hebbi, Vishwanath; Rathore, Anurag S

2017-07-01

Affordability of biopharmaceuticals continues to be a challenge, particularly in developing economies. This has fuelled advancements in manufacturing that can offer higher productivity and better economics without sacrificing product quality in the form of an integrated continuous manufacturing platform. While platform processes for monoclonal antibodies have existed for more than a decade, development of an integrated continuous manufacturing process for bacterial proteins has received relatively scant attention. In this study, we propose an end-to-end integrated continuous downstream process (from inclusion bodies to unformulated drug substance) for a therapeutic protein expressed in Escherichia coli as inclusion body. The final process consisted of a continuous refolding in a coiled flow inverter reactor directly coupled to a three-column periodic counter-current chromatography for capture of the product followed by a three-column con-current chromatography for polishing. The continuous bioprocessing train was run uninterrupted for 26 h to demonstrate its capability and the resulting output was analyzed for the various critical quality attributes, namely product purity (>99%), high molecular weight impurities (<0.5%), host cell proteins (<100 ppm), and host cell DNA (<10 ppb). All attributes were found to be consistent over the period of operation. The developed assembly offers smaller facility footprint, higher productivity, fewer hold steps, and significantly higher equipment and resin utilization. The complexities of process integration in the context of continuous processing have been highlighted. We hope that the study presented here will promote development of highly efficient, universal, end-to-end, fully continuous platforms for manufacturing of biotherapeutics. © 2016 American Institute of Chemical Engineers Biotechnol. Prog., 33:998-1009, 2017. © 2016 American Institute of Chemical Engineers.

Transport and degradation of metalaxyl and isoproturon in biopurification columns inoculated with pesticide-primed material.

PubMed

De Wilde, Tineke; Spanoghe, Pieter; Sniegowksi, Kristel; Ryckeboer, Jaak; Jaeken, Peter; Springael, Dirk

2010-01-01

Laboratory column displacement experiments were performed to examine whether addition of pesticide-primed material to the matrix of an on-farm biopurification system (BPS), intended to remove pesticides from agricultural waste water, positively affects the degradation of mobile pesticides in the system. Percolated column microcosms with varying types and amounts of metalaxyl and/or isoproturon-primed material or non-primed material were irrigated with water artificially contaminated with isoproturon and/or metalaxyl. Transport of isoproturon was well described using the convection dispersion equation and no dissipation was observed, even in columns inoculated with isoproturon-primed material. On the other hand, delayed dissipation of metalaxyl, i.e., after an initial lag phase, was encountered in all columns receiving metalaxyl. In all systems, dissipation could be described using the Monod model indicating that a metalaxyl degrading population grew in the systems. There was a clear correlation between the lag phase and the amount of metalaxyl-primed material added to the system, i.e., increasing amounts of added material resulted into shorter lag phases and hence more rapid initiation of growth-associated metalaxyl degradation in the system. Our observations suggest that indeed pesticide-primed material can reduce the start-up phase of degradation of mobile pesticides in a BPS and as such can increase its efficiency. However, the primed material should be chosen carefully and preferentially beforehand tested for its capacity to degrade the pesticide.

Innexin gap junctions in nerve cells coordinate spontaneous contractile behavior in Hydra polyps

NASA Astrophysics Data System (ADS)

Takaku, Yasuharu; Hwang, Jung Shan; Wolf, Alexander; Böttger, Angelika; Shimizu, Hiroshi; David, Charles N.; Gojobori, Takashi

2014-01-01

Nerve cells and spontaneous coordinated behavior first appeared near the base of animal evolution in the common ancestor of cnidarians and bilaterians. Experiments on the cnidarian Hydra have demonstrated that nerve cells are essential for this behavior, although nerve cells in Hydra are organized in a diffuse network and do not form ganglia. Here we show that the gap junction protein innexin-2 is expressed in a small group of nerve cells in the lower body column of Hydra and that an anti-innexin-2 antibody binds to gap junctions in the same region. Treatment of live animals with innexin-2 antibody eliminates gap junction staining and reduces spontaneous body column contractions. We conclude that a small subset of nerve cells, connected by gap junctions and capable of synchronous firing, act as a pacemaker to coordinate the contraction of the body column in the absence of ganglia.

Innexin gap junctions in nerve cells coordinate spontaneous contractile behavior in Hydra polyps

PubMed Central

Takaku, Yasuharu; Hwang, Jung Shan; Wolf, Alexander; Böttger, Angelika; Shimizu, Hiroshi; David, Charles N.; Gojobori, Takashi

2014-01-01

Nerve cells and spontaneous coordinated behavior first appeared near the base of animal evolution in the common ancestor of cnidarians and bilaterians. Experiments on the cnidarian Hydra have demonstrated that nerve cells are essential for this behavior, although nerve cells in Hydra are organized in a diffuse network and do not form ganglia. Here we show that the gap junction protein innexin-2 is expressed in a small group of nerve cells in the lower body column of Hydra and that an anti-innexin-2 antibody binds to gap junctions in the same region. Treatment of live animals with innexin-2 antibody eliminates gap junction staining and reduces spontaneous body column contractions. We conclude that a small subset of nerve cells, connected by gap junctions and capable of synchronous firing, act as a pacemaker to coordinate the contraction of the body column in the absence of ganglia. PMID:24394722

Innexin gap junctions in nerve cells coordinate spontaneous contractile behavior in Hydra polyps.

PubMed

Takaku, Yasuharu; Hwang, Jung Shan; Wolf, Alexander; Böttger, Angelika; Shimizu, Hiroshi; David, Charles N; Gojobori, Takashi

2014-01-07

Nerve cells and spontaneous coordinated behavior first appeared near the base of animal evolution in the common ancestor of cnidarians and bilaterians. Experiments on the cnidarian Hydra have demonstrated that nerve cells are essential for this behavior, although nerve cells in Hydra are organized in a diffuse network and do not form ganglia. Here we show that the gap junction protein innexin-2 is expressed in a small group of nerve cells in the lower body column of Hydra and that an anti-innexin-2 antibody binds to gap junctions in the same region. Treatment of live animals with innexin-2 antibody eliminates gap junction staining and reduces spontaneous body column contractions. We conclude that a small subset of nerve cells, connected by gap junctions and capable of synchronous firing, act as a pacemaker to coordinate the contraction of the body column in the absence of ganglia.

Modeling the Stability of Volatile Deposits in Lunar Cold Traps

NASA Technical Reports Server (NTRS)

Crider, D. H.; Vondrak, R. R.

2002-01-01

There are several mechanisms acting at the cold traps that can alter the inventory of volatiles there. Primarily, the lunar surface is bombarded by meteoroids which impact, melt, process, and redistribute the regolith. Further, solar wind and magnetospheric ion fluxes are allowed limited access onto the regions in permanent shadow. Also, although cold traps are in the permanent shadow of the Sun, there is a small flux of radiation incident on the regions from interstellar sources. We investigate the effects of these space weathering processes on a deposit of volatiles in a lunar cold trap through simulations. We simulate the development of a column of material near the surface of the Moon resulting from space weathering. This simulation treats a column of material at a lunar cold trap and focuses on the hydrogen content of the column. We model space weathering processes on several time and spatial scales to simulate the constant rain of micrometeoroids as well as sporadic larger impactors occurring near the cold traps to determine the retention efficiency of the cold traps. We perform the Monte Carlo simulation over many columns of material to determine the expectation value for hydrogen content of the top few meters of soil for comparison with Lunar Prospector neutron data.

Validated HPLC method for determination of sennosides A and B in senna tablets.

PubMed

Sun, Shao Wen; Su, Hsiu Ting

2002-07-31

This study developed an efficient and reliable ion-pair liquid chromatographic method for quantitation of sennosides A and B in commercial senna tablets. Separation was conducted on a Hypersil C 18 column (250 x 4.6 mm, 5 microm) at a temperature of 40 degrees C, using a mixture of 0.1 M acetate buffer (pH 6.0) and acetonitrile (70:30, v/v) containing 5 mM tetrahexylammonium bromide as mobile phase. Sennosides A and B were completely separated from other constituents within 14 min. The developed method was validated. Both run-to-run repeatability (n=10) and day-to-day reproducibility (n=3) of peak area were below 0.4% RSD. Linearity of peak area was tested in the range 30-70 microg/ml (r>0.9997). Accuracy was assessed with recovery and the recoveries for sennosides A and B were 101.73+/-1.30% and 101.81+/-2.18% (n=3 x 6), respectively. Robustness of the analytical method was tested using a three-leveled Plackett-Burman design in which 11 factors were assessed with 23 experiments. Eight factors (column, concentration of ion pair reagent, % of organic modifier (acetonitrile), buffer pH, column temperature, flow rate, time constant and detection wavelength) were investigated in a specified range above and below the nominal method conditions. It was found that: (1) column and % acetonitrile affected significantly resolution and retention time, (2) column, % acetonitrile, column temperature, flow rate and time constant affected significantly the plate number of sennoside A, and (3) column and time constant affected significantly the tailing factor.

Importance of mechanics and kinematics in determining the stiffness contribution of the vertebral column during body-caudal-fin swimming in fishes.

PubMed

Nowroozi, Bryan N; Brainerd, Elizabeth L

2014-02-01

Whole-body stiffness in fishes has important consequences for swimming mode, speed and efficiency, but the contribution of vertebral column stiffness to whole-body stiffness is unclear. In our opinion, this lack of clarity is due in part to the lack of studies that have measured both in vitro mechanical properties of the vertebral column as well as in vivo vertebral kinematics in the same species. Some lack of clarity may also come from real variation in the mechanical role of the vertebral column across species. Previous studies, based on either mechanics or kinematics alone, suggest species-specific variation in vertebral column locomotor function that ranges from highly stiff regimes that contribute greatly to whole-body stiffness, and potentially act as a spring, to highly compliant regimes that only prohibit excessive flexion of the intervertebral joints. We review data collected in combined investigations of both mechanics and kinematics of three species, Myxine glutinosa, Acipenser transmontanus, and Morone saxatilis, to illustrate how mechanical testing within the context of the in vivo kinematics more clearly distinguishes the role of the vertebral column in each species. In addition, we identify species for which kinematic data are available, but mechanical data are lacking. We encourage further investigation of these species to fill these mechanical data gaps. Finally, we hope these future combined analyses will identify certain morphological, mechanical, or kinematic parameters that might be associated with certain vertebral column functional regimes with respect to body stiffness. Copyright © 2013 Elsevier GmbH. All rights reserved.

Large-Scale Structure of the Molecular Gas in Taurus Revealed by High Spatial Dynamic Range Spectral Line Mapping

NASA Technical Reports Server (NTRS)

Goldsmith, Paul F.

2008-01-01

Viewgraph topics include: optical image of Taurus; dust extinction in IR has provided a new tool for probing cloud morphology; observations of the gas can contribute critical information on gas temperature, gas column density and distribution, mass, and kinematics; the Taurus molecular cloud complex; average spectra in each mask region; mas 2 data; dealing with mask 1 data; behavior of mask 1 pixels; distribution of CO column densities; conversion to H2 column density; variable CO/H2 ratio with values much less than 10(exp -4) at low N indicated by UV results; histogram of N(H2) distribution; H2 column density distribution in Taurus; cumulative distribution of mass and area; lower CO fractional abundance in mask 0 and 1 regions greatly increases mass determined in the analysis; masses determined with variable X(CO) and including diffuse regions agrees well with the found from L(CO); distribution of young stars as a function of molecular column density; star formation efficiency; star formation rate and gas depletion; and enlarged images of some of the regions with numerous young stars. Additional slides examine the origin of the Taurus molecular cloud, evolution from HI gas, kinematics as a clue to its origin, and its relationship to star formation.

Linking leach chemistry and microbiology of low-grade copper ore bioleaching at different temperatures

NASA Astrophysics Data System (ADS)

Jia, Yan; Sun, He-yun; Tan, Qiao-yi; Gao, Hong-shan; Feng, Xing-liang; Ruan, Ren-man

2018-03-01

The effects of temperature on chalcocite/pyrite oxidation and the microbial population in the bioleaching columns of a low-grade chalcocite ore were investigated in this study. Raffinate from the industrial bioleaching heap was used as an irrigation solution for columns operated at 20, 30, 45, and 60°C. The dissolution of copper and iron were investigated during the bioleaching processes, and the microbial community was revealed by using a high-throughput sequencing method. The genera of Ferroplasma, Acidithiobacillus, Leptospirillum, Acidiplasma, and Sulfobacillus dominated the microbial community, and the column at a higher temperature favored the growth of moderate thermophiles. Even though microbial abundance and activity were highest at 30°C, the column at a higher temperature achieved a much higher Cu leaching efficiency and recovery, which suggested that the promotion of chemical oxidation by elevated temperature dominated the dissolution of Cu. The highest pyrite oxidation percentage was detected at 45°C. Higher temperature resulted in precipitation of jarosite in columns, especially at 60°C. The results gave implications to the optimization of heap bioleaching of secondary copper sulfide in both enhanced chalcocite leaching and acid/iron balance, from the perspective of leaching temperature and affected microbial community and activity.

Supercritical Fluid Chromatography of Drugs: Parallel Factor Analysis for Column Testing in a Wide Range of Operational Conditions

PubMed Central

Al-Degs, Yahya; Andri, Bertyl; Thiébaut, Didier; Vial, Jérôme

2017-01-01

Retention mechanisms involved in supercritical fluid chromatography (SFC) are influenced by interdependent parameters (temperature, pressure, chemistry of the mobile phase, and nature of the stationary phase), a complexity which makes the selection of a proper stationary phase for a given separation a challenging step. For the first time in SFC studies, Parallel Factor Analysis (PARAFAC) was employed to evaluate the chromatographic behavior of eight different stationary phases in a wide range of chromatographic conditions (temperature, pressure, and gradient elution composition). Design of Experiment was used to optimize experiments involving 14 pharmaceutical compounds present in biological and/or environmental samples and with dissimilar physicochemical properties. The results showed the superiority of PARAFAC for the analysis of the three-way (column × drug × condition) data array over unfolding the multiway array to matrices and performing several classical principal component analyses. Thanks to the PARAFAC components, similarity in columns' function, chromatographic trend of drugs, and correlation between separation conditions could be simply depicted: columns were grouped according to their H-bonding forces, while gradient composition was dominating for condition classification. Also, the number of drugs could be efficiently reduced for columns classification as some of them exhibited a similar behavior, as shown by hierarchical clustering based on PARAFAC components. PMID:28695040

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

PubMed

Park, Sin Young; Cheong, Won Jo

2015-09-01

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

Depth dependent microbial carbon use efficiency in the capillary fringe as affected by water table fluctuations in a column incubation experiment

NASA Astrophysics Data System (ADS)

Pronk, G. J.; Mellage, A.; Milojevic, T.; Smeaton, C. M.; Rezanezhad, F.; Van Cappellen, P.

2017-12-01

Microbial growth and turnover of soil organic carbon (SOC) depend on the availability of electron donors and acceptors. The steep geochemical gradients in the capillary fringe between the saturated and unsaturated zones provide hotspots of soil microbial activity. Water table fluctuations and the associated drying and wetting cycles within these zones have been observed to lead to enhanced turnover of SOC and adaptation of the local microbial communities. To improve our understanding of SOC degradation under changing moisture conditions, we carried out an automated soil column experiment with integrated of hydro-bio-geophysical monitoring under both constant and oscillating water table conditions. An artificial soil mixture composed of quartz sand, montmorillonite, goethite and humus was used to provide a well-defined system. This material was inoculated with a microbial community extracted from a forested riparian zone. The soils were packed into 6 columns (60 cm length and 7.5 cm inner diameter) to a height of 45 cm; and three replicate columns were incubated under constant water table while another three were saturated and drained monthly. The initial soil development, carbon cycling and microbial community development were then characterized during 10 months of incubation. This system provides an ideal artificial gradient from the saturated to the unsaturated zone to study soil development from initially homogeneous materials and the same microbial community composition under controlled conditions. Depth profiles of SOC and microbial biomass after 329 days of incubation showed a depletion of carbon in the transition drying and wetting zone that was not associated with higher accumulation of microbial biomass, indicating a lower carbon use efficiency of the microbial community established within the water table fluctuation zone. This was supported by a higher ATP to microbial biomass carbon ratio within the same zone. The findings from this study highlight the importance of considering the effects of transient soil moisture and oxygen availability on microbial mediated SOC transformations. The effects of these changes in carbon use efficiency need to be included in soil models in order to accurately predict SOC turnover.

A segmentation algorithm based on image projection for complex text layout

NASA Astrophysics Data System (ADS)

Zhu, Wangsheng; Chen, Qin; Wei, Chuanyi; Li, Ziyang

2017-10-01

Segmentation algorithm is an important part of layout analysis, considering the efficiency advantage of the top-down approach and the particularity of the object, a breakdown of projection layout segmentation algorithm. Firstly, the algorithm will algorithm first partitions the text image, and divided into several columns, then for each column scanning projection, the text image is divided into several sub regions through multiple projection. The experimental results show that, this method inherits the projection itself and rapid calculation speed, but also can avoid the effect of arc image information page segmentation, and also can accurate segmentation of the text image layout is complex.

Carbofuran biodegradation in brackish groundwater and its effect on the hydraulic properties of the porous medium

NASA Astrophysics Data System (ADS)

Amiaz, Yanai; Ronen, Zeev; Adar, Eilon; Weisbrod, Noam

2015-04-01

A chalk fractured aquitard beneath an industrial site is subjected to intense contamination due to percolation of contaminants from the different facilities operating at the site. In order to reduce further contamination, draining trenches were excavated and filled with coarse gravel (3-4 cm in diameter) forming a porous medium, to which the contaminated groundwater discharges from the fractures surrounding the trenches. This research is aimed at establishing a biodegrading process of high efficiency and performance within the draining trenches. The research includes both field and laboratory experiments. An experimental setup of five columns (50 cm length and 4.5 cm in diameter) was constructed under highly controlled conditions. Over the course of the experiments, the columns were filled with different particle sizes and placed in a temperature controlled chamber. Filtered groundwater (0.2 µm) from the site groundwater, enriched by a model contaminant carbofuran (CRF), was injected to the columns; as two of the columns were inoculated by CRF degrading microorganisms native in the site's groundwater, two columns were inoculated by CRF degrading bacteria from the external environment, and one column was used as a control. During the experiment, measurements were taken from different locations along each column. These include: (a) CRF concentration and (b) hydraulic pressure and solution viscosity (in order to obtain the changes in permeability). A tracer test using uranine was carried out in parallel, in order to obtain the changes in hydraulic parameters. Correlating CRF concentration variations to changes of hydraulic parameters enable the deduction due to the effect that biological activity (under different temperature regimes) has on the hydraulic properties of the porous medium and its effect on the process of contaminant groundwater bodies' remediation. Preliminary results suggest that although biodegradation occurs, microbial activity has minor effect on the hydraulic properties of the porous medium under the explored conditions.

Distillation with Vapour Compression. An Undergraduate Experimental Facility.

ERIC Educational Resources Information Center

Pritchard, Colin

1986-01-01

Discusses the need to design distillation columns that are more energy efficient. Describes a "design and build" project completed by two college students aimed at demonstrating the principles of vapour compression distillation in a more energy efficient way. General design specifications are given, along with suggestions for teaching…

Column studies on the evaluation of novel spacer granules for the removal of arsenite and arsenate from contaminated water.

PubMed

Gupta, Anjali; Sankararamakrishnan, Nalini

2010-04-01

Decontamination of arsenic ions from aqueous media has been investigated using iron chitosan spacer granules (ICS) as an adsorbent. Drying of beads saturated with a spacer sucrose was considered as simple treatment, to prevent the restriction of polymer network and enhance sorption capacity. The novel sorbent was studied in up flow column experiments conducted at different flow rates, pH and bed depth to quantify the treatment performance. It was found that silicate was more inhibitory than phosphate, and the silicate in groundwater controlled the arsenic removal efficiency. The column regeneration studies were carried out for two sorption-desorption cycles using 0.1N NaOH as the eluant. TCLP leaching tests were conducted on the arsenic loaded adsorbent which revealed the containment of arsenic-laden sludge can be managed without adverse environmental impact. The developed procedure was successfully applied for the removal of both As(III) and As(V) from arsenic contaminated drinking water samples. Copyright 2009 Elsevier Ltd. All rights reserved.

Can biophysical properties of submersed macrophytes be determined by remote sensing?

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

Malthus, T.J.; Ciraolo, G.; La Loggia, G.

1997-06-01

This paper details the development of a computationally efficient Monte Carlo simulation program to model photon transport through submersed plant canopies, with emphasis on Seagrass communities. The model incorporates three components: the transmission of photons through a water column of varying depth and turbidity; the interaction of photons within a submersed plant canopy of varying biomass; and interactions with the bottom substrate. The three components of the model are discussed. Simulations were performed based on measured parameters for Posidonia oceanica and compared to measured subsurface reflectance spectra made over comparable seagrass communities in Sicilian coastal waters. It is shown thatmore » the output is realistic. Further simulations are undertaken to investigate the effect of depth and turbidity of the overlying water column. Both sets of results indicate the rapid loss of canopy signal as depth increases and water column phytoplankton concentrations increase. The implications for the development of algorithms for the estimation of submersed canopy biophysical parameters are briefly discussed.« less

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

PubMed

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

2016-10-01

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

Mitigating oil spills in the water column

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

Barry, Edward; Libera, Joseph A.; Mane, Anil U.

The scale and scope of uncontrolled oil spills can be devastating. Diverse marine environments and fragile ecologies are some of the most susceptible to the many ill effects, while the economic costs can be crippling. A notoriously difficult challenge with no known technological solution is the successful removal of oil dispersed in the water column. Here, we address this problem through cheap and reusable oil sorbents based on the chemical modification of polymer foams. Interfacial chemistry was optimized and subsequently tested in a simulated marine environment at the National Oil Spill Response Research & Renewable Energy Test Facility, Ohmsett. Wemore » find favorable performance for surface oil mitigation and, for the first time, demonstrate the advanced sorbent's efficiency and efficacy at pilot scale in extraction of crude oil and refined petroleum products dispersed in the water column. As a result, this is a potentially disruptive technology, opening a new field of environmental science focused on sub-surface pollutant sequestration.« less

Mitigating oil spills in the water column

DOE PAGES

Barry, Edward; Libera, Joseph A.; Mane, Anil U.; ...

2017-10-05

The scale and scope of uncontrolled oil spills can be devastating. Diverse marine environments and fragile ecologies are some of the most susceptible to the many ill effects, while the economic costs can be crippling. A notoriously difficult challenge with no known technological solution is the successful removal of oil dispersed in the water column. Here, we address this problem through cheap and reusable oil sorbents based on the chemical modification of polymer foams. Interfacial chemistry was optimized and subsequently tested in a simulated marine environment at the National Oil Spill Response Research & Renewable Energy Test Facility, Ohmsett. Wemore » find favorable performance for surface oil mitigation and, for the first time, demonstrate the advanced sorbent's efficiency and efficacy at pilot scale in extraction of crude oil and refined petroleum products dispersed in the water column. As a result, this is a potentially disruptive technology, opening a new field of environmental science focused on sub-surface pollutant sequestration.« less

Determination of alkenylbenzenes and related flavour compounds in food samples by on-column preconcentration-capillary liquid chromatography.

PubMed

Avila, Mónica; Zougagh, Mohammed; Escarpa, Alberto; Ríos, Angel

2009-10-23

A new, simple and versatile method is presented for the determination of different concentration levels of alkenylbenzenes (eugenol, isoeugenol, eugenol methyl ether, myristicin, anethole and estragole) and the related flavour compounds (coumarin and pulegone) in food samples. The method involves the use of a stationary phase (capillary column) for the enrichment with appropriate elution. After the sample had completely passed through the capillary column the eluent was changed and the separation/detection was achieved. Excellent linearity was obtained under the proposed conditions for a direct determination method and a method including on-line preconcentration. The limits of detection were in the ranges 97-148 and 9.5-14.2 ng/mL, respectively. Evidence for a matrix effect was not found and recoveries between 92 and 110% were obtained. The precision of the method, expressed as relative standard deviation values, was below 5% in all cases. The applicability of this methodology was tested by analyzing synthetic and real food samples.

Implications of Warm Rain in Shallow Cumulus and Congestus Clouds for Large-Scale Circulations

NASA Astrophysics Data System (ADS)

Nuijens, Louise; Emanuel, Kerry; Masunaga, Hirohiko; L'Ecuyer, Tristan

2017-11-01

Space-borne observations reveal that 20-40% of marine convective clouds below the freezing level produce rain. In this paper we speculate what the prevalence of warm rain might imply for convection and large-scale circulations over tropical oceans. We present results using a two-column radiative-convective model of hydrostatic, nonlinear flow on a non-rotating sphere, with parameterized convection and radiation, and review ongoing efforts in high-resolution modeling and observations of warm rain. The model experiments investigate the response of convection and circulation to sea surface temperature (SST) gradients between the columns and to changes in a parameter that controls the conversion of cloud condensate to rain. Convection over the cold ocean collapses to a shallow mode with tops near 850 hPa, but a congestus mode with tops near 600 hPa can develop at small SST differences when warm rain formation is more efficient. Here, interactive radiation and the response of the circulation are crucial: along with congestus a deeper moist layer develops, which leads to less low-level radiative cooling, a smaller buoyancy gradient between the columns, and therefore a weaker circulation and less subsidence over the cold ocean. The congestus mode is accompanied with more surface precipitation in the subsiding column and less surface precipitation in the deep convecting column. For the shallow mode over colder oceans, circulations also weaken with more efficient warm rain formation, but only marginally. Here, more warm rain reduces convective tops and the boundary layer depth—similar to Large-Eddy Simulation (LES) studies—which reduces the integrated buoyancy gradient. Elucidating the impact of warm rain can benefit from large-domain high-resolution simulations and observations. Parameterizations of warm rain may be constrained through collocated cloud and rain profiling from ground, and concurrent changes in convection and rain in subsiding and convecting branches of circulations may be revealed from a collocation of space-borne sensors, including the Global Precipitation Measurement (GPM) and upcoming Aeolus missions.

A green method using a micellar system for determination of andrographolide and dehydroandrographolide in human plasma.

PubMed

Zhao, Qi; Ding, Jie; Jin, Haiyan; Ding, Lan; Ren, Nanqi

2013-04-01

A method based on cloud point extraction (CPE) coupled with high-performance liquid chromatography separation and ultraviolet (UV) detection was developed to determine andrographolide and dehydroandrographolide in human plasma. The nonionic surfactant Triton X-114 was chosen as the extraction medium. Variable parameters affecting the CPE efficiency were evaluated and optimized, such as concentrations of Triton X-114 and NaCl, pH, equilibration temperature and equilibration time. A Zorbax SB C18 column (250 × 4.6 mm i.d., 5 µm) was used for separation of the two analytes at 30°C. The UV detection was performed at 254 nm. Under the optimum conditions, the limits of detection of andrographolide and dehydroandrographolide are 0.032 and 0.019 µg/mL, respectively. The intra-day and inter-day precisions expressed as relative standard deviation ranged from 3.2 to 7.3% and from 2.9 and 8.6%. The recoveries of andrographolide and dehydroandrographolide were in the range of 76.8-98.6% at three fortified concentrations of 0.1, 0.5 and 1.0 µg/mL. This method was efficient, environmentally friendly, rapid and inexpensive for the extraction and determination of andrographolide and dehydroandrographolide in human plasma.

Cross talk and diffraction efficiency in angular multiplexed memories using improved polypeptide

NASA Astrophysics Data System (ADS)

Ramenah, Harry K.; Bertrand, Paul; Soubari, E. H.; Meyrueis, Patrick

1996-12-01

We studied energy coupling between gratings and angularly multiplexed 20 gratings with a uniform diffraction efficiency within 25 micrometer layer thickness of dichromated gelatin. The dependence of diffraction efficiency on beam ratio is given. We recorded a matrix form memory of nxmxp elements, where n and m are the rows and columns and p the number of multiplexes. For indication only, n equals m equals 10, p equals 20, the surface area of the matrix is 1 cm2. Color diffractive images and digital data are illustrated as well as video, cartography and medical applications.

Functional Brachyury Binding Sites Establish a Temporal Read-out of Gene Expression in the Ciona Notochord

PubMed Central

Passamaneck, Yale J.; Gazdoiu, Stefan; José-Edwards, Diana S.; Kugler, Jamie E.; Oda-Ishii, Izumi; Imai, Janice H.; Nibu, Yutaka; Di Gregorio, Anna

2013-01-01

The appearance of the notochord represented a milestone in Deuterostome evolution. The notochord is necessary for the development of the chordate body plan and for the formation of the vertebral column and numerous organs. It is known that the transcription factor Brachyury is required for notochord formation in all chordates, and that it controls transcription of a large number of target genes. However, studies of the structure of the cis-regulatory modules (CRMs) through which this control is exerted are complicated in vertebrates by the genomic complexity and the pan-mesodermal expression territory of Brachyury. We used the ascidian Ciona, in which the single-copy Brachyury is notochord-specific and CRMs are easily identifiable, to carry out a systematic characterization of Brachyury-downstream notochord CRMs. We found that Ciona Brachyury (Ci-Bra) controls most of its targets directly, through non-palindromic binding sites that function either synergistically or individually to activate early- and middle-onset genes, respectively, while late-onset target CRMs are controlled indirectly, via transcriptional intermediaries. These results illustrate how a transcriptional regulator can efficiently shape a shallow gene regulatory network into a multi-tiered transcriptional output, and provide insights into the mechanisms that establish temporal read-outs of gene expression in a fast-developing chordate embryo. PMID:24204212

Functional Brachyury binding sites establish a temporal read-out of gene expression in the Ciona notochord.

PubMed

Katikala, Lavanya; Aihara, Hitoshi; Passamaneck, Yale J; Gazdoiu, Stefan; José-Edwards, Diana S; Kugler, Jamie E; Oda-Ishii, Izumi; Imai, Janice H; Nibu, Yutaka; Di Gregorio, Anna

2013-10-01

The appearance of the notochord represented a milestone in Deuterostome evolution. The notochord is necessary for the development of the chordate body plan and for the formation of the vertebral column and numerous organs. It is known that the transcription factor Brachyury is required for notochord formation in all chordates, and that it controls transcription of a large number of target genes. However, studies of the structure of the cis-regulatory modules (CRMs) through which this control is exerted are complicated in vertebrates by the genomic complexity and the pan-mesodermal expression territory of Brachyury. We used the ascidian Ciona, in which the single-copy Brachyury is notochord-specific and CRMs are easily identifiable, to carry out a systematic characterization of Brachyury-downstream notochord CRMs. We found that Ciona Brachyury (Ci-Bra) controls most of its targets directly, through non-palindromic binding sites that function either synergistically or individually to activate early- and middle-onset genes, respectively, while late-onset target CRMs are controlled indirectly, via transcriptional intermediaries. These results illustrate how a transcriptional regulator can efficiently shape a shallow gene regulatory network into a multi-tiered transcriptional output, and provide insights into the mechanisms that establish temporal read-outs of gene expression in a fast-developing chordate embryo.

Efficient recovery of the functional IP10-scFv fusion protein from inclusion bodies with an on-column refolding system.

PubMed

Guo, Jun-Qing; Li, Qing-Mei; Zhou, Ji-Yong; Zhang, Gai-Ping; Yang, Yan-Yan; Xing, Guang-Xu; Zhao, Dong; You, Shang-You; Zhang, Chu-Yu

2006-01-01

A functional IP10-scFv fusion protein retaining the antibody specificity for acidic isoferritin and chemokine function was produced at high level in Esherichia coli (E. coli). IP10-scFv gene from the recombinant plasmid pc3IP104c9 was subcloned into pET28a fused to N-terminal His-tag sequence in frame and overexpressed in E. coli BL21(DE3). With an on-column refolding procedure based on Ni-chelating chromatography, the active fusion protein was recovered efficiently from inclusion bodies with a refolding yield of approximate 45% confirmed by spectrophotometer. The activity of refolded IP10-scFv was determined through sodium dodecyl sulfate-polyacrylamide gel electrophoresis, Western blotting and enzyme-linked immunosorbent assay. The results showed the fusion protein retains the specific binding activity to AIF with an affinity constant of 4.48x10(-8) M as well as the chemokine function of IP-10. The overall yield of IP10-scFv with bioactivity in E. coli flask culture was more than 40 mg/L.

Development of an on-column enrichment technique based on C18-functionalized magnetic silica nanoparticles for the determination of lidocaine in rat plasma by high performance liquid chromatography.

PubMed

Chu, Bin; Lou, Dujuan; Yu, Panfeng; Hu, Shaonan; Shen, Shun

2011-10-14

In this study, a novel on-column enrichment technique filled with C(18)-functionalized magnetic silica nanoparticles was successfully developed for the determination of lidocaine in rat plasma by high performance liquid chromatography (HPLC). The synthesized Fe(3)O(4)@SiO(2)-C(18) nanoparticles were locally packed into the capillary by the application of magnets. Lidocaine in the sample solutions pumped into the capillary tube could be easily adsorbed by Fe(3)O(4)@SiO(2)-C(18) through hydrophobic interaction by the interior C(18) groups, and eluted by acetonitrile solution. Different extraction conditions were investigated. Method validations including linear range, quantification limit, detection limit, precision, accuracy and recovery were also studied. The results showed that the proposed method based on on-column enrichment by Fe(3)O(4)@SiO(2)-C(18) was a novel, little solvent and efficient approach for the determination of lidocaine in the complex plasma samples. Copyright © 2011 Elsevier B.V. All rights reserved.

Ureic nitrogen transformation in multi-layer soil columns treated with urease and nitrification inhibitors.

PubMed

Giovannini, Camilla; Garcia-Mina, Josè M; Ciavatta, Claudio; Marzadori, Claudio

2009-06-10

The use of N-(n-butyl)thiophosphoric triamide (NBPT), as a urease inhibitor, is one of the most successful strategies utilized to increase the efficiency of urea-based fertilization. To date, NBPT has been added to the soil incorporated in fertilizers containing either urea or the inhibitor at a fixed percentage on the urea weight. The possibility of using NBPT physically separated from urea-based fertilizers could make its use more flexible. In particular, a granulated product containing NBPT could be utilized in soils treated with different urea-based fertilizers including livestock urine, the amount depending on soil characteristics and/or the urea source (e.g., mineral fertilizer, organo-mineral fertilizer, or animal slurry). In this study, a multilayer soil column device was used to investigate the influence of an experimental granular product (RV) containing NBPT and a garlic extract, combining the ability to protect NBPT by oxidation and nitrification inhibition activity, on (a) spatial variability of soil urease and nitrification activities and (b) timing of urea hydrolysis and mineral-N form accumulation (NO(2)(-), NO(3)(-), NH(4)(+)) in soil treated with urea. The results clearly demonstrated that RV can, effectively, inhibit the soil urease activity along the soil column profile up to 8-10 cm soil layer depth and that the inhibition power of RV was dependent on time and soil depth. However, nitrification activity is not significantly influenced by RV addition. In addition, the soil N transformations were clearly affected by RV; in fact, RV retarded urea hydrolysis and reduced the accumulation of NH(4)(+)-N and NO(2)(-)-N ions along the soil profile. The RV product was demonstrated to be an innovative additive able to modify some key ureic N trasformation processes correlated with the efficiency of the urea-based fertilization, in a soil column higher than 10 cm.

Natural attenuation and biosurfactant-stimulated bioremediation of estuarine sediments contaminated with diesel oil.

PubMed

Bayer, Débora M; Chagas-Spinelli, Alessandra C O; Gavazza, Sávia; Florencio, Lourdinha; Kato, Mario T

2013-09-01

We evaluated the bioremediation, by natural attenuation (NA) and by natural attenuation stimulated (SNA) using a rhamnolipid biosurfactant, of estuarine sediments contaminated with diesel oil. Sediment samples (30 cm) were put into 35 cm glass columns, and the concentrations of the 16 polycyclic aromatic hydrocarbons (PAHs) prioritized by the US Environmental Protection Agency were monitored for 111 days. Naphthalene percolated through the columns more than the other PAHs, and, in general, the concentrations of the lower molecular weight PAHs, consisting of two and three aromatic rings, changed during the first 45 days of treatment, whereas the concentrations of the higher molecular weight PAHs, consisting of four, five, and six rings, were more stable. The higher molecular weight PAHs became more available after 45 days, in the deeper parts of the columns (20-30 cm). Evidence of degradation was observed only for some compounds, such as pyrene, with a total removal efficiency of 82 and 78 % in the NA and SNA treatments, respectively, but without significant difference. In the case of total PAH removal, the efficiencies were significantly different of 82 and 67 %, respectively.

Preparation and evaluation of surface-bonded tricationic ionic liquid silica as stationary phases for high-performance liquid chromatography.

PubMed

Qiao, Lizhen; Shi, Xianzhe; Lu, Xin; Xu, Guowang

2015-05-29

Two tricationic ionic liquids were prepared and then bonded onto the surface of supporting silica materials through "thiol-ene" click chemistry as new stationary phases for high-performance liquid chromatography. The obtained columns of tricationic ionic liquids were evaluated respectively in the reversed-phase liquid chromatography (RPLC) mode and hydrophilic interaction liquid chromatography (HILIC) mode, and possess ideal column efficiency of 80,000 plates/m in the RPLC mode with naphthalene as the test solute. The tricationic ionic liquid stationary phases exhibit good hydrophobic and shape selectivity to hydrophobic compounds, and RPLC retention behavior with multiple interactions. In the HILIC mode, the retention and selectivity were evaluated through the efficient separation of nucleosides and bases as well as flavonoids, and the typical HILIC retention behavior was demonstrated by investigating retention changes of hydrophilic solutes with water volume fraction in mobile phase. The results show that the tricationic ionic liquid columns possess great prospect for applications in analysis of hydrophobic and hydrophilic samples. Copyright © 2015 Elsevier B.V. All rights reserved.

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

PubMed

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

2017-05-01

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

Ammoniacal nitrogen and COD removal from semi-aerobic landfill leachate using a composite adsorbent: fixed bed column adsorption performance.

PubMed

Halim, Azhar Abdul; Aziz, Hamidi Abdul; Johari, Megat Azmi Megat; Ariffin, Kamar Shah; Adlan, Mohd Nordin

2010-03-15

The performance of a carbon-mineral composite adsorbent used in a fixed bed column for the removal of ammoniacal nitrogen and aggregate organic pollutant (COD), which are commonly found in landfill leachate, was evaluated. The breakthrough capacities for ammoniacal nitrogen and COD adsorption were 4.46 and 3.23 mg/g, respectively. Additionally, the optimum empty bed contact time (EBCT) was 75 min. The column efficiency for ammoniacal nitrogen and COD adsorption using fresh adsorbent was 86.4% and 92.6%, respectively, and these values increased to 90.0% and 93.7%, respectively, after the regeneration process. (c) 2009 Elsevier B.V. All rights reserved.

Improving membrane protein expression by optimizing integration efficiency

PubMed Central

2017-01-01

The heterologous overexpression of integral membrane proteins in Escherichia coli often yields insufficient quantities of purifiable protein for applications of interest. The current study leverages a recently demonstrated link between co-translational membrane integration efficiency and protein expression levels to predict protein sequence modifications that improve expression. Membrane integration efficiencies, obtained using a coarse-grained simulation approach, robustly predicted effects on expression of the integral membrane protein TatC for a set of 140 sequence modifications, including loop-swap chimeras and single-residue mutations distributed throughout the protein sequence. Mutations that improve simulated integration efficiency were 4-fold enriched with respect to improved experimentally observed expression levels. Furthermore, the effects of double mutations on both simulated integration efficiency and experimentally observed expression levels were cumulative and largely independent, suggesting that multiple mutations can be introduced to yield higher levels of purifiable protein. This work provides a foundation for a general method for the rational overexpression of integral membrane proteins based on computationally simulated membrane integration efficiencies. PMID:28918393

Cryogenic distillation facility for isotopic purification of protium and deuterium

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

Alekseev, I.; Arkhipov, Ev.; Bondarenko, S.

Isotopic purification of the protium and deuterium is an important requirement of many physics experiments. A cryogenic facility for high-efficiency separation of hydrogen isotopes with a cryogenic distillation column as the main element is described. The instrument is portable, so that it can be used at the experimental site. It was designed and built at the Petersburg Nuclear Physics Institute, Gatchina, Russia. Fundamental operating parameters have been measured including a liquid holdup in the column packing, the pressure drops across the column and the purity of the product at different operating modes. A mathematical model describes expected profiles of hydrogenmore » isotope concentration along the distillation column. An analysis of ortho-parahydrogen isomeric composition by gas chromatography was used for evaluation of the column performance during the tuning operations. The protium content during deuterium purification (≤100 ppb) was measured using gas chromatography with accumulation of the protium in the distillation column. A high precision isotopic measurement at the Institute of Particle Physics, ETH-Zurich, Switzerland, provided an upper bound of the deuterium content in protium (≤6 ppb), which exceeds all commercially available products.« less

Preparation and evaluation of open-tubular capillary columns modified with metal-organic framework incorporated polymeric porous layer for liquid chromatography.

PubMed

Zhu, Manman; Zhang, Lingyi; Chu, Zhanying; Wang, Shulei; Chen, Kai; Zhang, Weibing; Liu, Fan

2018-07-01

An open tubular capillary liquid phase chromatographic column (1 m × 25 µm i.d.× 375 µm o.d.) was prepared by incorporating metal organic framework particles modified with vancomycin directly into zwitterionic polymer coating synthesized by the copolymerization of [2-(methacryloyloxy)ethyl]dimethyl-(3-sulfopropyl) ammonium hydroxide and N,N'-methylenebisacrylamide. The incorporation of IRMOF-3 (isoreticular metal organic framework-3) particles improved selectivity of zwitterionic polymer coating with absolute column efficiency reaching 79900 plates for p-xylene. Besides strong hydrophilic interaction, the separation of neutral, basic, and acidic compounds demonstrates that π-π stacking interaction and the coordination effect of unsaturated Zn 2+ of MOF also contribute to separation of various analytes. The RSD values (run-to-run, day-to-day, column-to-column, n = 3) of retention time of neutral compounds were less than 0.71%, 0.69% and 3.08% respectively, suggesting good repeatability. In addition, the column was applied to the analysis of the trypsin digest of bovine serum albumin, revealing the potential in separating biological samples. Copyright © 2018 Elsevier B.V. All rights reserved.

Hollow Fibers Structured Packings in Olefin/Paraffin Distillation: Apparatus Scale-Up and Long-Term Stability

DOE PAGES

Yang, Dali; Le, Loan; Martinez, Ronald; ...

2013-06-21

Following the conceptual demonstration of high separation efficiency and column capacity obtained in olefin/paraffin distillation using hollow fiber structured packings (HFSPs) in a bench scale (J. Membr. Sci.2006, 2007, and 2010), we scaled-up this process with a 10-fold increase in the internal flow rate and a 3-fold increase in the module length. We confirmed that the HFSPs technology gives high separation efficiency and column capacity in iso-/n-butane distillation for 18 months. We systematically investigated the effects of packing density, concentration of light component, reflux ratio, and module age on the separation efficiency and operating stability. The comprehensive characterizations using scanningmore » electron microscopy (SEM), Brunauer–Emmett–Teller (BET), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), and dynamic mechanical analysis (DMA) were carried out to probe the changes in the morphological, thermal, and mechanical properties of polypropylene (PP) hollow fibers over the aging process. Our results suggest that after a long-term exposure to light hydrocarbon environments at ≤70 °C the morphological and mechanical properties of the PP polymer do not degrade significantly in a propane/propylene and iso-/n-butane environment.« less

Transport of biocolloids in water saturated columns packed with sand: Effect of grain size and pore water velocity

NASA Astrophysics Data System (ADS)

Syngouna, Vasiliki I.; Chrysikopoulos, Constantinos V.

2012-03-01

The main objective of this study was to evaluate the combined effects of grain size and pore water velocity on the transport in water saturated porous media of three waterborne fecal indicator organisms (Escherichia coli, MS2, and ΦX174) in laboratory-scale columns packed with clean quartz sand. Three different grain sizes and three pore water velocities were examined and the attachment behavior of Escherichia coli, MS2, and ΦX174 onto quartz sand was evaluated. The mass recoveries of the biocolloids examined were shown to be highest for Escherichia coli and lowest for MS2. However, no obvious relationships between mass recoveries and water velocity or grain size could be established from the experimental results. The observed mean dispersivity values for each sand grain size were smaller for bacteria than coliphages, but higher for MS2 than ΦX174. The single collector removal and collision efficiencies were quantified using the classical colloid filtration theory. Furthermore, theoretical collision efficiencies were estimated only for E. coli by the Interaction-Force-Boundary-Layer, and Maxwell approximations. Better agreement between the experimental and Maxwell theoretical collision efficiencies were observed.

Transport of biocolloids in water saturated columns packed with sand: Effect of grain size and pore water velocity

NASA Astrophysics Data System (ADS)

Syngouna, Vasiliki I.; Chrysikopoulos, Constantinos V.

2011-11-01

The main objective of this study was to evaluate the combined effects of grain size and pore water velocity on the transport in water saturated porous media of three waterborne fecal indicator organisms ( Escherichia coli, MS2, and ΦX174) in laboratory-scale columns packed with clean quartz sand. Three different grain sizes and three pore water velocities were examined and the attachment behavior of Escherichia coli, MS2, and ΦX174 onto quartz sand was evaluated. The mass recoveries of the biocolloids examined were shown to be highest for Escherichia coli and lowest for MS2. However, no obvious relationships between mass recoveries and water velocity or grain size could be established from the experimental results. The observed mean dispersivity values for each sand grain size were smaller for bacteria than coliphages, but higher for MS2 than ΦX174. The single collector removal and collision efficiencies were quantified using the classical colloid filtration theory. Furthermore, theoretical collision efficiencies were estimated only for E. coli by the Interaction-Force-Boundary-Layer, and Maxwell approximations. Better agreement between the experimental and Maxwell theoretical collision efficiencies were observed.

Computing rank-revealing QR factorizations of dense matrices.

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

Bischof, C. H.; Quintana-Orti, G.; Mathematics and Computer Science

1998-06-01

We develop algorithms and implementations for computing rank-revealing QR (RRQR) factorizations of dense matrices. First, we develop an efficient block algorithm for approximating an RRQR factorization, employing a windowed version of the commonly used Golub pivoting strategy, aided by incremental condition estimation. Second, we develop efficiently implementable variants of guaranteed reliable RRQR algorithms for triangular matrices originally suggested by Chandrasekaran and Ipsen and by Pan and Tang. We suggest algorithmic improvements with respect to condition estimation, termination criteria, and Givens updating. By combining the block algorithm with one of the triangular postprocessing steps, we arrive at an efficient and reliablemore » algorithm for computing an RRQR factorization of a dense matrix. Experimental results on IBM RS/6000 SGI R8000 platforms show that this approach performs up to three times faster that the less reliable QR factorization with column pivoting as it is currently implemented in LAPACK, and comes within 15% of the performance of the LAPACK block algorithm for computing a QR factorization without any column exchanges. Thus, we expect this routine to be useful in may circumstances where numerical rank deficiency cannot be ruled out, but currently has been ignored because of the computational cost of dealing with it.« less

Effect of pH on bacteriophage transport through sandy soils

USGS Publications Warehouse

Kinoshita, Takashi; Bales, Roger C.; Maguire, Kimberley M.; Gerba, Charles P.

1993-01-01

Effects of pH and hydrophobicity on attachment and detachment of PRD-1 and MS-2 in three different sandy soils were investigated in a series of laboratory-column experiments. Concentrations of the lipid-containing phage PRD-1 decreased 3–4 orders of magnitude during passage through the 10–15-cm-long columns. Attachment of the lipid-containing phage PRD-1 was insensitive to pH and was apparently controlled by hydrophobic interactions in soil media. The less-hydrophobic phage MS-2 acted conservatively; it was not removed in the columns at pH's 5.7–8.0. The sticking efficiency (α) in a colloid-filtration model was between 0.1 and 1 for PRD-1, indicating a relatively high removal efficiency. Phage attachment was reversible, but detachment under steady-state conditions was slow. An increase in pH had a moderate effect on enhancing detachment. Still, these soils should continue to release phage to virus-free water for days to weeks following exposure to virus-containing water. In sandy soils with a mass-fraction organic carbon as low as a few hundredths of a percent, pH changes in the range 5.7–8.0 should have little effect on retention of more-hydrophobic virus (e.g., PRD-1), in that retardation will be dominated by hydrophobic effects. Sharp increases in pH should enhance detachment and transport of virus previously deposited on soil grains. A more hydrophilic virus (e.g., MS-2) will transport as a conservative tracer in low-carbon sandy soil.

[Application of general retention time formula for gradient liquid chromatography in the studies of ladder-like gradient elution].

PubMed

Sun, Xiaoli; Hao, Weiqiang; Wang, Junde; Di, Bin; Chen, Qiang; Zhuang, Wei; Yu, Qiang; Zhang, Peipei

2013-08-01

By not explicitly specifying the type of solvent strength model, the features of ladder-like gradient elution were studied based on the general retention time formula that was derived in our previous work. For the case where the solute is eluted at like gradient, we derived the expression that connects the mobile phase composition (phiR), at which the solute is eluted from the column, with the gradient slope (B). It was shown that phiR will increase with the increase of B in this case. For the case where the solute is eluted at the last isocratic segment of the ladder-like gradient, it was proven that the retention time (tR) will correlate linearly with the reciprocal of the gradient slope (1/B) when the initial and final mobile phase compositions are set to be constant. In experiments, by taking biphenyl as the sample, the values of retention time in isocratic and gradient elution were measured on a C18 column by using a mixture of methanol and water as the mobile phase. The experimental values were found to be well consistent with the theoretical values that were calculated from the expressions. These expressions will be helpful to understand the features of the ladder-like gradient in practice.

A biofilter integrated with gas membrane separation unit for the treatment of fluctuating styrene loads.

PubMed

Li, Lin; Lian, Jing; Han, Yunping; Liu, Junxin

2012-05-01

Biofiltration for volatile organic compound control in waste gas streams is best operated at steady contaminant loadings. To provide long-term stable operation of a biofilter under adverse contaminant feeding conditions, an integrated bioreactor system with a gas separation membrane module installed after a biofilter was proposed for styrene treatment. Styrene was treated effectively, with average styrene effluent concentrations maintained at less than 50 mg m(-3) and a total removal efficiency of over 96% achieved when the biofiltration column faced fluctuating loads. The maximum elimination capacity of the integrated bioreactor system was 93.8 g m(-3)h(-1), which was higher than that obtained with the biofiltration column alone. The combination of these two processes (microbial and chemical) led to more efficient elimination of styrene and buffering of the fluctuating loads. The factors on gas membrane separation, microbial characteristics in the integrated bioreactor and membrane fouling were also investigated in this study. Copyright © 2012 Elsevier Ltd. All rights reserved.

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

PubMed

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

2009-02-06

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

Towards a method of rapid extraction of strontium-90 from urine: urine pretreatment and alkali metal removal

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

Hawkins, C.; Dietz, M.; Kaminski, M.

2016-03-01

A technical program to support the Centers of Disease Control and Prevention is being developed to provide an analytical method for rapid extraction of Sr-90 from urine, with the intent of assessing the general population’s exposure during an emergency response to a radiological terrorist event. Results are presented on the progress in urine sample preparation and chemical separation steps that provide an accurate and quantitative detection of Sr-90 based upon an automated column separation sequence and a liquid scintillation assay. Batch extractions were used to evaluate the urine pretreatment and the column separation efficiency and loading capacity based upon commercial,more » extractant-loaded resins. An efficient pretreatment process for decolorizing and removing organics from urine without measurable loss of radiostrontium from the sample was demonstrated. In addition, the Diphonix® resin shows promise for the removal of high concentrations of common strontium interferents in urine as a first separation step for Sr-90 analysis.« less

Rapid Column-Free Enrichment of Mononuclear Cells from Solid Tissues

PubMed Central

Scoville, Steven D.; Keller, Karen A.; Cheng, Stephanie; Zhang, Michael; Zhang, Xiaoli; Caligiuri, Michael A.; Freud, Aharon G.

2015-01-01

We have developed a rapid negative selection method to enrich rare mononuclear cells from human tissues. Unwanted and antibody-tethered cells are selectively depleted during a Ficoll separation step, and there is no need for magnetic-based reagents and equipment. The new method is fast, customizable, inexpensive, remarkably efficient, and easy to perform, and per sample the overall cost is less than one-tenth the cost associated with a magnetic column-based method. PMID:26223896

Investigating the efficiency of microscale zero valent iron-based in situ reactive zone (mZVI-IRZ) for TCE removal in fresh and saline groundwater.

PubMed

Xin, Jia; Tang, Fenglin; Yan, Jing; La, Chenghong; Zheng, Xilai; Liu, Wei

2018-06-01

In this study, long-term column experiments were conducted in three media (Milli-Q water, fresh groundwater and saline groundwater) to evaluate the trichloroethylene (TCE) removal performance, electron efficiency (EE), and permeability loss of a microscale zero valent iron-based in situ reactive zone (mZVI-IRZ) under different field conditions. A potential scenario of in situ contamination plume remediation was simulated by adding a TCE-containing influent to columns filled with mixed mZVI particles and silica sand at a flow rate of 4 mL h -1 for 6 months. Results showed that, over the course of 100 pore volumes (PV) for 6 months, mZVI displayed the lowest TCE breakthrough rate (0.0026 PV -1 ) and highest TCE removal capacity (43.72 mg) but the poorest EE value (25-40%) in saline groundwater. Mineral characterization (SEM, XRD), ion concentration analysis, and geochemical modeling corroborated that different dominant solid precipitates (magnetite, siderite, dolomite/magnetite) were identified inside the three columns. The column containing saline groundwater experienced the greatest porosity loss, approximately 30.23 mL over the course of 100 PVs. This study illustrates that, to improve designs of mZVI-IRZs, EE as well as hydraulic conductivity should be taken into consideration for predictive evaluations. Copyright © 2018 Elsevier B.V. All rights reserved.

In situ preparation of multilayer coated capillary column with HKUST-1 for separation of neutral small organic molecules by open tubular capillary electrochromatography.

PubMed

Xu, Yin-Yin; Lv, Wen-Juan; Ren, Cui-Ling; Niu, Xiao-Ying; Chen, Hong-Li; Chen, Xing-Guo

2018-01-12

The popularity of novel nanoparticles coated capillary column has aroused widespread attention of researchers. Metal organic frameworks (MOFs) with special structure and chemical properties have received great interest in separation sciences. This work presents the investigation of HKUST-1 (Hong Kong University of Science and Technology-1, called Cu 3 (BTC) 2 or MOF-199) nanoparticles as a new type of coating material for capillary electrochromatography. For the first time, three layers coating (3-LC), five layers coating (5-LC), ten layers coating (10-LC), fifteen layers coating (15-LC), twenty layers coating(20-LC) and twenty-five layers coating (25-LC) capillary columns coated with HKUST-1 nanoparticles were synthesized by covalent bond with in situ, layer-by-layer self-assembly approach. The results of scanning electron microscopy (SEM), X-ray diffraction (XRD) and plasma atomic emission spectrometry (ICP-AES) indicated that HKUST-1 was successfully grafted on the inner wall of the capillary. The separating performances of 3-LC, 5-LC, 10-LC, 15-LC, 20-LC and 25-LC open tubular (OT) capillary columns were studied with some neutral small organic molecules. The results indicated that the neutral small organic molecules were separated successfully with 10-LC, 15-LC and 20-LC OT capillary columns because of the size selectivity of lattice aperture and hydrophobicity of organic ligands. In addition, 10-LC and 15-LC OT capillary columns showed better performance for the separation of certain phenolic compounds. Furthermore, 10-LC, 15-LC and 20-LC OT capillary columns exhibited good intra-day repeatability with the relative standard deviations (RSDs; %) of migration time and peak areas lying in the range of 0.3-1.2% and 0.5-4.2%, respectively. For inter-day reproducibility, the RSDs of the three OT capillary columns were found to be lying in the range of 0.3-5.5% and 0.3-4.5% for migration time and peak area, respectively. The RSDs of retention times for column-to-column for three batches of 10-LC, 15-LC and 20-LC OT capillary columns were in the range from 2.3% to 7.2%. Moreover, the fabricated 10-LC, 15-LC and 20-LC OT capillary columns exhibited good repeatability and stability for separation, which could be used successively for more than 120 runs with no observable changes on the separation efficiency. Copyright © 2017 Elsevier B.V. All rights reserved.

Modeling of Cr(VI) Bioreduction Under Fermentative and Denitrifying Conditions

NASA Astrophysics Data System (ADS)

Molins, S.; Steefel, C.; Yang, L.; Beller, H. R.

2011-12-01

The mechanisms of bioreductive immobilization of Cr(VI) were investigated by reactive transport modeling of a set of flow-through column experiments performed using natural Hanford 100H aquifer sediment. The columns were continuously eluted with 5 μM Cr(VI), 5 mM lactate as the electron donor, and selected electron acceptors (tested individually). Here we focus on the two separate experimental conditions that showed the most removal of Cr(VI) from solution: fermentation and denitrification. In each case, a network of enzymatic and abiotic reaction pathways was considered to interpret the rate of chromate reduction. The model included biomass growth and decay, and thermodynamic limitations on reaction rates, and was constrained by effluent concentrations measured by IC and ICP-MS and additional information from bacterial isolates from column effluent. Under denitrifying conditions, Cr(VI) reduction was modeled as co-metabolic with nitrate reduction based on experimental observations and previous studies on a denitrifying bacterium derived from the Hanford 100H aquifer. The reactive transport model results supported this interpretation of the reaction mechanism and were used to quantify the efficiency of the process. The models results also suggest that biomass growth likely relied on a nitrogen source other than ammonium (e.g. nitrate). Under fermentative conditions and based on cell suspension studies performed on a bacterial isolate from the columns, the model assumes that Cr(VI) reduction is carried out directly by fermentative bacteria that convert lactate into acetate and propionate. The evolution to complete lactate fermentation and Cr(VI) reduction took place over a week's time and simulations were used to determine an estimate for a lower limit of the rate of chromate reduction by calibration with the flow-through column experimental results. In spite of sulfate being added to these columns, sulfate reduction proceeded at a slow rate and was not well constrained.

Generation of surface-wave microwave microplasmas in hollow-core photonic crystal fiber based on a split-ring resonator.

PubMed

Vial, Florian; Gadonna, Katell; Debord, Benoît; Delahaye, Frédéric; Amrani, Foued; Leroy, Olivier; Gérôme, Frédéric; Benabid, Fetah

2016-05-15

We report on a new and highly compact scheme for the generation and sustainment of microwave-driven plasmas inside the core of an inhibited coupling Kagome hollow-core photonic crystal fiber. The microwave plasma generator consists of a split-ring resonator that efficiently couples the microwave field into the gas-filled fiber. This coupling induces the concomitant generation of a microwave surface wave at the fiber core surround and a stable plasma column confined in the fiber core. The scheme allowed the generation of several centimeters long argon microplasma columns with a very low excitation power threshold. This result represents an important step toward highly compact plasma lasers or plasma-based photonic components.

Effects of reflux ratio and feed conditions for the purification of bioethanol in a continuous distillation column

NASA Astrophysics Data System (ADS)

Dasan, Y. K.; Abdullah, M. A.; Bhat, A. H.

2014-10-01

Continuous distillation column was used for the purification of bioethanol from fermentation of molasses using Saccharomyces cerevisia. Bioethanol produced was at 8.32% (v/v) level. The efficiency of continuous distillation process was evaluated based on reflux ratio, and feed condition. The lab results were validated using COFE simulation Software. The analyses showed that both reflux ratio and feed condition had significant effects on the distillation process. Stages increased from 1.79 to 2.26 as the reflux ratio was decreased from 90% to 45% and the saturated feed produced lower mole fraction of desired product. We concluded that the lower reflux ratio with cold feed condition was suitable for higher mole fraction of top product.

A Novel Crosstalk Suppression Method of the 2-D Networked Resistive Sensor Array

PubMed Central

Wu, Jianfeng; Wang, Lei; Li, Jianqing; Song, Aiguo

2014-01-01

The 2-D resistive sensor array in the row–column fashion suffered from the crosstalk problem for parasitic parallel paths. Firstly, we proposed an Improved Isolated Drive Feedback Circuit with Compensation (IIDFCC) based on the voltage feedback method to suppress the crosstalk. In this method, a compensated resistor was specially used to reduce the crosstalk caused by the column multiplexer resistors and the adjacent row elements. Then, a mathematical equivalent resistance expression of the element being tested (EBT) of this circuit was analytically derived and verified by the circuit simulations. The simulation results show that the measurement method can greatly reduce the influence on the EBT caused by parasitic parallel paths for the multiplexers' channel resistor and the adjacent elements. PMID:25046011

Dissolved organic matter removal during coal slag additive soil aquifer treatment for secondary effluent recharging: Contribution of aerobic biodegradation.

PubMed

Wei, Liangliang; Li, Siliang; Noguera, Daniel R; Qin, Kena; Jiang, Junqiu; Zhao, Qingliang; Kong, Xiangjuan; Cui, Fuyi

2015-06-01

Recycling wastewater treatment plant (WWTP) effluent at low cost via the soil aquifer treatment (SAT), which has been considered as a renewable approach in regenerating potable and non-potable water, is welcome in arid and semi-arid regions throughout the world. In this study, the effect of a coal slag additive on the bulk removal of the dissolved organic matter (DOM) in WWTP effluent during SAT operation was explored via the matrix configurations of both coal slag layer and natural soil layer. Azide inhibition and XAD-resins fractionation experiments indicated that the appropriate configuration designing of an upper soil layer (25 cm) and a mixture of soil/coal slag underneath would enhance the removal efficiency of adsorption and anaerobic biodegradation to the same level as that of aerobic biodegradation (31.7% vs 32.2%), while it was only 29.4% compared with the aerobic biodegradation during traditional 50 cm soil column operation. The added coal slag would preferentially adsorb the hydrophobic DOM, and those adsorbed organics could be partially biodegraded by the biomass within the SAT systems. Compared with the relatively lower dissolved organic carbon (DOC), ultraviolet light adsorption at 254 nm (UV-254) and trihalomethane formation potential (THMFP) removal rate of the original soil column (42.0%, 32.9%, and 28.0%, respectively), SSL2 and SSL4 columns would enhance the bulk removal efficiency to more than 60%. Moreover, a coal slag additive in the SAT columns could decline the aromatic components (fulvic-like organics and tryptophan-like proteins) significantly. Copyright © 2015 Elsevier Ltd. All rights reserved.

Removal of micropollutants during tertiary wastewater treatment by biofiltration: Role of nitrifiers and removal mechanisms.

PubMed

Rattier, M; Reungoat, J; Keller, J; Gernjak, W

2014-05-01

The objective of this study was to determine the extent to which a suite of organic micropollutants (MPs) can be removed by biological filtration and the role of bioavailability and ammonia oxidizing microorganisms (AOMs) in the biodegradation process. During approximately one year, laboratory-scale columns with 8 min empty bed contact time (EBCT) and packed with anthracite as filter media were used for treating a tertiary effluent spiked with a broad range of MPs at a target concentration of 2 μg L(-1). In parallel columns, aerobic biomass growth was inhibited by using either the biocide sodium azide (500 mg L(-1) NaN3) or allylthiourea (5 mg L(-1) ATU), specifically inhibiting nitrifying bacteria. Once the biomass had colonized the media, around 15% of the dissolved organic carbon (DOC) contained in the untreated tertiary effluent was removed by non-inhibited columns. The removal of several MPs increased over time indicating the relevance of biological activity for the removal of MPs, while the negative control, the NaN3 inhibited column, showed no significant removal. Out of 33 MPs, 19 were recalcitrant (<25%) to biodegradation under aerobic conditions with the others exhibiting a diverse range of removal efficiency up to 95%. Through inhibition by ATU it was shown that nitrifying bacteria were clearly having a role in the degradation of several MPs, whereas the removal of other MPs was not affected by the presence of the nitrification inhibitor. A relationship between the qualitative assessment of sorption of MPs on granular activated carbon (GAC) and their removal efficiency by biodegradation on anthracite was observed. This result suggested that the affinity of the MPs for GAC media could be a useful indicator of the bioavailability of compounds during biofiltration on anthracite. Copyright © 2014 Elsevier Ltd. All rights reserved.

Expression of growth differentiation factor 6 in the human developing fetal spine retreats from vertebral ossifying regions and is restricted to cartilaginous tissues.

PubMed

Wei, Aiqun; Shen, Bojiang; Williams, Lisa A; Bhargav, Divya; Gulati, Twishi; Fang, Zhimin; Pathmanandavel, Sarennya; Diwan, Ashish D

2016-02-01

During embryogenesis vertebral segmentation is initiated by sclerotomal cell migration and condensation around the notochord, forming anlagen of vertebral bodies and intervertebral discs. The factors that govern the segmentation are not clear. Previous research demonstrated that mutations in growth differentiation factor 6 resulted in congenital vertebral fusion, suggesting this factor plays a role in development of vertebral column. In this study, we detected expression and localization of growth differentiation factor 6 in human fetal spinal column, especially in the period of early ossification of vertebrae and the developing intervertebral discs. The extracellular matrix proteins were also examined. Results showed that high levels of growth differentiation factor 6 were expressed in the nucleus pulposus of intervertebral discs and the hypertrophic chondrocytes adjacent to the ossification centre in vertebral bodies, where strong expression of proteoglycan and collagens was also detected. As fetal age increased, the expression of growth differentiation factor 6 was decreased correspondingly with the progress of ossification in vertebral bodies and restricted to cartilaginous regions. This expression pattern and the genetic link to vertebral fusion suggest that growth differentiation factor 6 may play an important role in suppression of ossification to ensure proper vertebral segmentation during spinal development. © 2015 Orthopaedic Research Society. Published by Wiley Periodicals, Inc.

Human granulocyte colony stimulating factor (hG-CSF): cloning, overexpression, purification and characterization.

PubMed

Vanz, Ana Ls; Renard, Gaby; Palma, Mario S; Chies, Jocelei M; Dalmora, Sérgio L; Basso, Luiz A; Santos, Diógenes S

2008-04-04

Biopharmaceutical drugs are mainly recombinant proteins produced by biotechnological tools. The patents of many biopharmaceuticals have expired, and biosimilars are thus currently being developed. Human granulocyte colony stimulating factor (hG-CSF) is a hematopoietic cytokine that acts on cells of the neutrophil lineage causing proliferation and differentiation of committed precursor cells and activation of mature neutrophils. Recombinant hG-CSF has been produced in genetically engineered Escherichia coli (Filgrastim) and successfully used to treat cancer patients suffering from chemotherapy-induced neutropenia. Filgrastim is a 175 amino acid protein, containing an extra N-terminal methionine, which is needed for expression in E. coli. Here we describe a simple and low-cost process that is amenable to scaling-up for the production and purification of homogeneous and active recombinant hG-CSF expressed in E. coli cells. Here we describe cloning of the human granulocyte colony-stimulating factor coding DNA sequence, protein expression in E. coli BL21(DE3) host cells in the absence of isopropyl-beta-D-thiogalactopyranoside (IPTG) induction, efficient isolation and solubilization of inclusion bodies by a multi-step washing procedure, and a purification protocol using a single cationic exchange column. Characterization of homogeneous rhG-CSF by size exclusion and reverse phase chromatography showed similar yields to the standard. The immunoassay and N-terminal sequencing confirmed the identity of rhG-CSF. The biological activity assay, in vivo, showed an equivalent biological effect (109.4%) to the standard reference rhG-CSF. The homogeneous rhG-CSF protein yield was 3.2 mg of bioactive protein per liter of cell culture. The recombinant protein expression in the absence of IPTG induction is advantageous since cost is reduced, and the protein purification protocol using a single chromatographic step should reduce cost even further for large scale production. The physicochemical, immunological and biological analyses showed that this protocol can be useful to develop therapeutic bioproducts. In summary, the combination of different experimental strategies presented here allowed an efficient and cost-effective protocol for rhG-CSF production. These data may be of interest to biopharmaceutical companies interested in developing biosimilars and healthcare community.

Human granulocyte colony stimulating factor (hG-CSF): cloning, overexpression, purification and characterization

PubMed Central

Vanz, Ana LS; Renard, Gaby; Palma, Mario S; Chies, Jocelei M; Dalmora, Sérgio L; Basso, Luiz A; Santos, Diógenes S

2008-01-01

Background Biopharmaceutical drugs are mainly recombinant proteins produced by biotechnological tools. The patents of many biopharmaceuticals have expired, and biosimilars are thus currently being developed. Human granulocyte colony stimulating factor (hG-CSF) is a hematopoietic cytokine that acts on cells of the neutrophil lineage causing proliferation and differentiation of committed precursor cells and activation of mature neutrophils. Recombinant hG-CSF has been produced in genetically engineered Escherichia coli (Filgrastim) and successfully used to treat cancer patients suffering from chemotherapy-induced neutropenia. Filgrastim is a 175 amino acid protein, containing an extra N-terminal methionine, which is needed for expression in E. coli. Here we describe a simple and low-cost process that is amenable to scaling-up for the production and purification of homogeneous and active recombinant hG-CSF expressed in E. coli cells. Results Here we describe cloning of the human granulocyte colony-stimulating factor coding DNA sequence, protein expression in E. coli BL21(DE3) host cells in the absence of isopropyl-β-D-thiogalactopyranoside (IPTG) induction, efficient isolation and solubilization of inclusion bodies by a multi-step washing procedure, and a purification protocol using a single cationic exchange column. Characterization of homogeneous rhG-CSF by size exclusion and reverse phase chromatography showed similar yields to the standard. The immunoassay and N-terminal sequencing confirmed the identity of rhG-CSF. The biological activity assay, in vivo, showed an equivalent biological effect (109.4%) to the standard reference rhG-CSF. The homogeneous rhG-CSF protein yield was 3.2 mg of bioactive protein per liter of cell culture. Conclusion The recombinant protein expression in the absence of IPTG induction is advantageous since cost is reduced, and the protein purification protocol using a single chromatographic step should reduce cost even further for large scale production. The physicochemical, immunological and biological analyses showed that this protocol can be useful to develop therapeutic bioproducts. In summary, the combination of different experimental strategies presented here allowed an efficient and cost-effective protocol for rhG-CSF production. These data may be of interest to biopharmaceutical companies interested in developing biosimilars and healthcare community. PMID:18394164

Nitrogen oxides in the arctic stratosphere: Implications for ozone abundances. Ph.D. Thesis

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

Slusser, J.R.

1994-01-01

In the high latitude winter stratosphere, NO2 sequesters chlorine compounds which are extremely efficient at destroying ozone. During the nighttime, NO2 reacts with ozone to form N2O5 which acts as a reservoir of NO2. Under heavy aerosol loading, N2O5 may react with water on aerosol surfaces to form HNO3, a reservoir more resistant to photolysis. This heterogeneous reaction results in reduced NO2 concentration when the sun returns at the end of the winter. A spectrograph system has been developed to measure scattered zenith skylight and thereby determine stratospheric NO2 slant column abundance. Conversion of the measured slant column abundance tomore » vertical column abundance requires dividing by the air mass. The air mass is the enhancement in the optical path for the scattered twilight as compared to a vertical path. Air mass values determined using a multiple scattering radiative transfer code have been compared to those derived using a Monte Carlo code and were found to agree to within 6% at a 90 deg solar zenith angle for a stratospheric absorber. Six months of NO2 vertical column abundance measured over Fairbanks during the winter 1992-93 exhibited the daylight diminished and increased as the sunlight hours lengthened. The overall seasonal behavior was similar to high-latitude measurements made in the Southern Hemisphere. The ratios of morning to evening column abundance were consistent with predictions based on gas-phase chemistry. The possible heterogeneous reaction of N2O5 on sulfate aerosols was investigated using FTIR Spectrometer measurements of HNO3 column abundance and lidar determinations of the aerosol profile. Using an estimated N2O5 column abundance and aerosol profile as input to a simple model, significant HNO3 production was expected. No increase in HNO3 column abundance was measured. From this set of data, it was not possible to determine whether significant amounts of N2O5 were converted to HNO3 by this heterogeneous reaction.« less

Preparation and evaluation of silica-UIO-66 composite as liquid chromatographic stationary phase for fast and efficient separation.

PubMed

Yan, Zhiming; Zheng, Jiangnan; Chen, Jinfeng; Tong, Ping; Lu, Minghua; Lin, Zian; Zhang, Lan

2014-10-31

A silica-UIO-66 composite was fabricated by a simple hydrothermal method and then applied as liquid chromatographic stationary phase for fast and efficient separation. X-ray diffraction patterns showed the presence of UIO-66 crystals in the silica-UIO-66 composites; while scanning electron microscope (SEM) images revealed that silica-UIO-66 composites were a homogeneous mixture of silica bead and UIO-66 crystals. A variety of substituted aromatics, chlorobenzene compounds and polycyclic aromatic hydrocarbons (PAHs) were used to evaluate the retention properties of the silica-UIO-66 composite packed column. Under the optimized conditions, baseline separation of ethylbenzene (EB) and styrene was obtained with high resolution and short retention time. In addition, the silica-UIO-66 composite packed column also showed some advantages in separation of positional isomers, with which baseline separation of EB and xylene, chlorotoluene and dichlorobenzene isomers was achieved. Moreover, the retention mechanisms of these compounds were also discussed in detail. The relative standard deviations (RSDs) for the separation of EB and xylene, chlorotoluene and dichlorobenzene isomers, as well as EB and styrene were 0.42-0.9%, 1.0-1.9%, 0.75-2.0%, and 0.9-2.1% for the retention time, peak area, peak height, and half peak width, respectively. The column efficiencies for EB, p-chlorotoluene, p-dichlorobenzene and styrene were 8780, 9060, 9990 and 5130 plates/m. The successful applications suggested high potentials of silica-MOFs composite as stationary phase for fast and efficient liquid chromatography separation. Copyright © 2014 Elsevier B.V. All rights reserved.

Enrichment isolation of adipose-derived stem/stromal cells from the liquid portion of liposuction aspirates with the use of an adherent column.

PubMed

Doi, Kentaro; Kuno, Shinichiro; Kobayashi, Akira; Hamabuchi, Takahisa; Kato, Harunosuke; Kinoshita, Kahori; Eto, Hitomi; Aoi, Noriyuki; Yoshimura, Kotaro

2014-03-01

Adipose-derived stem/progenitor cells (ASCs) are typically obtained from the lipoaspirates; however, a smaller number of ASCs can be isolated without enzymatic digestion from the infranatant liposuction aspirate fluid (LAF). We evaluated the effectiveness of an adherent column, currently used to isolate mesenchymal stromal cells from bone marrow, to isolate LAF cells. We applied peripheral blood (PB), PB mixed with cultured ASCs (PB-ASC), and LAF solution to the column and divided it into two fractions, the adherent (positive) and the non-adherent (negative) fractions. We compared this method with hypotonic hemolysis (lysis) for the red blood cell count, nucleated cells count and cell compositions as well as functional properties of isolated mesenchymal cells. The column effectively removed red blood cells, though the removal efficiency was slightly inferior to hemolysis. After column processing of PB-ASC, 60.5% of ASCs (53.2% by lysis) were selectively collected in the positive fraction, and the negative fraction contained almost no ASCs. After processing of LAF solution, nucleated cell yields were comparable between the column and hemolysis; however, subsequent adherent culture indicated that a higher average ASC yield was obtained from the column-positive samples than from the lysis samples, suggesting that the column method may be superior to hemolysis for obtaining viable ASCs. Mesenchymal differentiation and network formation assays showed no statistical differences in ASC functions between the lysis and column-positive samples. Our results suggest that a column with non-woven rayon and polyethylene fabrics is useful for isolating stromal vascular fraction cells from LAF solutions for clinical applications. Copyright © 2014 International Society for Cellular Therapy. Published by Elsevier Inc. All rights reserved.

A new large-scale process for taxol and related taxanes from Taxus brevifolia.

PubMed

Rao, K V; Hanuman, J B; Alvarez, C; Stoy, M; Juchum, J; Davies, R M; Baxley, R

1995-07-01

In view of the demonstrated antitumor activity of taxol, ready availability of the drug is important. The current isolation methods starting from the bark of Taxus brevifolia involve multiple manipulations, leading to only taxol and in a yield of 0.01%. A new process consisting of a single reverse phase column is introduced here, and the present purpose is to determine its large scale applicability. The chloroform extractable fraction of the bark of T. brevifolia is applied directly on to a C-18 bonded silica column in 25% acetonitrile/water, with elution using a step gradient: 30-50% acetonitrile/water. On standing, eight different taxanes, including taxol, crystallize out directly from different fractions. The crystals are filtered and purified further by recrystallization. Taxol and four other taxanes are purified this way. The other three require a short silica column. Taxol is freed from cephalomannine by selective ozonolysis. The large scale process gave taxol (0.04%), 10-deacetylbaccatin III (0.02%), 10-deacetyl taxol-7-xyloside (0.1%), 10-deacetyl taxol-C-7-xyloside (0.04%), 10-deacetyl cephalomannine-7-xyloside (0.006%), taxol-7-xyloside (0.008%), 10-deacetyl taxol (0.008%) and cephalomannine (0.004%). Processing of the needles of T. brevifolia gave brevifoliol (0.17%), and that of the wood, 10-deacetyl taxol-C-7-xyloside (0.01%) and 10-deacetyl taxol-C. The reverse phase column process is simpler (one column, direct crystallization), more efficient (eight taxanes obtained simultaneously) and also gives higher yields.

Synthesis of zirconia monoliths for chromatographic separations.

PubMed

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

2006-03-17

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

Strong ion exchange in centrifugal partition extraction (SIX-CPE): effect of partition cell design and dimensions on purification process efficiency.

PubMed

Hamzaoui, Mahmoud; Hubert, Jane; Reynaud, Romain; Marchal, Luc; Foucault, Alain; Renault, Jean-Hugues

2012-07-20

The aim of this article was to evaluate the influence of the column design of a hydrostatic support-free liquid-liquid chromatography device on the process efficiency when the strong ion-exchange (SIX) development mode is used. The purification of p-hydroxybenzylglucosinolate (sinalbin) from a crude aqueous extract of white mustard seeds (Sinapis alba L.) was achieved on two types of devices: a centrifugal partition chromatograph (CPC) and a centrifugal partition extractor (CPE). They differ in the number, volume and geometry of their partition cells. The SIX-CPE process was evaluated in terms of productivity and sinalbin purification capability as compared to previously optimized SIX-CPC protocols that were carried out on columns of 200 mL and 5700 mL inner volume, respectively. The objective was to determine whether the decrease in partition cell number, the increase in their volume and the use of a "twin cell" design would induce a significant increase in productivity by applying higher mobile phase flow rate while maintaining a constant separation quality. 4.6g of sinalbin (92% recovery) were isolated from 25 g of a crude white mustard seed extract, in only 32 min and with a purity of 94.7%, thus corresponding to a productivity of 28 g per hour and per liter of column volume (g/h/LV(c)). Therefore, the SIX-CPE process demonstrates promising industrial technology transfer perspectives for the large-scale isolation of ionized natural products. Copyright © 2012 Elsevier B.V. All rights reserved.

Aqueous Reversed-Phase HPLC/FT-IR Using Diffuse Reflectance Detections

NASA Astrophysics Data System (ADS)

Kalasinsky, Victor F.; Pai, T. H.; Kenton, R. C.; Kalasinsky, Kathryn S.

1989-12-01

Solvent-elimination HPLC/FT-IR has become a viable combination of two important techniques, and we have been developing a system which is adaptable to both normal and reversed-phase liquid chromatography. The interface involves the deposition of HPLC eluites onto a KCI-laden train with subsequent analysis via diffuse reflectance spectroscopy, and with minor modifications, the system can be used with microbore and analytical columns. With aqueous solvents, the water is converted to methanol and acetone in a post-column reaction with 2,2-dimethoxypropane before the eluites are deposited. A number of different samples have been used to demonstrate the interface and its flexibility. Steroids, analgesics, and other pharmaceutical preparations have been separated with reverse-phase solvents and identified by their infrared spectra. For some of the compounds studied, different infrared spectra of a given compound have been found to exhibit intensity variations, which arise from different crystalline states. The differences can be concentration dependent and may be useful in obtaining semi-quantitative information from the infrared spectra. Applications involving both gradient elution and isocratic separations have been successful. The former provides the same advantages for HPLC/FT-IR as one finds in conventional HPLC. More recent work has been applied to the use of buffers such as those frequently used in bioanalytical separations. In trying to simplify the post-column reaction with water, we have immobilized dehydration reagents onto silica particles and packed these materials into a column which is inserted in-line after the analytical column. Of the reagents utilized to date, 3,3-dimethoxypropyltrimethoxysilane has been found to perform most efficiently. It has advantages over the simpler reagents because it can be regenerated in the reaction column. Results and the efficiency of the dehydration process and its relation to the type of reagent and its coverage will be discussed.

Continuous adsorption and biotransformation of micropollutants by granular activated carbon-bound laccase in a packed-bed enzyme reactor.

PubMed

Nguyen, Luong N; Hai, Faisal I; Dosseto, Anthony; Richardson, Christopher; Price, William E; Nghiem, Long D

2016-06-01

Laccase was immobilized on granular activated carbon (GAC) and the resulting GAC-bound laccase was used to degrade four micropollutants in a packed-bed column. Compared to the free enzyme, the immobilized laccase showed high residual activities over a broad range of pH and temperature. The GAC-bound laccase efficiently removed four micropollutants, namely, sulfamethoxazole, carbamazepine, diclofenac and bisphenol A, commonly detected in raw wastewater and wastewater-impacted water sources. Mass balance analysis showed that these micropollutants were enzymatically degraded following adsorption onto GAC. Higher degradation efficiency of micropollutants by the immobilized compared to free laccase was possibly due to better electron transfer between laccase and substrate molecules once they have adsorbed onto the GAC surface. Results here highlight the complementary effects of adsorption and enzymatic degradation on micropollutant removal by GAC-bound laccase. Indeed laccase-immobilized GAC outperformed regular GAC during continuous operation of packed-bed columns over two months (a throughput of 12,000 bed volumes). Copyright © 2016 Elsevier Ltd. All rights reserved.

Conventional and narrow bore short capillary columns with cyclodextrin derivatives as chiral selectors to speed-up enantioselective gas chromatography and enantioselective gas chromatography-mass spectrometry analyses.

PubMed

Bicchi, Carlo; Liberto, Erica; Cagliero, Cecilia; Cordero, Chiara; Sgorbini, Barbara; Rubiolo, Patrizia

2008-11-28

The analysis of complex real-world samples of vegetable origin requires rapid and accurate routine methods, enabling laboratories to increase sample throughput and productivity while reducing analysis costs. This study examines shortening enantioselective-GC (ES-GC) analysis time following the approaches used in fast GC. ES-GC separations are due to a weak enantiomer-CD host-guest interaction and the separation is thermodynamically driven and strongly influenced by temperature. As a consequence, fast temperature rates can interfere with enantiomeric discrimination; thus the use of short and/or narrow bore columns is a possible approach to speeding-up ES-GC analyses. The performance of ES-GC with a conventional inner diameter (I.D.) column (25 m length x 0.25 mm I.D., 0.15 microm and 0.25 microm d(f)) coated with 30% of 2,3-di-O-ethyl-6-O-tert-butyldimethylsilyl-beta-cyclodextrin in PS-086 is compared to those of conventional I.D. short column (5m length x 0.25 mm I.D., 0.15 microm d(f)) and of different length narrow bore columns (1, 2, 5 and 10 m long x 0.10 mm I.D., 0.10 microm d(f)) in analysing racemate standards of pesticides and in the flavour and fragrance field and real-world-samples. Short conventional I.D. columns gave shorter analysis time and comparable or lower resolutions with the racemate standards, depending mainly on analyte volatility. Narrow-bore columns were tested under different analysis conditions; they provided shorter analysis time and resolutions comparable to those of conventional I.D. ES columns. The narrow-bore columns offering the most effective compromise between separation efficiency and analysis time are the 5 and 2m columns; in combination with mass spectrometry as detector, applied to lavender and bergamot essential oil analyses, these reduced analysis time by a factor of at least three while separation of chiral markers remained unaltered.

Rapid and Green Separation of Mono- and Diesters of Monochloropropanediols by Ultrahigh Performance Supercritical Fluid Chromatography-Mass Spectrometry Using Neat Carbon Dioxide as a Mobile Phase.

PubMed

Jumaah, Firas; Jędrkiewicz, Renata; Gromadzka, Justyna; Namieśnik, Jacek; Essén, Sofia; Turner, Charlotta; Sandahl, Margareta

2017-09-20

This study demonstrates the effect of column selectivity and density of supercritical carbon dioxide (SC-CO 2 ) on the separation of monochloropropanediol (MCPD) esters, known as food toxicants, using SC-CO 2 without addition of cosolvent in ultrahigh performance supercritical fluid chromatography-mass spectrometry (UHPSFC-MS). This study shows that over 20 2-monochloropropanediol (2-MCPD) and 3-monochloropropanediol (3-MCPD) mono- and diesters are separated on a 2-picolylamine column in less than 12 min. The presence and position of a hydroxyl group in the structure, the number of unsaturated bonds, and the acyl chain length play a significant role in the separation of MCPD esters. The flow rate, backpressure, and column oven temperature, which affect the density of the mobile phase, were shown to have a substantial impact on retention, efficiency, and selectivity. The developed method was successfully applied for the determination of MCPD esters in refined oils and showed a close to excellent green analysis score using the Analytical Eco-Scale.

Interactive Data Exploration with Smart Drill-Down

PubMed Central

Joglekar, Manas; Garcia-Molina, Hector; Parameswaran, Aditya

2017-01-01

We present smart drill-down, an operator for interactively exploring a relational table to discover and summarize “interesting” groups of tuples. Each group of tuples is described by a rule. For instance, the rule (a, b, ⋆, 1000) tells us that there are a thousand tuples with value a in the first column and b in the second column (and any value in the third column). Smart drill-down presents an analyst with a list of rules that together describe interesting aspects of the table. The analyst can tailor the definition of interesting, and can interactively apply smart drill-down on an existing rule to explore that part of the table. We demonstrate that the underlying optimization problems are NP-Hard, and describe an algorithm for finding the approximately optimal list of rules to display when the user uses a smart drill-down, and a dynamic sampling scheme for efficiently interacting with large tables. Finally, we perform experiments on real datasets on our experimental prototype to demonstrate the usefulness of smart drill-down and study the performance of our algorithms. PMID:28210096

The hydrodynamic drag and the mobilisation of sediment into the water column of towed fishing gear components

NASA Astrophysics Data System (ADS)

O'Neill, F. G.; Summerbell, Keith David

2016-12-01

The hydrodynamic drag of towed fishing gears leads to direct impacts on the benthic environment, and can play a major role in the overall economic efficiency of the fishing operation and emissions of nitrogen oxides, sulphur oxides and greenhouse gases such as CO2. Here we investigate some of the underpinning processes which govern these issues and make direct hydrodynamic drag measurements and calculate the hydrodynamic drag coefficients for a range of well-defined gear components that, when fished, are in contact with the seabed. We measure the concentration and particle size distribution of the sediment mobilised into the water column in the wake of these gear elements, at a range of towing speeds, and demonstrate that as the hydrodynamic drag increases the amount of sediment mobilised also increases. We also vary the weight of the elements and show that this does not influence the amount of sediment put into the water column. These results provide a better understanding of the physical and mechanical processes that take place when a towed fishing gear interacts with the seabed. They will permit the development of more fuel efficient gears and gears of reduced benthic impact and will improve the empirical modelling of the sediment mobilised into the turbulent wake behind towed fishing gears which will lead to better assessments of the environmental and ecological impact of fishing gears.

A bioassay for the detection of perchlorate in the ppb range.

PubMed

Heinnickel, Mark; Smith, Stephen C; Koo, Jonathan; O'Connor, Susan M; Coates, John D

2011-04-01

A bioassay for the determination of ppb (μg·L(-1)) concentrations of perchlorate has been developed and is described herein. The assay uses the enzyme perchlorate reductase (PR) from the perchlorate-reducing organism Dechloromonas agitata in purified and partially purified forms to detect perchlorate. The redox active dye phenazine methosulfate (PMS) is shown to efficiently shuttle electrons to PR from NADH. Perchlorate can be determined indirectly by monitoring NADH oxidization by PR. To lower the detection limit, we have shown that perchlorate can be concentrated on a solid-phase extraction (SPE) column that is pretreated with the cation decyltrimethylammonium bromide (DTAB). Perchlorate is eluted from these columns with a solution of 2 M NaCl and 200 mM morpholine propane sulfonic acid (MOPS, pH 12.5). By washing these columns with 15 mL of 2.5 mM DTAB and 15% acetone, contaminating ions, such as chlorate and nitrate, are removed without affecting the bioassay. Because of the effect of complex matrices on the SPE columns, the method of standard additions is used to analyze tap water and groundwater samples. The efficacy of the developed bioassay was demonstrated by analyzing samples from 2-17000 ppb in deionized lab water, tap water, and contaminated groundwater.

Experimental design of a twin-column countercurrent gradient purification process.

PubMed

Steinebach, Fabian; Ulmer, Nicole; Decker, Lara; Aumann, Lars; Morbidelli, Massimo

2017-04-07

As typical for separation processes, single unit batch chromatography exhibits a trade-off between purity and yield. The twin-column MCSGP (multi-column countercurrent solvent gradient purification) process allows alleviating such trade-offs, particularly in the case of difficult separations. In this work an efficient and reliable procedure for the design of the twin-column MCSGP process is developed. This is based on a single batch chromatogram, which is selected as the design chromatogram. The derived MCSGP operation is not intended to provide optimal performance, but it provides the target product in the selected fraction of the batch chromatogram, but with higher yield. The design procedure is illustrated for the isolation of the main charge isoform of a monoclonal antibody from Protein A eluate with ion-exchange chromatography. The main charge isoform was obtained at a purity and yield larger than 90%. At the same time process related impurities such as HCP and leached Protein A as well as aggregates were at least equally well removed. Additionally, the impact of several design parameters on the process performance in terms of purity, yield, productivity and buffer consumption is discussed. The obtained results can be used for further fine-tuning of the process parameters so as to improve its performance. Copyright © 2017 Elsevier B.V. All rights reserved.

Comparison of various second-dimension gradient types in comprehensive two-dimensional liquid chromatography.

PubMed

Jandera, Pavel; Hájek, Tomás; Cesla, Petr

2010-06-01

Gradient elution provides significant improvement in peak capacity with respect to isocratic conditions. In the second dimension, gradients are limited to a short-time period available for separation. Various types of second-dimension gradients in comprehensive LC x LC are compared: (i) "full in fraction", (ii) "segment in fraction" and (iii) "continuously shifting" gradients, applied in orthogonal LC x LC separations of phenolic acids and flavones on a polyethylene glycol column in the first dimension and two types of porous shell fused-core C18 columns in the second dimension (Ascentis Express and Kinetex). The porous shell columns provide narrow bandwidths and fast second-dimension separations at moderate operating pressure that allows important savings of the overall separation time in comprehensive LC x LC separations. The effects of the gradient type on the bandwidths, theoretical peak capacity, separation time and column pressure in the second dimension were investigated. The type of gradient program controls the range of lipophilicity of sample compounds that can be separated in the second-dimension reversed-phase time period. This range can be calibrated using alkylbenzene standards, to design the separation conditions for complete sample separation, avoiding harmful wrap around of non-eluted compounds to the subsequent second-dimension fractions.

Partial Prestress Concrete Beams Reinforced Concrete Column Joint Earthquake Resistant On Frame Structure Building

NASA Astrophysics Data System (ADS)

Astawa, M. D.; Kartini, W.; Lie, F. X. E.

2018-01-01

Floor Building that requires a large space such as for the meeting room, so it must remove the column in the middle of the room, then the span beam above the room will be long. If the beam of structural element with a span length reaches 15.00 m, then it is less effective and efficient using a regular Reinforced Concrete Beam because it requires a large section dimension, and will reduce the beauty of the view in terms of aesthetics of Architecture. In order to meet these criteria, in this design will use partial prestressing method with 400/600 mm section dimension, assuming the partial Prestressed Beam structure is still able to resist the lateral force of the earthquake. The design of the reinforcement has taken into account to resist the moment due to the gravitational load and lateral forces. The earthquake occurring on the frame structure of the building. In accordance with the provisions, the flexural moment capacity of the tendon is permitted only by 25% of the total bending moment on support of the beam, while the 75% will be charged to the reinforcing steel. Based on the analysis result, bring ini 1 (one) tendon contains 6 strand with diameter 15,2 mm. On the beam pedestal, requires 5D25 tensile reinforcement and 3D25 for the compression reinforcement, for shear reinforcement on the pedestal using Ø10-100 mm. Dimensional column section are 600/600 mm with longitudinal main reinforcement of 12D25, and transverse reinforcement Ø10-150. At the core of the beam-column joint, use the transversal reinforcement Ø10-100 mm. The moment of Column versus Beam Moment ∑Me > 1.2 Mg, with a value of 906.99 kNm > 832.25 kNm, qualify for ductility and Strong Columns-weak beam. Capacity of contribution bending moment of Strand Tendon’s is 23.95% from the total bending moment capacity of the beam, meaning in accordance with the provisions. Thus, the stability and ductility structure of Beam-Column joint is satisfy the requirements of SNI 2847: 2013 and ACI 318-11.

On-line hyphenation of solid-phase extraction to chromatographic separation of sulfonamides with fused-core columns in sequential injection chromatography.

PubMed

Batista, Alex D; Chocholouš, Petr; Satínský, Dalibor; Solich, Petr; Rocha, Fábio R P

2015-02-01

On-line sample pretreatment (clean-up and analyte preconcentration) is for the first time coupled to sequential injection chromatography. The approach combines anion-exchange solid-phase extraction and the highly effective pentafluorophenylpropyl (F5) fused-core particle column for separation of eight sulfonamide antibiotics with similar structures (sulfathiazole, sulfanilamide, sulfacetamide, sulfadiazine, sulfamerazine, sulfadimidine, sulfamethoxazole and sulfadimethoxine). The stationary phase was selected after a critical comparison of the performance achieved by three fused-core reversed phase columns (Ascentis(®) Express RP-Amide, Phenyl-Hexyl, and F5) and two monolithic columns (Chromolith(®) High Resolution RP-18 and CN). Acetonitrile and acetate buffer pH 5.0 at 0.60 mL min(-1) were used as mobile phase to perform the separations before spectrophotometric detection. The first mobile phase was successfully used as eluent from SPE column ensuring transfer of a narrow zone to the chromatographic column. Enrichment factors up to 39.2 were achieved with a 500 µL sample volume. The developed procedure showed analysis time <10.5 min, resolutions >1.83 with peak symmetry ≤1.52, LODs between 4.9 and 27 µg L(-1), linear response ranges from 30.0 to 1000.0 µg L(-1) (r(2)>0.996) and RSDs of peak heights <2.9% (n=6) at a 100 µg L(-1) level and enabled the screening control of freshwater samples contaminated at the 100 µg L(-1) level. The proposed approach expanded the analytical potentiality of SIC and avoided the time-consuming batch sample pretreatment step, thus minimizing risks of sample contamination and analyte losses. Copyright © 2014 Elsevier B.V. All rights reserved.

RP-HPLC ANALYSIS OF ACIDIC AND BASIC DRUGS IN SYSTEMS WITH DIETHYLAMINE AS ELUENTS ADDITIVE.

PubMed

Petruczynik, Anna; Wroblewski, Karol; Strozek, Szymon; Waksmundzka-Hajnos, Monika

2016-11-01

The chromatographic behavior of some basic and acidic drugs was studied on Cl 8, Phenyl-Hexyl and Polar RP columns with methanol or acetonitrile as organic modifiers of aqueous mobile phases containing addition of diethylamine. Diethylamine plays a double function of silanol blocker reagent in analysis of basic drugs and ion-pair reagent in analysis of acidic drugs. Most symmetrical peaks and highest system efficiency were obtained on Phenyl-Hexyl and Polar RP columns in tested mobile phase systems compared to results obtained on C18 column. A new rapid, simple, specific and accurate reverse phase liquid chromatographic method was developed for the simultaneous determination of atorvastatin - antihyperlipidemic drug and amlodipine - calcium channel blocker in one pharmaceutical formulation. Atorvastatin is an acidic compounds while amlodipine is a basic substance. The chromatographic separation was carried out on Phenyl-Hexyl column by gradient elution mode with acetonitrile as organic modifier, acetate buffer at pH 3.5 and Q.025 M/L diethylamine. The proposed method was validated for specificity, precision, accuracy, linearity, and robustness. The linearity range of atorvastatin and amlodipine for 5 - 100 μg/mL was obtained with limits of-detection (LOD) 3.2750 gg/mL and 3.2102 μg/mL, respectively. The proposed method made use of DAD as a tool for peak identity and purity confirmation.

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

PubMed

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

2005-08-12

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

π-Extended triptycene-based material for capillary gas chromatographic separations.

PubMed

Yang, Yinhui; Wang, Qinsi; Qi, Meiling; Huang, Xuebin

2017-10-02

Triptycene-based materials feature favorable physicochemical properties and unique molecular recognition ability that offer good potential as stationary phases for capillary gas chromatography (GC). Herein, we report the investigation of utilizing a π-extended triptycene material (denoted as TQPP) for GC separations. As a result, the TQPP capillary column exhibited high column efficiency of 4030 plates m -1 and high-resolution performance for a wide range of analytes, especially structural and positional isomers. Interestingly, the TQPP stationary phase showed unique shape selectivity for alkanes isomers and preferential retention for analytes with halogen atoms and H-bonding nature mainly through their halogen-bonding and H-bonding interactions. In addition, the TQPP column had good repeatability and reproducibility with the RSD values of 0.02-0.34% for run-to-run, 0.09-0.80% for day-to-day and 1.4-5.2% for column-to-column, respectively, and favorable thermal stability up to 280 °C. This work demonstrates the promising future of triptycene-based materials as a new class of stationary phases for GC separations. Copyright © 2017 Elsevier B.V. All rights reserved.

Development of a purification procedure for the isolation of nucleosides from urine prior to mass spectrometric analysis.

PubMed

Dudley, E; El-Shakawi, S; Games, D E; Newton, R P

2000-03-01

A chromatographic separation of nucleosides from urine has been developed in order to facilitate their mass spectrometric analysis for clinical diagnosis. A number of chromatographic resins were studied in order to develop an effective and efficient purification procedure. The optimized sequential protocol comprises a centrifugation, acidification and neutralization step, followed by application of an affinity chromatographic column and finally further separation on an acidic cation exchange column and a basic anion exchanger. This scheme shows effective clean-up of a standard radiolabelled nucleoside with a recovery of 92.5%, and recovery of nucleosides added to urine samples before extraction showed recoveries of 72-82%.

Thermal Analysis for Ion-Exchange Column System

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

Lee, Si Y.; King, William D.

2012-12-20

Models have been developed to simulate the thermal characteristics of crystalline silicotitanate ion exchange media fully loaded with radioactive cesium either in a column configuration or distributed within a waste storage tank. This work was conducted to support the design and operation of a waste treatment process focused on treating dissolved, high-sodium salt waste solutions for the removal of specific radionuclides. The ion exchange column will be installed inside a high level waste storage tank at the Savannah River Site. After cesium loading, the ion exchange media may be transferred to the waste tank floor for interim storage. Models weremore » used to predict temperature profiles in these areas of the system where the cesium-loaded media is expected to lead to localized regions of elevated temperature due to radiolytic decay. Normal operating conditions and accident scenarios (including loss of solution flow, inadvertent drainage, and loss of active cooling) were evaluated for the ion exchange column using bounding conditions to establish the design safety basis. The modeling results demonstrate that the baseline design using one central and four outer cooling tubes provides a highly efficient cooling mechanism for reducing the maximum column temperature. In-tank modeling results revealed that an idealized hemispherical mound shape leads to the highest tank floor temperatures. In contrast, even large volumes of CST distributed in a flat layer with a cylindrical shape do not result in significant floor heating.« less

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

PubMed

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

2012-03-02

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

Using Reactive Transport Modeling to Understand Changes in Electrical Conductivity Associated with Bacterial Growth and Respiration

NASA Astrophysics Data System (ADS)

Regberg, A. B.; Singha, K.; Picardal, F.; Brantley, S. L.

2011-12-01

Previous research has linked measured changes in the bulk electrical conductivity (σb) of water-saturated sediments to the respiration and growth of anaerobic bacteria. If the mechanism causing this signal is understood and characterized it could be used to identify and monitor zones of bacterial activity in the subsurface. The 1-D reactive transport model PHREEQC was used to understand σb signals by modeling chemical gradients within two column reactors and corresponding changes in effluent chemistry. The flow-through column reactors were packed with Fe(III)-bearing sediment from Oyster, VA and inoculated with an environmental consortia of microorganisms. Influent in the first reactor was amended with 1mM Na-acetate to encourage the growth of iron-reducing bacteria. Influent in the second reactor was amended with 0.1mM Na-Acetate and 2mM NaNO3 to encourage the growth of nitrate-reducing bacteria. While effluent concentrations of acetate, Fe(II), NO3-, NO2-, and NH4+ remained at steady state, we measured a 3-fold increase (0.055 S/m - 0.2 S/m) in σb in the iron-reducing column and a 10-fold increase in σb (0.07 S/m - 0.8 S/m) in the nitrate-reducing column over 198 days. The ionic strength in both reactors remained constant through time indicating that the measured increases in σb were not caused by changing effluent concentrations. PHREEQC successfully matched the measured changes in effluent concentrations for both columns when the reaction database was modified in the following manner. For the iron-reducing column, kinetic expressions governing the rate of iron reduction, the rate of bacterial growth, and the production of methane were added to the reaction database. Additionally, surface adsorption and cation exchange reactions were added so that the model was consistent with measured effluent chemistry. For the nitrate-reducing column, kinetic expressions governing nitrate reduction and bacterial growth were added to the reaction database. Additionally, immobile porosity was added along with adsorption and cation exchange reactions. Although the model revealed the existence of chemical and biological gradients within the columns that were not discernable as changes in effluent concentrations, none of the chemical reactions or gradients could explain the measured σb increases in either column. This result is not consistent with chemical gradients within the column reactor causing the measured changes in σb. To test the alternate hypothesis that microbial biofilms are electrically conductive, we used the output from PHREEQC to calculate the amount of biomass produced within the column reactors. If biofilm causes the σb changes, our model is consistent with an electrical conductivity for biomass in the iron-reducing column between 2.75 and 220 S/m. The model is also consistent with an electrical conductivity for biomass in the nitrate-reducing column between 350 and 35,000 S/m. These estimates of biomass electrical conductivity are poorly constrained but represent a first step towards understanding the electrical properties associated with respiring biofilms.

Validation of a Microscale Extraction and High Throughput UHPLC-QTOF-MS Analysis Method for Huperzine A in Huperzia

PubMed Central

Cuthbertson, Daniel; Piljac-Žegarac, Jasenka; Lange, Bernd Markus

2011-01-01

Herein we report on an improved method for the microscale extraction of huperzine A (HupA), an acetylcholinesterase-inhibiting alkaloid, from as little as 3 mg of tissue homogenate from the clubmoss Huperzia squarrosa (G. Forst.) Trevis with 99.95 % recovery. We also validated a novel UHPLC-QTOF-MS method for the high-throughput analysis of H. squarrosa extracts in only 6 min, which, in combination with the very low limit of detection (20 pg on column) and the wide linear range for quantification (20 to 10,000 pg on column), allow for a highly efficient screening of extracts containing varying amounts of HupA. Utilization of this methodology has the potential to conserve valuable plant resources. PMID:22275140

Catalytic reactive separation system for energy-efficient production of cumene

DOEpatents

Buelna, Genoveva [Nuevo Laredo, MX; Nenoff, Tina M [Albuquerque, NM

2009-07-28

The present invention relates to an atmospheric pressure, reactive separation column packed with a solid acid zeolite catalyst for producing cumene from the reaction of benzene with propylene. Use of this un-pressurized column, where simultaneous reaction and partial separation occur during cumene production, allow separation of un-reacted, excess benzene from other products as they form. This high-yielding, energy-efficient system allows for one-step processing of cumene, with reduced need for product purification. Reacting propylene and benzene in the presence of beta zeolite catalysts generated a selectivity greater than 85% for catalytic separation reactions at a reaction temperature of 115 degrees C and at ambient pressure. Simultaneously, up to 76% of un-reacted benzene was separated from the product; which could be recycled back to the reactor for re-use.

Micro-columns packed with Chlorella vulgaris immobilised on silica gel for mercury speciation.

PubMed

Tajes-Martínez, P; Beceiro-González, E; Muniategui-Lorenzo, S; Prada-Rodríguez, D

2006-02-28

A method has been developed for mercury speciation in water by using columns packed with Chlorella vulgaris immobilised on silica gel. The method involves the retention of CH(3)Hg(+) and Hg(2+) in micro-columns prepared by packing immobilised algae in polypropylene tubes, followed by selective and sequential elution with 0.03 and 1.5M HCl for CH(3)Hg(+) and Hg(2+), respectively. The adsorption capacity of the micro-algae for Hg(2+) and CH(3)Hg(+) has been evaluated using free and immobilised C. vulgaris. The efficiency uptake for both species at pH 3 was higher than 97%. Studies were carried out on the effect of retention and elution conditions for both species. Furthermore, the stability of mercury species retained on algae-silica gel micro-columns and lifetime of the columns were also investigated. Hg(2+) showed a higher stability than CH(3)Hg(+) at 0 degrees C (21 and 3 days, respectively) and a better lifetime than for the organic species. The developed method was applied to the analysis of spiked tap, sea and wastewater samples. Recovery studies on tap and filtered seawater provided results between 96+/-3 and 106+/-2 for Hg(2+) and from 98+/-5 to 107+/-5 for CH(3)Hg(+), for samples spiked with single species. For samples spiked with both CH(3)Hg(+) and Hg(2+), the average recoveries varied from 96+/-5 to 99+/-3 and from 103+/-6 to 115+/-5 for Hg(2+) and CH(3)Hg(+), respectively. However, the percentages of retention and elution on wastewater and unfiltered seawater were only adequate for the inorganic species.

[High-performance liquid-liquid chromatography in beverage analysis].

PubMed

Bricout, J; Koziet, Y; de Carpentrie, B

1978-01-01

Liquid liquid chromatography was performed with columns packed with stationary phases chemically bonded to silica microparticules. These columns show a high efficiency and are used very easily. Flavouring compounds like aromatic aldehydes which have a low volatility were analyzed in brandy using a polar phase alkylnitrile. Sapid substances like amarogentin in Gentiana lutea or glyryrrhizin in Glycyrrhiza glabra were determined by reversed phase chromatography. Finally ionizable substances like synthetic dyes can be analyzed by paired ion chromatography witha non polar stationary phase.

Honeycomb-Fin Heat Sink

NASA Technical Reports Server (NTRS)

Rippel, Wally E.

1989-01-01

Improved finned heat sink for electronic components more lightweight, inexpensive, and efficient. Designed for use with forced air, easily scaled up to dissipate power up to few hundred watts. Fins are internal walls of aluminum honeycomb structure. Cell structure gives strength to thin aluminum foil. Length of channels chosen for thermodynamic efficency; columns of cells combined in any reasonable number because flowing air distributed to all. Heat sink cools nearly as effectively at ends as near its center, no matter how many columns of cells combined.

Nonlinear Adjustment with or without Constraints, Applicable to Geodetic Models

DTIC Science & Technology

1989-03-01

corrections are neglected, resulting in the familiar (linearized) observation equations. In matrix notation, the latter are expressed by V = A X + I...where A is the design matrix, x=X -x is the column-vector of parametric corrections , VzLa-L b is the column-vector of residuals, and L=L -Lb is the...X0 . corresponds to the set ua of model-surface 0 coordinates describing the initial point P. The final set of parametric corrections , X, then

Q-marker based strategy for CMC research of Chinese medicine: A case study of Panax Notoginseng saponins.

PubMed

Zhong, Yi; Zhu, Jieqiang; Yang, Zhenzhong; Shao, Qing; Fan, Xiaohui; Cheng, Yiyu

2018-01-31

To ensure pharmaceutical quality, chemistry, manufacturing and control (CMC) research is essential. However, due to the inherent complexity of Chinese medicine (CM), CMC study of CM remains a great challenge for academia, industry, and regulatory agencies. Recently, quality-marker (Q-marker) was proposed to establish quality standards or quality analysis approaches of Chinese medicine, which sheds a light on Chinese medicine's CMC study. Here manufacture processes of Panax Notoginseng Saponins (PNS) is taken as a case study and the present work is to establish a Q-marker based research strategy for CMC of Chinese medicine. The Q-markers of Panax Notoginseng Saponins (PNS) is selected and established by integrating chemical profile with pharmacological activities. Then, the key processes of PNS manufacturing are identified by material flow analysis. Furthermore, modeling algorithms are employed to explore the relationship between Q-markers and critical process parameters (CPPs) of the key processes. At last, CPPs of the key processes are optimized in order to improving the process efficiency. Among the 97 identified compounds, Notoginsenoside R 1 , ginsenoside Rg 1 , Re, Rb 1 and Rd are selected as the Q-markers of PNS. Our analysis on PNS manufacturing show the extraction process and column chromatography process are the key processes. With the CPPs of each process as the inputs and Q-markers' contents as the outputs, two process prediction models are built separately for the extraction process and column chromatography process of Panax notoginseng, which both possess good prediction ability. Based on the efficiency models of extraction process and column chromatography process we constructed, the optimal CPPs of both processes are calculated. Our results show that the Q-markers derived from CMC research strategy can be applied to analyze the manufacturing processes of Chinese medicine to assure product's quality and promote key processes' efficiency simultaneously. Copyright © 2018 Elsevier GmbH. All rights reserved.

[hHO-1 structure prediction and its mutant construct, expression, purification and activity analysis].

PubMed

Xia, Zhen Wei; Cui, Wen Jun; Zhou, Wen Pu; Zhang, Xue Hong; Shen, Qing Xiang; Li, Yun Zhu; Yu, Shan Chang

2004-10-01

Human Heme Oxygenase-1 (hHO-1) is the rate-limiting enzyme in the catabolism reaction of heme, which directly regulates the concentration of bilirubin in human body. The mutant structure was simulated by Swiss-pdbviewer procedure, which showed that the structure of active pocket was changed distinctly after Ala25 substituted for His25 in active domain, but the mutated enzyme still binded with heme. On the basis of the results, the expression vectors, pBHO-1 and pBHO-1(M), were constructed, induced by IPTG and expressed in E. coli DH5alpha strain. The expression products were purified with 30%-60% saturation (NH4)2SO4 and Q-Sepharose Fast Flow column chromatography. The concentration of hHO-1 in 30%-60% saturation (NH4)2SO4 components and in fractions through twice column chromatography was 3.6-fold and 30-fold higher than that in initial product, respectively. The activity of wild hHO-1 (whHO-1) and mutant hHO-1 (deltahHO-1) showed that the activity of deltahHO-1 was reduced 91.21% compared with that of whHO-1. The study shows that His25 is of importance for the mechanism of hHO-1, and provides the possibility for effectively regulating the activity to exert biological function.

Comparison of Niskin vs. in situ approaches for analysis of gene expression in deep Mediterranean Sea water samples

NASA Astrophysics Data System (ADS)

Edgcomb, V. P.; Taylor, C.; Pachiadaki, M. G.; Honjo, S.; Engstrom, I.; Yakimov, M.

2016-07-01

Obtaining an accurate picture of microbial processes occurring in situ is essential for our understanding of marine biogeochemical cycles of global importance. Water samples are typically collected at depth and returned to the sea surface for processing and downstream experiments. Metatranscriptome analysis is one powerful approach for investigating metabolic activities of microorganisms in their habitat and which can be informative for determining responses of microbiota to disturbances such as the Deepwater Horizon oil spill. For studies of microbial processes occurring in the deep sea, however, sample handling, pressure, and other changes during sample recovery can subject microorganisms to physiological changes that alter the expression profile of labile messenger RNA. Here we report a comparison of gene expression profiles for whole microbial communities in a bathypelagic water column sample collected in the Eastern Mediterranean Sea using Niskin bottle sample collection and a new water column sampler for studies of marine microbial ecology, the Microbial Sampler - In Situ Incubation Device (MS-SID). For some taxa, gene expression profiles from samples collected and preserved in situ were significantly different from potentially more stressful Niskin sampling and preservation on deck. Some categories of transcribed genes also appear to be affected by sample handling more than others. This suggests that for future studies of marine microbial ecology, particularly targeting deep sea samples, an in situ sample collection and preservation approach should be considered.

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

NASA Astrophysics Data System (ADS)

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

2015-02-01

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